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A Process For Fiber Extraction From Pine Needles (Perul)

Abstract: This invention relates to a process for extraction of textile fibers from pine needles comprises steps of:- - conditioning of pine fibers, - treatment of conditioned pine fibers with Alkali, - treatment with metallic salt, - decorortication of metallic salt treated pine fibers, - bleaching and drying.

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Patent Information

Application #
Filing Date
18 January 2017
Publication Number
29/2018
Publication Type
INA
Invention Field
TEXTILE
Status
Email
lsdavar@ndf.vsnl.net.in
Parent Application
Patent Number
Legal Status
Grant Date
2021-01-12
Renewal Date

Applicants

1. Northern India Textile Research Association
Sector-23, Raj Nagar, Ghaziabad, Uttar Pradesh-201 002, India.
2. Ethnic Attire India Pvt. Ltd.
Noida, U.P., India.

Inventors

1. Shweta Chauhan
Northern India Textile Research Association, Sector-23, Raj Nagar, Ghaziabad, Uttar Pradesh-201 002, India.
2. Arindam Basu
Northern India Textile Research Association, Sector-23, Raj Nagar, Ghaziabad, Uttar Pradesh-201 002, India.
3. Ajay Tamta
Ministry of Textiles, Government of India, Udyog Bhavan, New Delhi, India

Specification

FIELD OF INVENTION
[001] This invention relates to a process for fiber extraction from Pine Needles (Perul). The same involves low temperature and low alkali fiber extraction followed by silica removal together with provisions for softening of fibers.

BACKGROUND/PRIOR ART
[002] A plant fiber forms a fiber extracted from stem, leaf of plant and can be also produced by plant as protecting seed hairs.

[003] In existing extraction process pine fiber is extracted from leaf of pine tree that is also called as pine needle or ‘perul’. Fiber extraction is carried out by cooking the needles.

[004] Cooking constitutes a process in which pine leaves are treated with certain chemicals at boiling temperature.

[005] Further the extraction processes are accompanied by manual/machine decortications of boiled pine needles. The chemicals that are used in extraction are generally alkali or salt, which are used at boiling or elevated temperature.

[006] In order to impart clean look the process is generally accompanied by bleaching. The bleaching can be done by any of the available method like hypochlorite bleaching or peroxide bleaching etc. However, the fibers produced are short and coarse.

[007] Now, reference may be made to the following publications.

[008] US397240A:- This talks about extraction of pine fiber by treatment with alkali followed by soaking in water, wherein material must be treated at 212 Fahrenheit. Here, variable size fibers can be obtained.

[009] US409608:- According to this process, the needles or pine-straw not only has the effect of dissecting the fiber vascular bundles, but the contour of the fibrils are also altered. By the constant circulation of the alkaline solution and subsequent washings with water, the pores or cells are thoroughly permeated, a great deal of foreign matter is driven out, and the place of the old natural constituents is taken by the new chemical compounds. By the decorticating process a great deal of organic matter is rubbed out and the teeth of the cards are enabled to readily take hold of the mass to finally remove all foreign and objectionable matter and to effect the shredding of the leaves, which may be done to a greater or less degree to produce‘ a fiber of ‘fine or coarser grade, as desired.

[0010] US437555:- In this patent pine needles are treated with warm or hot alkali. After alkali treatment needles are passed between pressure rolls. Pressure applications are followed by washing, wherein pressures are applied to loosen the silica.

[0011] All the aforesaid researches deal with extraction of fiber at higher temperature and at higher concentration of alkali. Also none of research process utilize chemical process for complete removal of silica. Silica removal is necessary as it is the constituent in the fiber that is majorly responsible for brittleness.

[0012] Also in the currently available technologies, there are no provisions to achieve softness and for textile processes flexibility is required because stiffness leads to breakages during fiber processing in different textile process.

[0013] In view of the above, it is required to devise a novel fiber extraction process which can address various issues of the prior art(s) and also serve the purpose efficiently.

OBJECTS OF THE INVENTION
[0014] The principal object of the present invention is to provide a process for fiber extraction which obviates shortcomings of prior art(s).

[0015] Another object of the present invention is to provide a process for fiber extraction which is low alkali and low temperature process.

[0016] Still another object of the present invention is to provide a process for fiber extraction which involves complete removal of silica.

[0017] Yet another object of the present invention is to provide a process for fiber extraction which leads to production of soft fibers.

SUMMARY OF THE INVENTION

[0018] According to this invention there is provided a process for extraction of textile fibers from pine needles comprises steps of:- conditioning of pine fibers, - treatment of conditioned pine fibers with Alkali, - treatment with metallic salt, -decortications of metallic salt treated pine fibers, - bleaching and drying.

[0019] The pine fibers are conditioned at 27 + 2°C and 65% + 5 Relative Humidity.

[0020] Said treatment of conditioned pine fibers carried out with alkali for 30 minutes to 10 hours, in which the alkali (base) includes LiOH, NaOH, KOH, RbOH, CsOH, (MgOH)2, Ca(OH)2, stanic hydroxide, Cr(OH)2, Barium Hydroxide or Ba(OH)2, concentration of which varies from 0.5 to 5%.

[0021] The treatment with metallic salt is conducted for 30 minutes to 10 hours having concentration of 0.5 to 5%, in which the metallic salt comprises NaCl, MgCl2, CuCL2, KCl, AlCl3 orFeCl2.

[0022] The treated pine fibers undergoes decorortication followed by washing.

[0023] The washing is done by means of distilled water.

[0024] The bleaching is conducted by Hydrogen Peroxide (H2O2) having concentration of 1-2 grams per litre together with 0.5-2 grams per litre NaoH and 0.25-1 grams per litre peroxide stabilizer.

[0025] The drying is carried out for example at 120°C for about 20 minutes to extract fiber.

BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING

[0026] Further objects and advantages of this invention will be more apparent from the ensuing description when read in conjunction with the accompanying drawings of the exemplary embodiment and wherein:

Fig.1 shows: Flow diagram of a process for extraction of textile fibers from pine needles according to present invention.

DETAIL DESCRIPTION OF THE PRESENT INVENTION WITH REFERENCE TO THE ACCOMPANYING DRAWING

[0027] The present invention makes a disclosure regarding a technology pertaining to a process for extraction of textile fibers from pine needles.

[0028] According to this invention, there is provided a process for fiber extraction from pine needles comprising steps of sorting of pine needles, pine fibers conditioning, dual chemical treatment, decortication, washing, bleaching, drying of fibers followed by softening and fiber extraction as illustrated in the accompanying figure 1.

[0029] The above is associated with low temperature and low alkali fiber extraction process followed by silica removal resulting in softening of fibers.

[0030] Now, the process can be detailed out as follows:-

[0031] The pine needles collected from uttarakhand region of India are subjected to conditioning at 27+2°C and 65%+5°C Relative Humidity. Thereafter, the conditioned pine fiber thus obtained is treated with cold alkali for 30 minutes to 10 hours, wherein the alkali (base) includes LiOH, NaOH, KOH, RbOH, CsOH, (MgOH)2, Ca(OH)2, stanic hydroxide, Cr(OH)2, Barium Hydroxide or Ba(OH)2, concentration of which varies from 0.5 to 5%.

[0032] The above treated pine fiber is further subjected to treatment with metallic salt for 30 minutes to 10 hours having concentration of 0.5 to 5%. The metallic salt comprises NaCl, MgCl2, CuCL2, KCl, AlCl3 orFeCl2.

[0033] Here, the metallic salt has silica removal action, which decreases harshness. This leads to softening of fibers. Thus, loosening of lignin and silica removal is carried out by the aforesaid chemical processes.

[0034] The finally treated pine fibers undergoes decortication manually or by a machine. The decorticated fibers are then washed by means of distilled water.

[0035] The washing is followed by bleaching and drying. The bleaching is conducted by Hydrogen Peroxide (H2O2) having concentration of 1-2 grams per litre together with 0.5-2 grams per litre NaoH and 0.25-1 grams per litre peroxide stabilizer for nearly 15 minutes. The bleached pine fibers thus obtained are dried in a drying chamber for example at 120°C for about 20 minutes to extract fiber.

[0036] The devised process of invention results in production of soft fibers facilitating the process. Softening is achieved by means of oil in water emulsion method.

[0037] The temperature is near to room temperature and said alkali is in the range of 0-8%.

[0038] The silica removal is accomplished at low concentration of chemical for complete removal thereof.

[0039] Out of the whole experiment, significant results are indicted in the following table.
(ii) Testing Parameters

a) Tensile strength and elongation

Data Pine Needle experiment
sample size= 5 grms All testings done 27±5°C

Serial no Formulation 1 Formulation 2 Strength
gm/tex Strength Elon
Gation (uni t??)
concentration in gpl Time (hrs) concentration gpl Time (hrs)
1 3 4 3 4 5.47 6.17 6
2 3 4 3 3 5 5.5 6
3 3 4 3 2 4.6 5.06 7
4 3 6 3 6 4.42 4.862 8
5 3 6 3 4 4.7 5.17 7
6 3 6 3 2 4.45 4.895 6
7 2 4 2 4 4.44 4.884 9
8 2 4 2 3 3.58 3.938 8
9 2 4 2 2 4.09 4.499 11
10 2 6 2 6 4.65 5.115 8
11 2 6 2 4 4.6 5.06 7
12 2 6 2 2 5.32 5.852 9
13 3 6 0 0 4.4 4.84 9

[0040] Bundle strength were determined by IS 3675. Properties found on different concentration are given in table. Best result was found on 3 grams per litre of both the agents. The time period for both the treatment was found to be 4 hours.

b) Moisture Regain:-
Moisture regain of fiber were checked by IS 199.The moisture regain were found to be 11%.
c) Fiber Length Range:-

Fiber length of the experimental fibers were found in the range of 3-8 cm
d) Anti-Microbial Property
Anti-microbial testing was carried out on extracted samples. The results
Showed fiber possessing anti-microbial activity.
e) Average fiber Fineness
Average fiber fineness was calculated as per ASTMD 1448.
The value was found to be 88.56 micron.
f) Crystallinity

The fibers were tested for crystallinity and orientation by X-Ray Diffractogram. The fibers were found to have 61.76 percent crystalline. The Average crystallite size was found to be 22.52 ºA

g) SEM analysis
Sample was also analysed for surface characteristics by Scan Electron Microscope. Samples were found with some internal cavities and outer surface have some irregularspace.
Working Example:
[0041] For the process of fiber extraction from pine needles, the pine needles are sorted, which are conditioned at 28°C and 65% Relative Humidity. The conditioned pine fibers are treated with LioH for 4 hours having concentration of 3%.

[0042] Thereafter, it undergoes treatment with Mgcl2 for 4 hours, in which magnesium chloride has concentration of 3%. Then the pine fibers thus obtained are decororticated, which are washed with the help of distilled water. Then, the clean fibers are subjected to bleaching wherein the bleaching is conducted by Hydrogen peroxide (H2O2) having concentration of 2 grams per litre together with 2 grams per litre NaoH and 0.25 grams per litre peroxide stabilizer for 15 minutes.

[0043] Eventually, the bleached pine fibers are dried at 120°C for 20 minutes to extract fibers.

[0044] Although exemplary embodiments of the present invention have been described in detail herein above, it should be clearly understood that many variations and modifications of the basic inventive concepts herein taught which may appear to those skilled in the present art will still fall within the spirit and scope of the present invention, as defined in the appended claims.

WE CLAIM:
1. A process for extraction of textile fibers from pine needles comprises steps of:-
- conditioning of pine fibers,
- treatment of conditioned pine fibers with Alkali,
- treatment with metallic salt,
- decorortication of metallic salt treated pine fibers,
- bleaching and drying.

2. A process for extraction of textile fibers from pine needles as claimed in claim 1 wherein the pine fibers are conditioned at 27 + 2°C and 65% + 5 Relative Humidity.

3. A process for extraction of textile fibers from pine needles as claimed in claim 1 or 2 wherein said treatment of conditioned pine fibers is carried out with alkali for 30 minutes to 10 hours, in which the alkali (base) includes LiOH, NaOH, KOH, RbOH, CsOH, (MgOH)2, Ca(OH)2, stanic hydroxide, Cr(OH)2, Barium Hydroxide or Ba(OH)2, concentration of which varies from 0.5 to 5%.

4. A process for extraction of textile fibers from pine needles as claimed in any of the preceding claims wherein the treatment with metallic salt is conducted for 30 minutes to 10 hours having concentration of 0.5 to 5%, in which the metallic salt comprises NaCl, MgCl2, CuCL2, KCl, AlCl3 orFeCl2.
5. A process for extraction of textile fibers from pine needles as claimed in any of the preceding claims wherein the treated pine fibers undergoes decorortication followed by washing.

6. A process for extraction of textile fibers from pine needles as claimed in claim 5 wherein the washing is done by means of distilled water.

7. A process for extraction of textile fibers from pine needles as claimed in any of the preceding claims wherein the bleaching is conducted by Hydrogen Peroxide (H2O2) having concentration of 1-2 grams per litre together with 0.5-2 grams per litre NaoH and 0.25-1 grams per litre peroxide stabilizer.

8. A process for extraction of textile fibers from pine needles as claimed in any of the preceding claims wherein the drying is carried out for example at 120°C for about 20 minutes to extract fiber.

Documents

Application Documents

# Name Date
1 201711001977- Certificate of Inventorship-011000143( 27-01-2025 ).pdf 2025-01-27
1 201711001977-Annexure [10-01-2025(online)].pdf 2025-01-10
1 Form 3 [18-01-2017(online)].pdf 2017-01-18
2 201711001977-Annexure [10-01-2025(online)].pdf 2025-01-10
2 201711001977-Response to office action [10-01-2025(online)].pdf 2025-01-10
2 Drawing [18-01-2017(online)].pdf 2017-01-18
3 201711001977-FORM 8A [23-04-2024(online)].pdf 2024-04-23
3 201711001977-Response to office action [10-01-2025(online)].pdf 2025-01-10
3 Description(Provisional) [18-01-2017(online)].pdf 2017-01-18
4 Other Patent Document [20-05-2017(online)].pdf 2017-05-20
4 201711001977-RELEVANT DOCUMENTS [23-08-2022(online)].pdf 2022-08-23
4 201711001977-FORM 8A [23-04-2024(online)].pdf 2024-04-23
5 201711001977-RELEVANT DOCUMENTS [23-09-2021(online)].pdf 2021-09-23
5 201711001977-RELEVANT DOCUMENTS [23-08-2022(online)].pdf 2022-08-23
5 201711001977-OTHERS-230517.pdf 2017-05-25
6 201711001977-RELEVANT DOCUMENTS [23-09-2021(online)].pdf 2021-09-23
6 201711001977-IntimationOfGrant12-01-2021.pdf 2021-01-12
6 201711001977-Correspondence-230517.pdf 2017-05-25
7 Form 26 [30-05-2017(online)].pdf 2017-05-30
7 201711001977-PatentCertificate12-01-2021.pdf 2021-01-12
7 201711001977-IntimationOfGrant12-01-2021.pdf 2021-01-12
8 201711001977-CLAIMS [01-12-2020(online)].pdf 2020-12-01
8 201711001977-PatentCertificate12-01-2021.pdf 2021-01-12
8 201711001977-Power of Attorney-060617.pdf 2017-06-16
9 201711001977-CLAIMS [01-12-2020(online)].pdf 2020-12-01
9 201711001977-Correspondence-060617.pdf 2017-06-16
9 201711001977-FER_SER_REPLY [01-12-2020(online)].pdf 2020-12-01
10 201711001977-FER_SER_REPLY [01-12-2020(online)].pdf 2020-12-01
10 201711001977-FORM 3 [01-12-2020(online)].pdf 2020-12-01
10 201711001977-FORM 3 [17-01-2018(online)].pdf 2018-01-17
11 201711001977-ENDORSEMENT BY INVENTORS [17-01-2018(online)].pdf 2018-01-17
11 201711001977-FER.pdf 2020-06-03
11 201711001977-FORM 3 [01-12-2020(online)].pdf 2020-12-01
12 201711001977-DRAWING [17-01-2018(online)].pdf 2018-01-17
12 201711001977-FER.pdf 2020-06-03
12 201711001977-FORM 18 [31-05-2018(online)].pdf 2018-05-31
13 201711001977-FORM 18 [31-05-2018(online)].pdf 2018-05-31
13 201711001977-CORRESPONDENCE-OTHERS [17-01-2018(online)].pdf 2018-01-17
13 201711001977-COMPLETE SPECIFICATION [17-01-2018(online)].pdf 2018-01-17
14 201711001977-COMPLETE SPECIFICATION [17-01-2018(online)].pdf 2018-01-17
14 201711001977-CORRESPONDENCE-OTHERS [17-01-2018(online)].pdf 2018-01-17
15 201711001977-CORRESPONDENCE-OTHERS [17-01-2018(online)].pdf 2018-01-17
15 201711001977-DRAWING [17-01-2018(online)].pdf 2018-01-17
15 201711001977-FORM 18 [31-05-2018(online)].pdf 2018-05-31
16 201711001977-DRAWING [17-01-2018(online)].pdf 2018-01-17
16 201711001977-ENDORSEMENT BY INVENTORS [17-01-2018(online)].pdf 2018-01-17
16 201711001977-FER.pdf 2020-06-03
17 201711001977-FORM 3 [01-12-2020(online)].pdf 2020-12-01
17 201711001977-FORM 3 [17-01-2018(online)].pdf 2018-01-17
17 201711001977-ENDORSEMENT BY INVENTORS [17-01-2018(online)].pdf 2018-01-17
18 201711001977-FER_SER_REPLY [01-12-2020(online)].pdf 2020-12-01
18 201711001977-FORM 3 [17-01-2018(online)].pdf 2018-01-17
18 201711001977-Correspondence-060617.pdf 2017-06-16
19 201711001977-CLAIMS [01-12-2020(online)].pdf 2020-12-01
19 201711001977-Correspondence-060617.pdf 2017-06-16
19 201711001977-Power of Attorney-060617.pdf 2017-06-16
20 201711001977-PatentCertificate12-01-2021.pdf 2021-01-12
20 201711001977-Power of Attorney-060617.pdf 2017-06-16
20 Form 26 [30-05-2017(online)].pdf 2017-05-30
21 201711001977-Correspondence-230517.pdf 2017-05-25
21 201711001977-IntimationOfGrant12-01-2021.pdf 2021-01-12
21 Form 26 [30-05-2017(online)].pdf 2017-05-30
22 201711001977-Correspondence-230517.pdf 2017-05-25
22 201711001977-OTHERS-230517.pdf 2017-05-25
22 201711001977-RELEVANT DOCUMENTS [23-09-2021(online)].pdf 2021-09-23
23 201711001977-OTHERS-230517.pdf 2017-05-25
23 201711001977-RELEVANT DOCUMENTS [23-08-2022(online)].pdf 2022-08-23
23 Other Patent Document [20-05-2017(online)].pdf 2017-05-20
24 201711001977-Response to office action [10-01-2025(online)].pdf 2025-01-10
24 Description(Provisional) [18-01-2017(online)].pdf 2017-01-18
24 Other Patent Document [20-05-2017(online)].pdf 2017-05-20
25 Drawing [18-01-2017(online)].pdf 2017-01-18
25 Description(Provisional) [18-01-2017(online)].pdf 2017-01-18
25 201711001977-Annexure [10-01-2025(online)].pdf 2025-01-10
26 Form 3 [18-01-2017(online)].pdf 2017-01-18
26 Drawing [18-01-2017(online)].pdf 2017-01-18
26 201711001977- Certificate of Inventorship-011000143( 27-01-2025 ).pdf 2025-01-27
27 Form 3 [18-01-2017(online)].pdf 2017-01-18

Search Strategy

1 searchstrategyE_18-05-2020.pdf

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