CN110820333A - Preparation method for improving tussah silk fiber strength - Google Patents
Preparation method for improving tussah silk fiber strength Download PDFInfo
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- CN110820333A CN110820333A CN201911134697.0A CN201911134697A CN110820333A CN 110820333 A CN110820333 A CN 110820333A CN 201911134697 A CN201911134697 A CN 201911134697A CN 110820333 A CN110820333 A CN 110820333A
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- 239000000835 fiber Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 52
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000661 sodium alginate Substances 0.000 claims abstract description 48
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 48
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 48
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000008014 freezing Effects 0.000 claims abstract description 21
- 238000007710 freezing Methods 0.000 claims abstract description 21
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000010257 thawing Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000001110 calcium chloride Substances 0.000 claims description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 6
- 230000000052 comparative effect Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 108010013296 Sericins Proteins 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001891 gel spinning Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/13—Alginic acid or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/02—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fibres, slivers or rovings
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a preparation method for improving the tussah silk fiber strength, which comprises the following steps: (1) adding sodium alginate into water, and carrying out ultrasonic crushing to obtain a sodium alginate aqueous solution; (2) washing the degummed and bleached tussah silk with water, freezing, vacuumizing and drying; (3) soaking the tussah silk treated in the step (2) into the sodium alginate aqueous solution in the step (1), keeping the temperature of the solution at 70-90 ℃, and stirring for 40-50 min; (4) putting the tussah silk sodium alginate aqueous solution obtained in the step (3) into a sealed tank, increasing the pressure to 0.8-1.0MPa, increasing the temperature to 90-100 ℃, keeping high-temperature and high-pressure treatment for 30-90 s, then removing the high pressure, and washing with water; (5) and (4) soaking the tussah silk treated in the step (4) in an aqueous solution containing a cross-linking agent, taking out the tussah silk, freezing and thawing for multiple times, and finally drying. The invention reserves the original fiber structure of the tussah silk and obviously improves the breaking strength of the tussah silk.
Description
Technical Field
The invention relates to the technical field of tussah silk processing, in particular to a preparation method for improving tussah silk fiber strength.
Background
The tussah silk is at the in-process that comes unstuck, causes the change of silk structure easily to make mechanical properties reduce, current method of improving the fiber strength of tussah silk adopts to smash the tussah silk and dissolves, then mixes with other solution materials and carries out the spinning and obtain the silk fibre, smash the dissolution with the tussah silk earlier, destroys the existing fiber structure of tussah silk easily, influences the fibrous mechanical strength of silk.
CN102011212B discloses a preparation method of tussah silk cellulose fiber, which comprises the steps of degumming and crushing tussah silk, adding the crushed tussah silk into ionic liquid, performing microwave treatment to obtain tussah silk ionic liquid solution, adding the same crushed cellulose, uniformly stirring to obtain tussah silk spinning solution, and finally spinning, wherein the dry fracture strength of the obtained fiber is 1.03-1.90cN/dtex, which is lower than the original fracture strength of the tussah silk.
Disclosure of Invention
The invention provides a preparation method for improving the tussah silk fiber strength, which reserves the original fiber structure of the tussah silk and obviously improves the breaking strength of the tussah silk.
The technical scheme of the invention is realized as follows: a preparation method for improving the strength of tussah silk fiber comprises the following steps:
(1) adding 0.3-0.8 part by weight of sodium alginate into 100 parts by weight of water, and performing ultrasonic crushing, wherein the temperature of the water is kept at 80-90 ℃ to obtain a sodium alginate aqueous solution;
(2) washing the degummed and bleached tussah silk with water, freezing, vacuumizing and drying;
(3) soaking the tussah silk treated in the step (2) into the sodium alginate aqueous solution in the step (1), keeping the temperature of the solution at 70-90 ℃, and stirring for 40-50min, wherein the weight part of the tussah silk is 7-9;
(4) putting the tussah silk sodium alginate aqueous solution obtained in the step (3) into a sealed tank, increasing the pressure to 0.8-1.0MPa, increasing the temperature to 90-100 ℃, keeping high-temperature and high-pressure treatment for 30-90 s, then removing the high pressure, taking out the tussah silk, washing the tussah silk in the aqueous solution at 80-90 ℃, and cleaning the sodium alginate adhered to the surface of the tussah silk;
(5) and (4) putting the tussah silk treated in the step (4) into an aqueous solution containing a cross-linking agent, soaking for 15-30min, taking out the tussah silk, freezing and thawing for multiple times, and finally drying.
Further, in the step (5), tussah silk is frozen for 3-4h at the temperature of below 0 ℃, then taken out and soaked in an aqueous solution containing a cross-linking agent, unfrozen for 3-4h at room temperature, and the freezing and unfreezing are repeated for 3 times.
Further, the ultrasonic frequency of the ultrasonic crushing in the step (1) is 20-25KHz, and the time is 20-30 min.
Further, the crosslinking agent adopted in the step (5) is CaCl2The concentration of the cross-linking agent aqueous solution is 0.1-0.5 wt%; the weight ratio of the tussah silk to the cross-linking agent aqueous solution is 6-8: 20.
The invention has the beneficial effects that:
the preparation method of the invention retains the original fiber structure of the tussah silk, obviously improves the breaking strength of the tussah silk, and improves the breaking strength by 34.92 to 46.44 percent; the tussah silk is frozen, vacuumized and dried to form a bulky microporous structure, the sodium alginate is favorably introduced into the microporous structure of the tussah silk in cooperation with the ultrasonic crushing treatment of the sodium alginate, and the subsequent high-temperature and high-pressure treatment is favorably carried out in cooperation, so that the sodium alginate is favorably further infiltrated into the tussah silk, the subsequent sodium alginate is favorably linked with sericin in the tussah silk under the action of a cross-linking agent, and the breaking strength of the tussah silk is improved; after the high-temperature and high-pressure treatment, washing the residual sodium alginate on the surface of the tussah silk, and then adding a cross-linking agent to prevent the sodium alginate from forming a covering film on the surface of the tussah silk to influence the appearance of the tussah silk; and the repeated freezing and thawing are also used for improving the crosslinking degree of the sodium alginate and the sericin, and are beneficial to improving the mechanical property of the tussah silk.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example one
A preparation method for improving the strength of tussah silk fiber comprises the following steps:
(1) adding 0.3 weight part of sodium alginate into 100 weight parts of water, and performing ultrasonic crushing at 80-90 deg.C for 20-30min at ultrasonic frequency of 20-25KHz to obtain sodium alginate aqueous solution;
(2) washing degummed and bleached tussah silk with water, freezing at-4 ℃ for 5 hours, and then vacuumizing and drying;
(3) soaking the tussah silk treated in the step (2) into the sodium alginate aqueous solution in the step (1), keeping the temperature of the solution at 70 ℃, and stirring for 40-50min, wherein the weight part of the tussah silk is 7;
(4) putting the tussah silk sodium alginate aqueous solution obtained in the step (3) into a sealed tank, raising the pressure to 0.8MPa, raising the temperature to 90 ℃, keeping high-temperature and high-pressure treatment for 30s, then removing high pressure, taking out tussah silk, washing in the aqueous solution at 80-90 ℃, and cleaning the sodium alginate adhered to the surface of the tussah silk;
(5) soaking the tussah silk treated in the step (4) in an aqueous solution containing a cross-linking agent for 15min, wherein the cross-linking agent is CaCl2The concentration of the aqueous solution of the crosslinking agent was 0.1 wt%; the weight ratio of the tussah silk to the cross-linking agent aqueous solution is 6: 20; then freezing tussah silk at-4 deg.C for 3-4 hr, taking out, soaking in water solution containing cross-linking agent, thawing at room temperature for 3-4 hr, repeating freezing and thawing for 3 times, and dryingAnd (5) drying.
Example two
A preparation method for improving the strength of tussah silk fiber comprises the following steps:
(1) adding 0.5 weight part of sodium alginate into 100 weight parts of water, and performing ultrasonic crushing at 80-90 deg.C for 20-30min at ultrasonic frequency of 20-25KHz to obtain sodium alginate aqueous solution;
(2) washing degummed and bleached tussah silk with water, freezing at-4 ℃ for 5 hours, and then vacuumizing and drying;
(3) soaking the tussah silk treated in the step (2) into the sodium alginate aqueous solution in the step (1), keeping the temperature of the solution at 75 ℃, and stirring for 40-50min, wherein the weight part of the tussah silk is 7;
(4) putting the tussah silk sodium alginate aqueous solution obtained in the step (3) into a sealed tank, raising the pressure to 0.8MPa, raising the temperature to 95 ℃, keeping high-temperature and high-pressure treatment for 50s, then removing high pressure, taking out tussah silk, washing in the aqueous solution at 80-90 ℃, and cleaning the sodium alginate adhered to the surface of the tussah silk;
(5) soaking the tussah silk treated in the step (4) in an aqueous solution containing a cross-linking agent for 20min, wherein the cross-linking agent is CaCl2The concentration of the aqueous solution of the crosslinking agent was 0.3 wt%; the weight ratio of the tussah silk to the cross-linking agent aqueous solution is 6: 20; then taking out tussah silk, freezing at-4 deg.C for 3-4 hr, taking out, soaking in water solution containing cross-linking agent, thawing at room temperature for 3-4 hr, repeating freezing and thawing for 3 times, and drying.
EXAMPLE III
A preparation method for improving the strength of tussah silk fiber comprises the following steps:
(1) adding 0.6 weight part of sodium alginate into 100 weight parts of water, and performing ultrasonic crushing at 80-90 deg.C for 20-30min at ultrasonic frequency of 20-25KHz to obtain sodium alginate aqueous solution;
(2) washing degummed and bleached tussah silk with water, freezing at-4 ℃ for 5 hours, and then vacuumizing and drying;
(3) soaking the tussah silk treated in the step (2) into the sodium alginate aqueous solution in the step (1), keeping the temperature of the solution at 80 ℃, and stirring for 40-50min, wherein the weight part of the tussah silk is 8;
(4) putting the tussah silk sodium alginate aqueous solution obtained in the step (3) into a sealed tank, raising the pressure to 0.9MPa, raising the temperature to 95 ℃, keeping high-temperature and high-pressure treatment for 70s, then removing high pressure, taking out tussah silk, washing in the aqueous solution at 80-90 ℃, and cleaning the sodium alginate adhered to the surface of the tussah silk;
(5) soaking the tussah silk treated in the step (4) in an aqueous solution containing a cross-linking agent for 25min, wherein the cross-linking agent is CaCl2The concentration of the aqueous solution of the crosslinking agent was 0.4 wt%; the weight ratio of the tussah silk to the cross-linking agent aqueous solution is 7: 20; then taking out tussah silk, freezing at-4 deg.C for 3-4 hr, taking out, soaking in water solution containing cross-linking agent, thawing at room temperature for 3-4 hr, repeating freezing and thawing for 3 times, and drying.
Example four
A preparation method for improving the strength of tussah silk fiber comprises the following steps:
(1) adding 0.8 part by weight of sodium alginate into 100 parts by weight of water, and carrying out ultrasonic crushing, wherein the temperature of the water is 80-90 ℃, the ultrasonic frequency of the ultrasonic crushing is 20-25KHz, and the time is 20-30min, so as to obtain a sodium alginate aqueous solution;
(2) washing degummed and bleached tussah silk with water, freezing at-4 ℃ for 5 hours, and then vacuumizing and drying;
(3) soaking the tussah silk treated in the step (2) into the sodium alginate aqueous solution in the step (1), keeping the temperature of the solution at 90 ℃, and stirring for 40-50min, wherein the weight part of the tussah silk is 9;
(4) putting the tussah silk sodium alginate aqueous solution obtained in the step (3) into a sealed tank, raising the pressure to 1.0MPa, raising the temperature to 100 ℃, keeping high-temperature and high-pressure treatment for 90s, then removing high pressure, taking out tussah silk, washing in the aqueous solution at 80-90 ℃, and cleaning the sodium alginate adhered to the surface of the tussah silk;
(5) putting the tussah silk treated in the step (4) into a cross-containing bagSoaking in aqueous solution of coupling agent for 30min, wherein the crosslinking agent is CaCl2The concentration of the aqueous solution of the crosslinking agent was 0.5 wt%; the weight ratio of the tussah silk to the cross-linking agent aqueous solution is 8: 20; then taking out tussah silk, freezing at-4 deg.C for 3-4 hr, taking out, soaking in water solution containing cross-linking agent, thawing at room temperature for 3-4 hr, repeating freezing and thawing for 3 times, and drying.
Comparative example 1
This embodiment is substantially the same as the first embodiment, except that: in the step (1), sodium alginate is replaced by equal weight parts of water.
Comparative example No. two
This embodiment is substantially the same as the first embodiment, except that: and (3) crushing and dissolving the tussah silk treated in the step (2) in the sodium alginate aqueous solution in the step (1), then performing the step (3) and the step (4), and spinning the tussah silk sodium alginate solution by adopting a conventional dry-wet spinning process after removing high pressure in the step (4).
Comparative example No. three
This embodiment is substantially the same as the first embodiment, except that: removing the high-temperature high-pressure treatment in the step (4), taking the tussah silk treated in the step (3) out of the sodium alginate aqueous solution, washing the tussah silk in the aqueous solution at the temperature of 80-90 ℃, and cleaning the sodium alginate adhered to the surface of the tussah silk.
The fracture strength method of the silk is adopted to carry out the mechanical property test on the first to fourth examples and the first to third comparative examples by the GB/T1798-2008 raw silk test method, and the test results are as follows:
as can be seen from the table above, the fracture strength of the tussah silk after degumming and bleaching is low, the fracture strength of the tussah silk can be obviously improved by adopting the preparation method disclosed by the invention, and the fracture strength is improved by 34.92-46.44%; according to the comparative example I and the example I, the addition of the sodium alginate is beneficial to obviously improving the breaking strength of the tussah silk, and according to the comparative example II and the example I, the tussah silk is crushed and dissolved and then is re-spun, so that the breaking strength of the prepared silk is reduced; as can be seen from the third comparative example and the first example, the breaking strength of the tussah silk is slightly improved but the improvement effect is limited if the aqueous solution of the sodium alginate of the tussah silk obtained in the step (3) is not treated at high temperature and high pressure.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. The preparation method for improving the strength of the tussah silk fiber is characterized by comprising the following steps:
(1) adding 0.3-0.8 part by weight of sodium alginate into 100 parts by weight of water, and carrying out ultrasonic crushing, wherein the temperature of the water is kept at 80-90 ℃ to obtain a sodium alginate aqueous solution;
(2) washing the degummed and bleached tussah silk with water, freezing, vacuumizing and drying;
(3) soaking the tussah silk treated in the step (2) in the sodium alginate aqueous solution in the step (1), keeping the temperature of the solution at 70-90 ℃, and stirring for 40-50min, wherein the weight part of the tussah silk is 7-9;
(4) putting the tussah silk sodium alginate aqueous solution obtained in the step (3) into a sealed tank, increasing the pressure to 0.8-1.0MPa, increasing the temperature to 90-100 ℃, keeping high-temperature and high-pressure treatment for 30-90 s, then removing the high pressure, taking out the tussah silk, washing the tussah silk in the aqueous solution at 80-90 ℃, and cleaning the sodium alginate adhered to the surface of the tussah silk;
(5) and (4) putting the tussah silk treated in the step (4) into an aqueous solution containing a cross-linking agent, soaking for 15-30min, taking out the tussah silk, freezing and thawing for multiple times, and finally drying.
2. The preparation method for improving the strength of the tussah silk fiber according to claim 1, wherein in the step (5), the tussah silk is frozen at a temperature below 0 ℃ for 3-4h, then taken out and soaked in the aqueous solution containing the cross-linking agent, unfrozen at room temperature for 3-4h, and the freezing and unfreezing are repeated for 3 times.
3. The preparation method for improving the strength of the tussah silk fiber according to claim 1, wherein the ultrasonic frequency of the ultrasonic crushing in the step (1) is 20-25KHz, and the time is 20-30 min.
4. The preparation method for improving the strength of the tussah silk fiber according to claim 1, wherein the cross-linking agent adopted in the step (5) is CaCl2The concentration of the cross-linking agent aqueous solution is 0.1-0.5 wt%; the weight ratio of the tussah silk to the cross-linking agent aqueous solution is 6-8: 20.
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Denomination of invention: A preparation method for improving the strength of Wild silk fiber Effective date of registration: 20230630 Granted publication date: 20220104 Pledgee: Henan Sheqi Rural Commercial Bank Co.,Ltd. Pledgor: HENAN MINXING BIOTECHNOLOGY CO.,LTD. Registration number: Y2023980046817 |