Abstract: The present disclosure relates to a fiber having non-circular cross section obtained from a polyester composition, said fiber having improved dyeability, gloss and tenacity. The present disclosure also relates to a process for preparing the polyester composition for making fiber having non-circular cross section. The present disclosure further relates to a process for making an embroidery yarn from said fiber.
FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULE, 2003 COMPLETE SPECIFICATION
(See section 10; rule 13)
A FIBER MADE FROM A POLYESTER COMPOSITION AND A PROCESS FOR PREPARING THE POLYESTER COMPOSITION
RELIANCE INDUSTRIES LIMITED
an Indian Company of 3rd Floor, Maker Chamber-IV, 222, Nariman Point, Mumbai-400021,
Maharashtra, India
Inventors: Jain Ashwin Kumar, Huilgol Santosh Raghavendra, Pushap Sudan,
Kashetwar Abhijit Vasantrao, Mane Bhalchandra Ramchandra, Garg Vijay Kumar and Agarwal Uday Shankar.
THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED
FIELD OF DISCLOSURE
The present disclosure relates to a fiber made from a polyester composition. The present disclosure particularly relates to a fiber having non-circular cross section. The present disclosure also relates to a process for preparing a polyester composition.
BACKGROUND:
Polyesters, especially polyalkylene terephthalates, have excellent physical and chemical properties. In particular, polyester fibers have a high melting point, and can attain high orientation and crystallinity. Further, polyester fibers have excellent properties such as chemical, heat and light stability, and high strength. Polyesters are used for resins, films and fibers. Further, blends of polyester with viscose, cotton, acrylic, wool and the like have been widely used in apparels / upholstery because of their properties such as crease recovery, durability, wash and wear properties. However, Polyester fibers and fabrics have, poor dyeability and, in particular, are hardly dyeable with dyes other than disperse dyes. The molecular structure and the high levels of orientation and crystallinity contribute to a resistance to coloration by dye compounds. Also contributing to the difficulty in dyeing polyesters is that they do not have dye sites within the polymer chain that are reactive to basic or acid dye compounds.
Conventionally, polyesters can be dyed with only disperse dyes. Such dyeing processes require high temperatures and special dyeing equipment such as High Temperature High Pressure (HTHP) dyeing machines. Various proposals have been made to
improve the dyeability of the polyester. In order to carry out dyeing of polyester at lower
temperature, carrier additives which promote dye solubility at lower temperature are
used. However, such carrier additives are non-environment friendly and hence not
recommended.
The most representative process for the improvement in dyeability is disclosed in
Japanese Patent Publication No. 10497/1959 which comprises copolymerizing sodium
5-sulfoisophthalate into raw material polyester.
The drawback associated with the process disclosed in Japanese Patent Publication No. 10497/1959 is that it employs a large amount of sodium 5-sulfoisophthalate to obtain dyeability of satisfactory level. Copolymerization of sodium 5-sulfoisophthalate in a large amount significantly increases the melt viscosity of the resulting copolymerized polyester so that it becomes difficult to increase the degree of polymerization of the copolymerized polyester sufficiently and to spin the resulting copolymerized polyester stably. This problem may be resolved by decreasing the degree of polymerization of the copolymerized polyester to such a level that assures ready polymerization and stable melt spinning. However, the fiber obtained by this process is poor in strength with limited end applications. On the other hand, if the degree of polymerization of the copolymerized polyester is increased, within a limit to assure melt spinnability, to obtain a high-strength fiber, the drawability of the as-spun fiber will decrease. Further, the gloss of the polymer obtained by the process as disclosed in Japanese Patent Publication No. 10497/1959 is not satisfactory for embroidery applications.
Therefore, there is a felt need for a fiber having improved dyeability, tenacity and gloss.
DEFINITION:
As used in the present specification, the following word/s and phrase/s are generally intended to have the meanings as set forth below, except to the extent that the context in which they are used indicate otherwise.
The term "fiber' in the context of the specification means a staple fiber or a filament yarn.
OBJECTS:
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
It is an object of the present disclosure to provide a fiber having non-circular cross section.
It is another object of the present disclosure to provide a fiber having non-circular cross section with improved dyeability, tenacity and gloss.
It is still another object of the present disclosure to provide a process for preparing a polyester composition for making a fiber having non-cricular cross section.
It is still another object of the present disclosure to provide a simple and economic process for preparing a polyester composition.
It is still another object of the present disclosure to provide a process for making an embroidery yarn.
It is yet another object of the present disclosure to provide a process for making an
embroidery yarn which obviates the use of non-environment friendly chemicals for
dyeing.
It is yet another object of the present disclosure to provide a process for making an
embroidery yarn which is energy efficient.
It is yet another object of the present disclosure to provide an article which is adapted to receive embroidery.
Other objects and advantages of the present disclosure will be more apparent from the following description, which are not intended to limit the scope of the present disclosure.
SUMMARY:
In one aspect of the present disclosure there is provided a fiber having non-circular cross section made from a polyester composition, said polyester composition being a poly-condensation product of a mixture comprising:
a. polyethylene terephthalate in an amount ranging between 85.0 % and
95.0 % with respect to the total mass of the polyester composition,
b. polyalkylene diol being at least one selected from the group consisting of
polymethylene glycol, polyethylene glycol and polypropylene glycol, and
c. at least one co-monomer, wherein the co-monomer is a metal salt of
sulfoisophthalic acid or an ester thereof, the metal being selected from
the group consisting of sodium, potassium, lithium, rubidium, cesium,
magnesium, calcium and cobalt,
said polyester composition characterized in that the proportion of the polyalkylene diol and the co-monomer ranges between 3:1 and 1:3 and the sum total of (b) and (c) ranges between 5.0 % and 15.0 % with respect to the total mass of the polyester . composition.
Typically, the non-circular cross section is tri-lobal cross section.
Typically, the fiber of the present disclosure further comprises at least one compound selected from the group consisting of pentaerythritol, phthalic anhydride, trimellitic anhydride and pyromellitic dianhydride.
Typically, the fiber of the present disclosure further comprises at least one particulate agent selected from the group consisting of zinc oxide, titanium dioxide (Ti02) and barium sulphate (BaS04), wherein the amount of the particulate agent ranges between 0.01 % and 0.5 % with respect to the total mass of the polyester composition.
Typically, the fiber of the present disclosure further comprises at least one toner selected from the group consisting of elemental cobalt, cobalt acetate, cobalt chloride, cobalt formate, cobalt terephthalate, cobalt nitrate, cobalt sulfate, ammonium cobalt chloride, ultramarine blue and iron oxide, wherein the amount of the toner ranges between 2 ppm and 100 ppm with respect to the total mass of the polyester composition.
Typically, the fiber of the present disclosure further comprises at least one thermal stabilizer selected from the group consisting of phosphoric acid, phosphorous acid, trimethyl phosphite, triphenyl phosphite, trisnonyl phenyl phosphite, triethyl phosphono acetate and triethyl phosphate, wherein the concentration of elemental phosphrous (P)
ranges between 10 ppm and 35 ppm with respect to the total mass of the polyester composition.
Typically, the co-monomer further comprises at least one dicarboxylic acid compound selected from the group consisting of isophthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 4,4'-diphenyl dicarboxylic acid, 4,4'-diphenylmethane dicarboxylic acid, diphenyl ketone dicarboxylic acid, 4,4'-diphenylsulfone dicarboxylic acid, succinic acid, adipic acid and azelaic acid.
Typically, the co-monomer further comprises at least one a hydroxyl compound selected from the group consisting of 1,2-propyfene glycol, trimethylene glycol, tetramethylene glycol, heptamethylene glycol, hexamethylene glycol, diethylene glycol, dipropylene glycol, bis(trimethylene glycol), bis(tetramethylene glycol), triethylene glycol, 1,4-dihydroxy cyclohexane, 1,4-cyclohexanedimethanol, methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, hexyl alcohol, octyl alcohol, decyl alcohol, phenol, benzyl alcohol and ethylene glycol.
Typically, the fiber of the present disclosure is characterized by a tenacity of less than 3 gpd, gloss of at least 3, and dye ability at less than 100 °C.
Typically, the polyalkylene diol is polyethylene glycol having molecular weight ranging between 1000 and 2000.
In another aspect of the present disclosure there is provided a process for preparing a polyester composition for making fibers having non-circular cross section, said process comprising the following steps:
i. esterifying terephthalic acid using monoethylene glycol at a temperature of 225 °C to 260 °C under inert gas pressure of 1 to 2 kg/cm2g to obtain an esterified mixture,
ii. adding
a. Sb203 catalyst, wherein, the concentration of elemental antimony (Sb)
in the reaction mixture ranges between 250 ppm and 350 ppm with
respect to the total mass of the reaction mixture,
b. polyalkylene diol being at least one selected from the group consisting
of polymethylene glycol, polyethylene glycol and polypropylene glycol,
and
c. at least one co-monomer, wherein the co-monomer is a metal salt of
sulfoisophthalic acid or an ester thereof, the metal being selected from
the group consisting of sodium, potassium, lithium, rubidium, cesium,
magnesium, calcium and cobalt,
into the esterified mixture to obtain a reaction mixture and subjecting said reaction mixture to polycondensation at a temperature of 270 °C to 300 °C under vacuum of 1 mmHg to 5 mmHg to obtain a polyester composition,
said process characterized in that the proportion of the polyalkylene diol and the co-monomer ranges between 3:1 and 1:3 and the sum total of (b) and (c) ranges between 5.0 % and 15.0 % with respect to the total mass of the reaction mixture.
Typically, the non-circular cross section is tri-lobal cross section.
Typically, the process of the present disclosure further comprises incorporating at least one compound selected from the group consisting of pentaerythritol, phthalic anhydride, trimellitic anhydride and pyromellitic dianhydride.
Typically, the process of the present disclosure further comprises incorporating at least one particulate agent selected from the group consisting of zinc oxide, titanium dioxide (Ti02) and barium sulphate (BaS04), wherein the amount of the particulate agent ranges between 0.01 % and 0.5 % with respect to the total mass of the reaction mixture.
Typically, the process of the present disclosure further comprises incorporating at least one toner selected from the group consisting of elemental cobalt, cobalt acetate, cobalt chloride, cobalt formate, cobalt terephthalate, cobalt nitrate, cobalt sulfate, ammonium cobalt chloride, ultramarine blue and iron oxide, wherein the amount of the toner ranges between 2 ppm and 100 ppm with respect to the total mass of the reaction mixture.
Typically, the process of the present disclosure further comprises incorporating at least one thermal stabilizer selected from the group consisting of phosphoric acid,
phosphorous acid, trimethyl phosphite, triphenyl phosphite, trisnonyl phenyl phosphite, triethyl phosphono acetate and triethyl phosphate, wherein the concentration of elemental phosphrous (P) ranges between 10 ppm and 35 ppm with respect to the total mass of the reaction mixture.
Typically, the co-monomer further comprises at least one dicarboxylic acid compound selected from the group consisting of isophthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 4,4'-diphenyl dicarboxylic acid, 4,4'-diphenylmethane dicarboxylic acid, diphenyl ketone dicarboxylic acid, 4,4'-diphenylsulfone dicarboxylic acid, succinic acid, adipic acid and azelaic acid.
Typically, the co-monomer further comprises at least one a hydroxyl compound selected from the group consisting of 1,2-propylene glycol, trimethylene glycol, tetramethylene glycol, heptamethylene glycol, hexamethylene glycol, diethylene glycol, dipropylene glycol, bis(trimethylene glycol), bis(tetramethylene glycol), triethylene glycol, 1,4-dihydroxy cyclohexane, 1,4-cyclohexanedimethanol, methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, hexyl alcohol, octyl alcohol, decyl alcohol, phenol, benzyl alcohol and ethylene glycol.
Typically, the molar ratio of terephthalic acid and monoethylene glycol ranges between 1:1 and 1:5.
Typically, the polyalkylene diol is polyethylene glycol having molecular weight ranging between 1000 and 2000.
In yet another aspect of the present disclosure there is provided a process for making embroidery yarn, said process comprising at least one of the following steps:
i. spinning the fiber of the present disclosure to form Fully Drawn Yarn
(FDY) or Draw twisted yarn (DTY), ii. rewinding the Fully Drawn Yarn or Draw twisted yarn at a rate of 300 to
1200 mpm, iii. twisting the rewinded Fully Drawn Yarn or Draw twisted yarn at a rate of
5000 to 12000 rpm/20 to 100 mpm and subsequently at a rate of 5000 to
12000 rpm/20 to 100 mpm to obtain twisted tubes, iv. setting the twisted tubes by heating at a temperature ranging between 80
°C and 130 °C for a time period ranging between 0.5 hrs and 3.0 hours to
obtain a heat set yarn, v. rewinding the heat set yarn at a rate of 300 to 700 mpm to obtain soft
winding packages, vi. dyeing the soft winding packages at less than 100 °C followed by drying
by passing through a radio frequency drier to obtain a dyed yarn, and vii. tubing the dyed yarn on tube reels to obtain embroidery yarn.
Typically, the method step (ii) is carried out on cops.
Typically, the method step (v) is carried out on an apparatus selected from the group consisting of metallic spring, metallic perforated tubes and polyvinyl chloride perforated tubes.
In yet another aspect of the present disclosure there is provided a twisted yarn made from the fiber of the present disclosure.
In yet another aspect of the present disclosure there is provided an article adapted to receive embroidery obtained from fiber of the present disclosure, said article being selected from the group consisting of fabric and garment.
In yet another aspect of the present disclosure there is provided a blend comprising a fiber of the present disclosure and at least one fibrous material selected from the group consisting of cotton, viscose, wool and acrylic.
DETAILED DESCRIPTION:
In accordance,with one aspect of the present disclosure there is provided a fiber having non-circular cross section with improved dyeability. The non-circular cross section of the fiber of the present disclosure is tri-lobal cross section. The fiber of the present disclosure is made from a polyester composition which in turn is a poly-condensation product of a mixture comprising: (a) polyethylene terephthalate in an amount ranging between 85.0 % and 95.0 % with respect to the total mass of the polyester composition,
(b) at least one polyalkylene diol, and (c) at least one co-monomer selected from the group consisting of a metal salt of sulfoisophthalic acid or ester thereof. The metal present in the metal salt of sulfoisophthalic acid or ester thereof is selected from the group consisting of sodium, potassium, lithium, rubidium, cesium, magnesium, calcium and cobalt.
The poly-condensation product useful in making fiber of the present disclosure is modified with defined proportions of polyalkylene diol and co-monomer. The fiber extruded or made from the polyester composition where the proportion of the polyalkylene'diol and the co-monomer is maintained between 3:1 and 1:3 and the sum total of the polyalkylene diol and co-monomer is maintained in the range of 5.0 % and 15.0 % with respect to the total mass of the polyester composition, possesses improved properties in terms of tenacity, dyeability and gloss.
The polyalkylene diol used along with co-monomer is at least one selected from the group consisting of polymethylene glycol, polyethylene glycol and polypropylene glycol.
Though the desired results may be obtained by using any polyalkylene diol, the use of polyethylene glycol having molecular weight ranging between 1000 and 2000 provides desired results. It was observed that if the molecular weight of the polyalkylene diol is less than 1000 then the dyeing temperature of the fiber made from the polyester composition is not effectively lowered. On the other hand, if the molecular weight of the polyalkylene diol is higher than 2000 then the required level of randomization in the resulting polymer may not be achieved.
The co-monomer present in the polyester composition additionally may comprise at least one dicarboxylic acid compound selected from the group consisting of isophthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 4,4'-diphenyl dicarboxylic acid, 4,4'-diphenylmethane dicarboxylic acid, diphenyl ketone dicarboxylic acid, 4,4,-diphenylsulfone dicarboxylic acid, succinic acid, adipic acid and azelaic acid.
The co-monomer further, optionally may comprise a hydroxyl compound selected from the group consisting of 1,2-propylene glycol, trimethylene glycol, tetramethylene glycol, heptamethylene glycol, hexamethylene glycol, diethylene glycol, dipropylene glycol, bis(trimethylene glycol), bis(tetramethylene glycol), triethylene glycol, 1,4-dihydroxy cyclohexane, 1,4-cyclohexanedimethanol, methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, hexyl alcohol, octyl alcohol, decyl alcohol, phenol, benzyl alcohol and ethylene glycol.
The physical and chemical properties such as dyeability, tensile strength, color fastness or gloss and softness of an article prepared from the polyester composition of the present disclosure may be improved by further addition of various components into the polyester composition. Further, the quantity of the individual component is so adjusted that it provides the requisite physical and chemical properties to an article prepared from the polyester composition of the present disclosure.
For example, compounds such as pentaerythritol, phthalic anhydride, trimellitic anhydride and pyromellitic dianhydride and combinations thereof may be added to further reduce tensile strength of a fiber prepared from the polyester composition of the
present disclosure. Further reduction in tensile strength is desirable in case the fiber is to be used for hand embroidery.
Inorganic oxides such as zinc oxide, titanium dioxide, barium sulphate and combinations thereof may further be added into the polyester composition of the present disclosure as particulate agent in an amount ranging between 0.01% and 0.5 % with respect to the total mass of the polyester composition. The function of the particulate agent is added to provide sheen or glow to a fiber/an article prepared from the polyester composition of the present disclosure.
The polyester composition may additionally comprise at least one toner selected from the group consisting of elemental cobalt, cobalt acetate, cobalt chloride, cobalt formate, cobalt terephthalate, cobalt nitrate, cobalt sulfate, ammonium cobalt chloride, ultramarine blue and iron oxide, wherein the amount of the toner ranges between 2 ppm and 100 ppm with respect to the total mass of the polyester composition.
The polyester composition may also comprise at least one thermal stabilizer selected from the group consisting of phosphoric acid, phosphorous acid, trimethyl phosphite, triphenyl phosphite, trisnonyl phenyl phosphite, triethyl phosphono acetate and triethyl phosphate. The thermal stabilizer provides a thermal stability to polyester composition and/or to an article prepared from the polyester composition. It is observed that the concentration of elemental phosphrous (P) when maintained between 10 ppm and 35 ppm provides sufficient thermal stability to the. polyester composition and/or an article prepared from the polyester composition.
The fiber of the present disclosure is characterized by a tenacity of less than 3 gpd, gloss of at least 3, and dye ability at less than 100 °C
In another aspect of the present disclosure there is provided a process for preparing polyester composition for making a fiber having non-circular cross section, the non-circular cross section being tri-lobal cross section. In the first step, terephthalic acid is esterified using monoethylene glycol. The molar ratio of terephthalic acid and monoethylene glycol ranges between 1:1 and 1:5. The esterification is carried out at a temperature of 225 °C to 260 °C under inert gas pressure of 1 to 2 kg/cm2g to obtain an esterified mixture.
Then to the esterified mixture various components in predetermined quantity are added which is subjected to poly-condensation reaction.
The components added into the esterified mixture to obtain a reaction mixture comprise Sb2O3 catalyst, at least one polyalkylene diol, at least one co-monomer selected from the group consisting of a metal salt of sulfoisophthalic acid or an ester thereof, optionally, at least one compound selected from the group consisting of pentaerythritol, phthalic anhydride, trimellitic anhydride and pyromellitic dianhydride, optionally, at least one particulate agent selected from the group consisting of zinc oxide, titanium dioxide (Ti02) and barium sulphate (BaS04), wherein the amount of the particulate agent ranges between 0.01 % and 0.5 % with respect to the total mass of the reaction mixture, optionally, at least one toner selected from the group consisting of elemental cobalt, cobalt acetate, cobalt chloride, cobalt formate, cobalt terephthalate, cobalt nitrate, cobalt sulfate, ammonium cobalt chloride, ultramarine blue and iron oxide, wherein the amount of the toner ranges between 2 ppm and 100 ppm with respect to the total mass of the
reaction mixture, and optionally, at least one thermal stabilizer selected from the group consisting of phosphoric acid, phosphorous acid, trimethyl phosphite, triphenyl phosphite, trisnonyl phenyl phosphite, triethyl phosphono acetate and triethyl phosphate, wherein the concentration of elemental phosphrous (P) ranges between 10 ppm and 35 ppm with respect to the total mass of the reaction mixture.
The metal present in the metal salt of sulfoisophthalic acid or an ester thereof is selected from the group consisting of sodium, potassium, lithium, rubidium, cesium, magnesium, calcium and cobalt.
Tne reaction mixture is then subjected to poly-condensation at a temperature of 270 °C to 300°C under vacuum of 1 mmHg to 5 mmHg to obtain a polyester composition of the present disclosure.
The amount of the catalyst added into the esterified mixture is such that the concentration of elemental antimony (Sb) in the reaction mixture ranges between 250 ppm and 350 ppm with respect to the total mass of the reaction mixture.
The various components added into the esterified mixture may be added at any stage i.e., before, during or after the poly-condensation reaction.
The process of the present disclosure is characterized in that the proportion of poiyalkylene diol and the co-monomer ranges between 3:1 and 1:3 and the sum total of polyalkylene diol and the co-monomer ranges between 5.0 % and 15.0 % with respect to the total mass of the reaction mixture. The polyakylene diol used for preparing polyester composition of the present disclosure is at teast one selected from the group consisting of polymethylene glycol, polyethylene glycol and polypropylene glycol.
Particularly, the polyalkylene diol used is polyethylene glycol having molecular weight ranging between 1000 and 2000.
The co-monomer additionally may comprise at least one dicarboxylic acid compound selected from the group consisting of isophthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 4,4'-diphenyl dicarboxylic acid, 4,4'-diphenylmethane dicarboxylic acid, diphenyl ketone dicarboxylic acid, 4,4'-diphenylsulfone dicarboxylic acid, succinic acid, adipic acid and azelaic acid. .
The co-monomer optionally may also comprise hydroxyl compound selected from the group consisting of 1,2-propylne glycol, trimethylene glycol, tetramethyl heptamethylene glycol, hexamethylene glycol, diethylene glycol, dipropylene glycol, bis(trimethylene glycol), bis(tetramethylene glycol), triethylene glycol, 1,4-dihydroxy cyclohexane, 1,4-cyclohexanedimethanol, methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, hexyl alcohol, octyl alcohol, decyl alcohol, phenol, benzyl alcohol and ethylene glycol.
In yet another aspect of the present disclosure there is provided a process for making embroidery yarn. The process is described herein after which comprises at least one of the described steps. Initially, the non-circular fiber of the present disclosure is spun to form Fully Drawn Yarn (FDY) or Draw twisted yarn (DTY). This Fully Drawn Yarn or Draw twisted yarn are rewinded on cops at a rate of 300 to 1200 mpm. The rewinded Fully Drawn Yarn or Draw twisted yarn are twisted at a rate of 5000 to 12000 rpm/20 to 100 mpm to obtain twisted tubes. The twisted tubes are then subjected to heat setting at
a temperature ranging between 80 °C and 130 °C for a time period ranging between 0.5 hrs and 3.0 hours to obtain a heat set yarn.
The heat set yarn is again rewinded at a rate of 300 to 700 mpm on an apparatus selected from the group consisting of metallic spring, metallic perforated tubes and polyvinyl chloride perforated tubes to obtain soft winding packages which are dyed at less than 100 °C followed by drying. The drying is carried out by passing dyed yarn through a radio frequency drier to obtain a dried yarn. Finally, the dried yarn is tubed on tube reels to obtain yarn. The yarn obtained is characterized by a tenacity of less than 3 gpd and gloss of at least 3.
In still another aspect of the present disclosure there is provided a twisted yarn made from the fiber of the present disclosure.
In yet another aspect of the present disclosure there is provided an article adapted to receive embroidery obtained from fiber of the present disclosure. The article prepared from the fiber is selected from the group consisting of fabric and garment.
In yet another aspect of the present disclosure there is provided a blend comprising a fiber of the present disclosure and at least one fibrous material selected from the group consisting of cotton, viscose, wool and acrylic.
The present disclosure is further described in light of the following examples which are set forth for illustration purposes only and are not to be construed limiting the scope of the disclosure.
Example 1
Purified terephthalic acid and monoethyleneglycol were esterified in the mole ratio of 1:2 at temperature of 225°C to 260°C and under nitrogen pressure of 1 to 2 kg/cm2 g. Water formed during theesterification reaction and excess MEG were removed, cooled and recovered. To the esterified mixture, catalyst, SD2O3 (290ppm Sb); thermal stabilizer, H3PO4 {25 ppm P); toner, cobalt acetate (25 ppm Co), delusterant, Ti02 (0.05% with respect to the total mass of the reaction mixture), polyethylene glycol of molecular weight 1500 (3.0% with respect to the total mass of the reaction mixture) and bishydroxyethyl ester of sulfoisophthalic acid, sodium salt, (4.0 % with respect to the total mass of the reaction mixture) were added. The reaction mixture was polycondensed at a temperature of 280 to 290°C and under vacuum of around 1mm Hg.
The polymer formed was drained into strands and quenched in water bath. The strands were cut into chips in a pelletizer. The polymer chips were crystallized, dried and melt spun in a spinning machine in the form of Fully Drawn Yarn (FDY) (110 denier / 36 filaments) with trilobal cross-section. The FDY sample was twisted (2-ply, 500 twists/meter); heat set at 85°C to form embroidery thread and was then knitted into hose , and dyed with cationic dye in 2% shade at 90°C for 45 min. The results of physical properties and dyeability are tabulated in Table I.
Comparative Example 1
Purified terephthalic acid and monoethyleneglycol were esterified in the mole ratio of 1:2 at temperature of 225°C to 260°C and under nitrogen pressure of 1 to 2 kg/cm2g. Water formed during the esterification reaction and excess MEG were removed, cooled and recovered. To the esterified mixture, catalyst, Sb203 (290ppm Sb); thermal stabilizer,
H3PO4 (25 ppm P); toner, cobalt acetate (25 ppm Co), delusterant, Ti02 (0.05% with respect to the total mass of the reaction mixture ) and bishydroxyethyl ester of sulfoisophthallc acid, sodium salt, 4.0 % with respect to the total mass of the reaction mixture) were added. The reaction mixture was polycondensed at a temperature, of 280 to 290°C and under vacuum of around 1mm Hg.
The polymer formed was drained into strands and quenched in water bath. The strands were cut into chips in a pelletizer. The polymer chips were crystallized, dried and melt spun in a spinning machine in the form of Fully Drawn Yarn (FDY) (110 denier / 36 filaments) with trilobal cross-section. The FDY sample was twisted (2-ply, 500 twists/meter); heat set at 85°C to form embroidery thread and was then knitted into hose and dyed with cationic dye in 2% shade at 90°C for 45 min. The results of physical properties and dyeability are tabulated in Table I.
Table I:
Example Tenacity (9Pd) Dyebath Exhaustion (%) Dye Depth (K/S)
1 2.9 100 33
Comparative Example 1 3.5 40 14
Example 2
Purified terephthalic acid and monoethyleneglycol were esterified in the mole ratio of 1:2 at temperature of 225°C to 260°C and under nitrogen pressure of 1 to 2 kg/cm2g. Water formed during the esterification reaction and excess MEG were removed, cooled and recovered. To the esterified mixture, catalyst, Sb2O3 (290ppm Sb); thermal stabilizer, H3PO4 (25 ppm P); toner, cobalt acetate (25 ppm Co), delusterant, Ti02 (0.05% with respect to the total mass of the reaction mixture ), polyethylene glycol of molecular weight 1500 (3.0% with respect to the total mass of the reaction mixture) and bishydroxyethyl ester of sulfoisophthalic acid, sodium salt, (4.0 % with respect to the total mass of the reaction mixture) were added. The reaction mixture was polycondensed at a temperature of 280 to 290°C and under vacuum of around 1mm Hg.
The polymer formed was drained into strands and quenched in water bath. The strands were cut into chips in a pelletizer. The polymer chips were crystallized, dried and melt spun in a spinning machine in the form of Fully Drawn Yarn (FDY) (110 denier / 36 filaments) with trilobal cross-section. The FDY sample was wound on white flat strip and gloss was measured using Gloss meter. The results are tabulated in Table II.
Comparative Example 2
Purified terephthalic acid and monoethyleneglycol were esterified in the mole ratio of 1:2 at temperature of 225°C to 260°C and under nitrogen pressure of 1 to 2 kg/cm2g. Water formed during the esterification reaction and excess MEG were removed, cooled and recovered. To the esterified mixture, catalyst, Sb2O3 (290ppm Sb); thermal stabilizer, H3PO4 (25 ppm P); toner, cobalt acetate (25 ppm Co), delusterant, Ti02 (0.05% with respect to the total mass of the reaction mixture ) and bishydroxyethyl ester of
sulfoisophthalic acid, sodium salt, (4.0 % with respect to the total mass of the reaction mixture) were added. The reaction mixture was polycondensed at a temperature of 280 to 290°C and under vacuum of around 1 mm Hg.
The polymer formed was drained into strands and quenched in water bath. The strands were cut into chips in a pelletizer. The polymer chips were crystallized, dried and melt spun in a spinning machine in the form of Fully Drawn Yarn (FDY) (110 denier / 36 filaments) with circular cross-section. The FDY sample was wound on white flat strip and gloss was measured using Gloss meter at 60 degree angle. The results are tabulated in Table II.
Table II:
Example Gloss
2 4.7
Comparative Example 2 3.7
Higher gloss values in example-2 indicate better shine which is desirable in embroidery yarn applications.
Throughout this specification the word "comprise", or variations such as "comprises" or "comprising'', will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression "at least" or "at least one" suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results.
Any discussion of documents, acts, materials, devices, articles or the like that has been included in this specification is solely for the purpose of providing a context for the disclosure. It is not to be taken as an admission that any or all of these matters form a part of the prior art base or were common general knowledge in the field relevant to the disclosure as it existed anywhere before the priority date of this application.
The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the disclosure, unless there is a statement in the specification specific to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated toai many additional features can be added-and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.
We Claim:
1. A fiber having non-circular cross section made from a polyester composition, said
polyester composition being a poly-condensation product of a mixture
comprising:
a. polyethylene terephthalate in an amount ranging between 85.0 % and
95.0 % with respect to the total mass of the polyester composition,
b. polyalkylene diol being at least one selected from the group consisting of
polymethylene glycol, polyethylene glycol and polypropylene glycol, and
c. at least one co-monomer, wherein the co-monomer is a metal salt of
sulfoisophthalic acid or an ester thereof, the metal being selected from
the group consisting of sodium, potassium, lithium, rubidium, cesium,
magnesium, calcium and cobalt,
said polyester composition characterized in that the proportion of the polyalkylene diol and the co-monomer ranges between 3:1 and 1:3 and the sum total of (b) and (c) ranges between 5.0 % and 15.0 % with respect to the total mass of the polyester composition.
2. The fiber as claimed in claim 1, wherein the non-circular cross section is tri-lobal cross section.
3. The fiber as claimed in claim 1, further comprises at least one compound selected from the group consisting of pentaerythritol, phthalic anhydride, trimellitic anhydride and pyromellitic dianhydride.
4. The fiber as claimed in claim 1, further comprises at least one particulate agent selected from the group consisting of zinc oxide, titanium dioxide (Ti02) and barium sulphate (BaS04), wherein the amount of the particulate agent ranges between 0.01 % and 0.5 % with respect to the total mass of the polyester composition.
5. The fiber as claimed in claim 1, further comprises at least one toner selected from the group consisting of elemental cobalt, cobalt acetate, cobalt chloride, cobalt formate, cobalt terephthalate, cobalt nitrate, cobalt sulfate, ammonium cobalt chloride, ultramarine blue and iron oxide, wherein the amount of the toner ranges between 2 ppm and 100 ppm with respect to the total mass of the polyester composition.
6. The fiber as claimed in claim 1, further comprises at least one thermal stabilizer selected from the group consisting of phosphoric acid, phosphorous acid, trimethyl phosphite, triphenyl phosphite, trisnonyl phenyl phosphite, triethyl phosphono acetate and triethyl phosphate, wherein the concentration of elemental phosphrous (P) ranges between 10,ppm and 35 ppm with respect to the total mass of the polyester composition.
7. The fiber as claimed in claim 1, wherein the co-monomer further comprises at least one dicarboxylic acid compound selected from the group consisting of isophthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 4,4'-diphenyl dicarboxylic acid, 4,4'-diphenylmethane dicarboxylic acid,
diphenyl ketone tricarboxylic acid, 4,4'-diphenylsulfone dicarboxylic acid, succinic acid, adipic acid and azelaic acid.
8. The fiber as claimed in claim 1, wherein the co-monomer further comprises at least one a hydroxyl compound selected from the group consisting of 1,2-propylene glycol, trimethylene glycol, tetramethylene glycol, heptamethylene glycol, hexamethylene glycol, diethylene glycol, dipropylene glycol, bis(trimethylene glycol), bis{tetramethylene glycol), triethylene glycol, 1,4-dihydroxy cyclohexane, 1,4-cyclohexanedimethanol, methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, hexyl alcohol, octyl alcohol, decyl alcohol, phenol, benzyl alcohol and ethylene glycol.
9. The fiber as claimed in claim 1, being characterized by a tenacity of less than 3 gpd, gloss of at least 3, and dye ability at less than 100 °C.
10. The fiber as claimed in claim 1, wherein the polyalkylene diol is polyethylene
-glycol having molecular weight ranging between 1000 and 2000.
11. A process for preparing a polyester composition for making fibers having non-
circular cross section, said process comprising the following steps:
i. esterifying terephthalic acid using monoethylene glycol at a temperature of 225 °C to 260 °C under inert gas pressure of 1 to 2 kg/cm2g to obtain an esterified mixture,
ii. adding
a. Sb203 catalyst, whereirvthe concentration of elemental antimony (Sb) in
the reaction mixture ranges between 250 ppm and 350 ppm with respect
to the total mass of the reaction mixture,
b. polyalkylene diol being at least one selected from the group consisting of
polymethylene glycol, polyethylene glycol and polypropylene glycol, and
c. at least one co-monomer, wherein the co-monomer is a metal salt of
sulfoisophthalic acid or an ester thereof, the metal being selected from
the group consisting of sodium, potassium, lithium, rubidium, cesium,
magnesium, calcium and cobalt,
into the esterified mixture to obtain a reaction mixture and subjecting said reaction mixture to polycondensation at a temperature of 270 °C to 300 °C under vacuum of 1 mmHg to 5 mmHg to obtain a polyester composition,
said process characterized in that the proportion of the polyalkylene diol and the co-monomer ranges between 3:1 and 1:3 and the sum total of (b) and (c) ranges between 5.0 % and 15.0 % with respect to the total mass of the reaction mixture.
12. The process as claimed in claim 11, wherein the non-circular cross section is tri-lobal cross section.
13. The process as claimed in claim 11, further comprises incorporating at least one compound selected from the group consisting of pentaerythritol, phthalic anhydride, trimellitic anhydride and pyromellitic dianhydride.
14. The process as claimed in claim 11, further comprises incorporating at least one particulate agent selected from the group consisting of zinc oxide, titanium dioxide (Ti02) and barium sulphate (BaS04), wherein the amount of the particulate agent ranges between 0.01 % and 0.5 % with respect to the total mass of the reaction mixture.
15. The process as claimed in claim 11, further comprises incorporating at least one toner selected from the group consisting of elemental cobalt, cobalt acetate, cobalt chloride, cobalt formate, cobalt terephthalate, cobalt nitrate, cobalt sulfate, ammonium cobalt chloride, ultramarine blue and iron oxide, wherein the amount of the toner ranges between 2 ppm and 100 ppm with respect to the total mass of the reaction mixture.
16. The process as claimed in claim 11, further comprises incorporating at least one thermal stabilizer selected from the group consisting of phosphoric acid, phosphorous acid, trimethyl phosphite, triphenyl phosphite, trisnonyl phenyl phosphite, triethyl phosphono acetate and triethyl phosphate, wherein the concentration of elemental phosphrous (P) ranges between 10 ppm and 35 ppm with respect to the total mass of the reaction mixture.
17. The process as claimed in claim 11, wherein the co-monomer further comprises at least one dicarboxylic acid compound selected from the group consisting of isophthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 4,4'-diphenyl dicarboxylic acid, 4,4'-diphenylmethane dicarboxylic acid,
diphenyl ketone dicarboxyfic acid, 4,4'-diphenylsulfone dicarboxylic acid, succinic acid, adipic acid and azelaic acid.
18. The process as claimed in claim 11, wherein the co-monomer further comprises at least one a hydroxy! compound selected from the group consisting of 1,2-propyfene glycol, trimethylene glycol, tetramethylene glycol, heptamethylene glycol, hexamethylene glycol, diethylene glycol, dipropylene glycol, bis(trimethylene glycol), bis(tetramethylene glycol), triethylene glycol, 1,4-dihydroxy cyclohexane, 1,4-cyclohexanedimethanol, methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, hexyl alcohol, octyl alcohol, decyl alcohol, phenol, benzyl alcohol and ethylene glycol.
19. The process as claimed in claim 11, wherein the molar ratio of terephthalic acid and monoethylene glycol ranges between 1:1 and 1:5.
20. The process as claimed in claim 11, wherein the polyalkylene diol is polyethylene glycol having molecular weight ranging between 1000 and 2000.
21. A process for making embroidery yarn, said process comprising at least one of the following steps:
i. spinning the fiber of claim 1 to form Fully Drawn Yarn (FDY) or Draw
twisted yarn (DTY), ii. rewinding the Fully Drawn Yarn or Draw twisted yarn at a rate of 300 to
1200 mpm,
iii. twisting the rewinded Fully Drawn Yarn or Draw twisted yarn at a rate of
5000 to 12000 rpm/20 to 100 mpm and subsequently at a rate of 5000 to
12000 rpm/20 to 100 mpm to obtain twisted tubes, iv. setting the twisted tubes by heating at a temperature ranging between 80
°C and 130 °C for a time period ranging between 0.5 hrs and 3.0 hours to
obtain a heat set yarn, v. rewinding the heat set yarn at a rate of 300 to 700 mpm to obtain soft
winding packages, vi. dyeing the soft winding packages at less than 100 °C followed by drying
by passing through a radio frequency drier to obtain a dyed yarn, and vii. tubing the dyed yarn on tube reels to obtain embroidery yarn.
22. The process as claimed in claim 21, wherein the method step (ii) is carried out on cops.
23. The process as claimed in claim 21, wherein the method step (v) is carried out on an apparatus selected from the group consisting of metallic spring, metallic perforated tubes and polyvinyl chloride perforated tubes.
24. A twisted yarn made from the fiber of claim 1.
25. An article adapted to receive embroidery obtained from fiber as claimed in claim 1, said article being selected from the group consisting of fabric and garment.
26.A blend comprising a fiber of claim 1 and at least one fibrous material selected from the group consisting of cotton, viscose, wool and acrylic.
| # | Name | Date |
|---|---|---|
| 1 | 1293-MUM-2012-Power of Attorney-291015.pdf | 2018-08-11 |
| 1 | 1293-MUM-2012-RELEVANT DOCUMENTS [22-09-2023(online)].pdf | 2023-09-22 |
| 2 | 1293-MUM-2012-FORM 5(23-4-2013).pdf | 2018-08-11 |
| 2 | 1293-MUM-2012-RELEVANT DOCUMENTS [30-09-2022(online)].pdf | 2022-09-30 |
| 3 | 1293-MUM-2012-RELEVANT DOCUMENTS [30-09-2021(online)].pdf | 2021-09-30 |
| 3 | 1293-MUM-2012-FORM 3.pdf | 2018-08-11 |
| 4 | 1293-MUM-2012-RELEVANT DOCUMENTS [28-03-2020(online)].pdf | 2020-03-28 |
| 4 | 1293-MUM-2012-FORM 2.pdf | 2018-08-11 |
| 5 | 1293-MUM-2012-FORM 4 [24-06-2019(online)].pdf | 2019-06-24 |
| 5 | 1293-MUM-2012-FORM 2(TITLE PAGE).pdf | 2018-08-11 |
| 6 | 1293-MUM-2012-RELEVANT DOCUMENTS [30-03-2019(online)].pdf | 2019-03-30 |
| 6 | 1293-MUM-2012-FORM 2(TITLE PAGE)-(23-4-2013).pdf | 2018-08-11 |
| 7 | 1293-MUM-2012-FORM 2(23-4-2013).pdf | 2018-08-11 |
| 7 | 1293-MUM-2012- ORIGINAL UR 6(1A) FORM 26-310818.pdf | 2018-12-04 |
| 8 | 1293-MUM-2012-IntimationOfGrant06-09-2018.pdf | 2018-09-06 |
| 8 | 1293-MUM-2012-FORM 13(23-4-2013).pdf | 2018-08-11 |
| 9 | 1293-MUM-2012-FORM 1.pdf | 2018-08-11 |
| 9 | 1293-MUM-2012-PatentCertificate06-09-2018.pdf | 2018-09-06 |
| 10 | 1293-MUM-2012-FER.pdf | 2018-08-11 |
| 10 | 1293-MUM-2012-Written submissions and relevant documents (MANDATORY) [05-09-2018(online)].pdf | 2018-09-05 |
| 11 | 1293-MUM-2012-DESCRIPTION(PROVISIONAL).pdf | 2018-08-11 |
| 11 | 1293-MUM-2012-FORM-26 [31-08-2018(online)].pdf | 2018-08-31 |
| 12 | 1293-MUM-2012-DESCRIPTION(COMPLETE)-(23-4-2013).pdf | 2018-08-11 |
| 12 | 1293-MUM-2012-HearingNoticeLetter.pdf | 2018-08-28 |
| 13 | 1293-MUM-2012-ABSTRACT [23-08-2018(online)].pdf | 2018-08-23 |
| 13 | 1293-MUM-2012-CORRESPONDENCE.pdf | 2018-08-11 |
| 14 | 1293-MUM-2012-CLAIMS [23-08-2018(online)].pdf | 2018-08-23 |
| 14 | 1293-MUM-2012-Correspondence-291015.pdf | 2018-08-11 |
| 15 | 1293-MUM-2012-CORRESPONDENCE(23-4-2013).pdf | 2018-08-11 |
| 15 | 1293-MUM-2012-FER_SER_REPLY [23-08-2018(online)].pdf | 2018-08-23 |
| 16 | 1293-MUM-2012-ABSTRACT(23-4-2013).pdf | 2018-08-11 |
| 16 | 1293-MUM-2012-CLAIMS(23-4-2013).pdf | 2018-08-11 |
| 17 | 1293-MUM-2012-CLAIMS(23-4-2013).pdf | 2018-08-11 |
| 17 | 1293-MUM-2012-ABSTRACT(23-4-2013).pdf | 2018-08-11 |
| 18 | 1293-MUM-2012-CORRESPONDENCE(23-4-2013).pdf | 2018-08-11 |
| 18 | 1293-MUM-2012-FER_SER_REPLY [23-08-2018(online)].pdf | 2018-08-23 |
| 19 | 1293-MUM-2012-CLAIMS [23-08-2018(online)].pdf | 2018-08-23 |
| 19 | 1293-MUM-2012-Correspondence-291015.pdf | 2018-08-11 |
| 20 | 1293-MUM-2012-ABSTRACT [23-08-2018(online)].pdf | 2018-08-23 |
| 20 | 1293-MUM-2012-CORRESPONDENCE.pdf | 2018-08-11 |
| 21 | 1293-MUM-2012-DESCRIPTION(COMPLETE)-(23-4-2013).pdf | 2018-08-11 |
| 21 | 1293-MUM-2012-HearingNoticeLetter.pdf | 2018-08-28 |
| 22 | 1293-MUM-2012-DESCRIPTION(PROVISIONAL).pdf | 2018-08-11 |
| 22 | 1293-MUM-2012-FORM-26 [31-08-2018(online)].pdf | 2018-08-31 |
| 23 | 1293-MUM-2012-FER.pdf | 2018-08-11 |
| 23 | 1293-MUM-2012-Written submissions and relevant documents (MANDATORY) [05-09-2018(online)].pdf | 2018-09-05 |
| 24 | 1293-MUM-2012-PatentCertificate06-09-2018.pdf | 2018-09-06 |
| 24 | 1293-MUM-2012-FORM 1.pdf | 2018-08-11 |
| 25 | 1293-MUM-2012-IntimationOfGrant06-09-2018.pdf | 2018-09-06 |
| 25 | 1293-MUM-2012-FORM 13(23-4-2013).pdf | 2018-08-11 |
| 26 | 1293-MUM-2012-FORM 2(23-4-2013).pdf | 2018-08-11 |
| 26 | 1293-MUM-2012- ORIGINAL UR 6(1A) FORM 26-310818.pdf | 2018-12-04 |
| 27 | 1293-MUM-2012-RELEVANT DOCUMENTS [30-03-2019(online)].pdf | 2019-03-30 |
| 27 | 1293-MUM-2012-FORM 2(TITLE PAGE)-(23-4-2013).pdf | 2018-08-11 |
| 28 | 1293-MUM-2012-FORM 4 [24-06-2019(online)].pdf | 2019-06-24 |
| 28 | 1293-MUM-2012-FORM 2(TITLE PAGE).pdf | 2018-08-11 |
| 29 | 1293-MUM-2012-RELEVANT DOCUMENTS [28-03-2020(online)].pdf | 2020-03-28 |
| 29 | 1293-MUM-2012-FORM 2.pdf | 2018-08-11 |
| 30 | 1293-MUM-2012-RELEVANT DOCUMENTS [30-09-2021(online)].pdf | 2021-09-30 |
| 30 | 1293-MUM-2012-FORM 3.pdf | 2018-08-11 |
| 31 | 1293-MUM-2012-FORM 5(23-4-2013).pdf | 2018-08-11 |
| 31 | 1293-MUM-2012-RELEVANT DOCUMENTS [30-09-2022(online)].pdf | 2022-09-30 |
| 32 | 1293-MUM-2012-Power of Attorney-291015.pdf | 2018-08-11 |
| 32 | 1293-MUM-2012-RELEVANT DOCUMENTS [22-09-2023(online)].pdf | 2023-09-22 |
| 1 | Search_23-07-2018.pdf |