Description:FORM 2
THE PATENT ACT, 1970
(39 OF 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)
1. Title of the invention: “Resin binder system for Tap hole clay/Mud Gun mass to achieve long aging life”
2. Applicant:
NAME NATIONALITY ADDRESS
Promis Industries INDIAN B-27 Phase 3, Adityapur Industrial area, Adityapur, Jamshedpur, 832109
Email: ndpatel47@yahoo.com shreedattalawconsultancy@gmail.com Chothani18preeti@gmail.com
(M) +91- 9031087907
3. Preamble to the description
COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it is to be performed:

 
Field of the Invention:
The present invention relates to a chemical composition for resin binder system for tap hole clay/mud gun mass to plug metal tapping hole in a blast furnace for steel to achieve long aging life. The tap hole clay/mud gun mass compositions for blast furnace tap holes comprising of phenol-formaldehyde resin, extender and acid catalysis.
Background of the Invention:
The blast furnace process is generally used for the iron ore smelting with the characteristic features of high output with economic viability. The smelting cost of blast furnace is dependent upon the life of blast furnace. During the process, a large amount of molten iron is produced everyday which badly impact on the iron mouth. Therefore, the durability of iron mouth is of concern among the community.
To address the durability of blast furnace iron taps, the clay bricks have been used but erosion of clay bricks also lead to the gas leakage between the iron frame and the combined bricks. Moreover, the gas leakage is formed, due to the scouring effect of the gas flow, the gas passage will show a trend of deterioration. Therefore, the gas leak in the iron mouth area must be treated to ensure that the blast furnace condition is stable and forward and to ensure the safe production of the blast furnace. Generally, tap clay/mud gun have been utilised to plug the metal tapping hole in the blast furnace. The main functions of the mud gun include the following three aspects: (1) blocking iron, requiring good filling and sintering of the mud gun: (2) stabilizing the iron, requiring easy opening and corrosion resistance of the mud gun; (3) To protect the hearth, it requires no cracks when the gun mud is heated quickly, and the bonding strength of the new and old mud gun is high.
At present, there are two main types of mud are available in the market, namely tar-based mud and resin-based mud. Tar is widely used as a binder for sludge because of its low cost and simple production process. Both low and high volatile tar can be used to prepare sludge. When low-softening point tar is selected, the mud can maintain plasticity at room temperature, but because this tar contains a large amount of light oil and naphthalene, its high-temperature strength is low. To solve this problem, a high softening point with little oil content is used. The tar is used to prepare mud, however, this mud is hardened immediately after cooling, which is not conducive to squeezing the mud.
Therefore, the use of this tar system mud has the following limitations: (1) The high-temperature flexural strength of this material is not sufficient to withstand high top pressure operation because of its low β resin content; (2) During the volatilization of volatiles; it must be aimed at the tap hole for a long time before the tap hole mud hardens; (3) tar pitch combined with clay is easy to distribute on the lining of the furnace, so the coke adjacent to the inner end of the tap hole cannot be placed Pushed aside to form a "mushroom-like"; (4) black smoke comes out when the tar evaporates, polluting the environment.
In order to improve the service life of the tap hole and prevent gas leakage, it is necessary to develop a blast furnace tap/mud gun with appropriate binders exhibiting a long life and good fire resistance according to the operating characteristics and erosion characteristics of the blast furnace.
Binders consisting the resin for tap-hole clay must exhibit the characteristics like high plasticity, excellent storage stability, low emissions, controlled cure rate, tight control consistency and cost effectiveness. In this connection, novolaks and resols are frequently used in this application.
EP0332162A2 discloses the Phenol formaldehyde adhesive for bonding wood pieces of high moisture content and composite board and veneers bonded with such adhesive. An adhesive composition intended particularly for use in bonding veneers or wafers of wood having a moisture content greater than 8% said adhesive composition comprising; A: A highly advanced high molecular weight resin prepared by condensing phenol with an excess of formaldehyde in the presence of an alkaline hydroxide catalyst under reflux conditions; B: A resin powder or aqueous dispersion which is a phenol formaldehyde (PF) condensation product partially cross-linked so that the particles swell when added to component A without dissolving; C: A component selected from the group consisting of alkylene carbonates and phenol resorcinol formaldehyde (PRF) resins in an amount between about 1 and 10 weight percent based on the amount of solid resin in components A and B; and D: Optionally borax in the amount of 0 to 3 weight percent based on the amount of solid resin of components A and B.
US4339361A discloses the Phenol-formaldehyde resins extended with carbohydrates for use in binder compositions. Phenol-formaldehyde product and reacting said product with an amide as an extender to form a phenol-formaldehyde-amide resin, the amide compound being selected from the group consisting of urea, dicyandiamide, melamine and mixtures thereof and the sugar being selected from the group consisting of mono- and oligosaccharides and water-soluble polysaccharides.
In order to improve the environment and improve the performance of the mortar, resin-based mortar has been developed. Two resins have been tried out, which are resole phenolic resin and novolac phenolic resin. Resol phenolic resin is thermosetting, the tree refers to The tendency to harden easily when the temperature is just above 25° C limits its use. Novolac resins are thermoplastic and have a high curing initiation temperature, but because of their low wettability, larger amounts are required to achieve the same wetting effect as resole phenolic resins, which in turn accelerates the curing speed. And the faster curing speed makes the adhesion between the refractory of the furnace wall and the gun mud, and between the layers adjacent to the gun mud destroyed, the length of the iron outlet cannot be extended, which is not conducive to extending the iron time.
IN201831041620 discloses the TQ- putty for development and application of chemical compound for arresting gas leakage in blast furnaces. A novel composition for arresting gas leakage at high temperature and pressure condition in Blast furnace comprises Mud Gun Mass, Refractory Dust, two parts epoxy based adhesive, graphite rope, Hydraulic Oil, Glass wool and soap solution.
The present invention discloses the use of phenol resins or phenol-formaldehyde resins obtained by the polymerization of phenol and formaldehyde which possess good physical and chemical properties such as high mechanical strength, low toxicity, good heat resistance, low smoke formation and high thermal stability which provides more stability and long ageing life to the refractories.
Object of the Invention:
The main objective of present invention is to propose phenol-formaldehyde resin for tap hole clay/mud gun mass to plug metal tapping hole in a blast furnace.

Another objective of the present invention is to reduce the generation of flue gas.

Yet another objective of the present invention is to extend the depth of the tap hole and protect the hearth, prolong the tap time, and reduce the number of taps per day.

Yet another objective of the present invention is to provide phenol-formaldehyde resin with high mechanical strength, low toxicity, good heat resistance, low smoke formation and high thermal stability which provides more stability and long ageing life to the refractories.

Yet another objective of the present invention is to provide a chemical composition for resin binder system for tap hole clay/mud gun mass to plug metal tapping hole in a blast furnace for steel to achieve long aging life.
Summary of the Invention:
The present invention relates to the resin binder system for Tap hole clay/Mud Gun mass, which includes phenol formaldehyde resin with blend of different grades of novolac and resole resins which is part A. Part B is life extender and moisture retainer called aging time, as present steel industries need these mass need to remain moisten for more than 24 hours and Part C is catalyst to achieve maximum mechanical and thermal strength and the mass ratio of each component is: Part A: 5% on wt. of grits; Part B: 6-12 % on wt Part-A; Part C: 30-40 % on wt. of Part-A.

The main aspect of the present invention, a resin binder system for mud gun mass for plugging the tap hole of blast furnace to achieve long aging life comprising of:
a) 5 - 6% phenol-formaldehyde resin;
b) 2.5 % glycols mixture as a life extender and moisture retainer characterized by boiling range 200 to 3000C;
c) 1-3 % catalyst; and
d) 70 – 80 % glycol as a solvent.

Detailed Description of the Invention:
The following description relates to a particular manifestation of the present invention. The present invention relates to resin binder system for Tap hole clay/Mud Gun mass which contains the base resin, extender and catalyst for curing and achieve final strength.
The present invention relates to specially developed Resin binder system for Tap hole clay / Mud Gum mass to achieve long aging life of mass. More specifically, it related to Phenolic Resin Binder for Tap hole mass/ Mudgunmass. The phenolic resins or phenol-formaldehyde resins are the synthetic polymers obtained by the polymerization of phenol and formaldehyde. Phenolic resins possess good physical and chemical properties such as high mechanical strength, low toxicity, good heat resistance, low smoke formation and high thermal stability. Different grade of resins developed keeping in view of application in refractory industries who make Tap whole mass/ clay, this is being used to plug metal tapping hole in blast furnace for steel.
The present invention is made up with Phenol formaldehyde resin with blend of different grades of novolac and resole resins, that is part A, out of our 3 part system, Part B is life extender and moisture retainer called aging time, as present steel industries need these mass need to remain moisten for more than 24 hours; and Part C is catalyst to achieve maximum mechanical and thermal strength.
PROLAC 7026 FOR MUDGUNMASS:
Composition:
It comprising of
(1) 32.4% phenol
(2) 21.91% formaldehyde
(3) 0.315% acid catalyst
Process:
- First charge phenol in to reactor then add acid catalyst
- Heat it up to 105 to 110 0 c
- Add formaldehyde slowly
- Reaction is going on, react it for 2 to 3 hours
- After reaction dehydrate it up to 1800 c
- Then add 45.36 % glycols mixture
The present invention relates to system with 3 parts system:
1. Part A: Phenol formaldehyde resin with blend of different grades of novolac and resole resins,
2. Part B: Life extender and moisture retainer (Glycols mixture) called aging time, as present steel industries need these mass need to remain moisten for more than 24 hours.
3. Part C: Catalyst (Acid catalyst) to achieve maximum mechanical and thermal strength.
4. Based on requirement, user can mix this composition with grits as per refractory grits requirement.
According to an embodiment of the present invention, the percentage of different materials used for manufacture of the tap hole/mud gun mass as below:
Materials Percentage
Part A (Phenol formaldehyde Resin) 5 -6%
Part B (Extender) 2.5%
Part C (Catalyst) 1-3%
The main embodiment of the present invention, a resin binder system for mud gun mass for plugging the tap hole of blast furnace to achieve long aging life comprising of:
a) 5 - 6% phenol-formaldehyde resin;
b) 2.5 % glycols mixture as a life extender and moisture retainer characterized by boiling range 200 to 3000C;
c) 1-3 % catalyst; and
d) 70 – 80 % glycol as a solvent.
Another embodiment of the present invention, a phenol-formaldehyde resin contains 32.4% phenol and 21.91% formaldehyde.
Another embodiment of the present invention, Hexamethylene tetra amine of 99% purity is used as catalyst which provides maximum mechanical and thermal strength.
Another embodiment of the present invention, gel time of resin binder system is 45 to 60 secs.
According to an embodiment of the invention, a process for the preparation of tap hole clay/ mud gun mass for plugging the tap hole of blast furnace, the process comprising of:
- Homogenously mix phenol and 50 % oxalic acid in reaction vessel. Then heat it at 98C followed by the slow addition of formaldehyde within 45 minutes to control exothermic reaction.
- Allow reaction to take place till the content of free formaldehyde is less than 0.5 followed by the atmospheric distillation with continues heating up to the temperature 170 C.
- Then atmospheric distillation carried out by heating on and allow to raise the temp to 170 degree, finally solid content is obtained.
- Viscosity of the composition is achieved by adding requisite quantity of solvents in solid content.
- The resultant solid content is tested for the viscosity and suitable solvents are added to achieve optimum viscosity of the product.

The different ingredients used for the manufacture of tap hole mass are described below:
Phenolic Resin (Part A):
Part A is base resin such as Phenolic resins or phenol-formaldehyde resins are the synthetic polymers obtained by the polymerization of phenol and formaldehyde. Phenolic resins possess good physical and chemical properties such as high mechanical strength, low toxicity, good heat resistance, low smoke formation and high thermal stability. The specifications of the resin used during the process are as follows:
Tests Specification Test Method
Viscosity At 250 C 5000 To 14000 Cps ISO 2555
Specific Gravity 1.19 To 1.24 ISO 3675
Free Monomeric Aromatic Group 6 To 8 % By Titration
Silane Content 1% Min Added By Weight
Methyl Content 5 % Max Added By Weight

Resin is basic polymer and its concentration is measure in solid content, the range in the present invention is 50% to 70% depends on user’s requirement.
Life Extender/ Plasticizer (Part B):
Part B is life extender and moisture retainer called aging time as present steel industries need this mass need to remain moisten for more than 24 hours. The Life extender is different type of Glycol based on boiling range 200 to 300 degree Celsius.
Catalyst (Part C):
Part C is catalyst to achieve maximum mechanical and thermal strength. It is used for curing and achieving final strength. Hexamethylene tetra amine of 99% purity is used as catalyst. The specifications of the catalyst used during the process are as follows:
Tests Specification Test Method
Hexa Content 94 % ISO 8988
Sieve Analysis 90% Pass Through 200 Mess IS 460

Solvent:
Solvent is used to achieve the desired viscosity of the product for the application of tap hole clay/mud gun mass for blast furnace. In present invention, Glycol and its 70 to 80% glycol content is used as solvent. The specifications of the solvent used during the process are as follows:
Tests Specification Test Method
Viscosity At 250 C 200 To 300 ISO 2555
Specific gravity 1.17 To 1.2 ISO 3675
Boiling 264 To 2660 C

The present invention described with reference to following example without restricting the scope of the invention.
Example 1:
The new tap hole/mud gun mass includes the following components and the mass ratio of each component is: Part A: 5% on wt. of grits; Part B: 6-12 % on wt Part-A; Part C: 30-40 % on wt. of Part-A. The above-mentioned blasting mud adopts the following preparation method: 32.4 % phenol is charged in reactor followed by the addition of 0.315 % of acid catalyst at the temperature of 105 to 110 C. Then, 21.90 % of formaldehyde is added slowly and allowed reaction to take place for 2 to 3 hrs followed by the dehydration at 180 C. Then, 45.36 % glycols as a solvent are added to attain the desirable viscosity of the product.
The present composition further evaluated for Viscosity (CPS), Solid content (%), PH, Gel time (sec). The gel time is 45 to 60 secs.

The present invention comprising of 94% of Phenol, 37% of Formaldehyde, Acid is 99 % pure, Glycols are having different boiling range from 200 to 300 degree and in combination of Mono, di, tri form. The acid catalysts are selected from 99% pure Oxalic acid, 40 % Hydrochloric acid. , Claims:We claim,
1. A resin binder system for mud gun mass for plugging the tap hole of blast furnace to achieve long aging life comprising of:
a) 5 - 6% phenol-formaldehyde resin;
b) 2.5 % glycols mixture as a life extender and moisture retainer characterized by boiling range 200 to 300C;
c) 1-3 % catalyst; and
d) 70 – 80 % glycol as a solvent.
2. The resin binder system as claimed in claim 1, wherein phenol-formaldehyde resin contains 32.4% phenol and 21.91% formaldehyde.
3. The resin binder system as claimed in claim 1, wherein Hexamethylene tetra amine of 99% purity is used as catalyst which provides maximum mechanical and thermal strength.
4. The resin binder system as claimed in claim 1, wherein gel time of resin binder system is 45 to 60 secs.
5. A process for the preparation of mud gun mass for plugging the tap hole of blast furnace comprising of:
a) Mix phenol and 50 % oxalic acid in reaction vessel, then heat it at 98C followed by the slow addition of formaldehyde within 45 minutes to control exothermic reaction;
b) Allow reaction to take place till the content of free formaldehyde is less than 0.5 followed by the atmospheric distillation with continues heating up to the temperature 170 C;
c) Atmospheric distillation carried out by heating on and allow to raise the temp to 170 degree, finally solid content is obtained; and
d) The resultant solid content is tested for the viscosity and requisite quantity of solvents are added to achieve optimum viscosity of the product.  
Dated 24th Aug, 2022

Chothani Pritibahen Bipinbhai
Reg. No.: IN/PA-3148
For and on behalf of the applicant