CN110129897B - High-light-resistance silk and preparation method thereof - Google Patents
High-light-resistance silk and preparation method thereof Download PDFInfo
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- CN110129897B CN110129897B CN201910430967.6A CN201910430967A CN110129897B CN 110129897 B CN110129897 B CN 110129897B CN 201910430967 A CN201910430967 A CN 201910430967A CN 110129897 B CN110129897 B CN 110129897B
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- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
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Abstract
The invention provides high-light-resistance silk and a preparation method thereof, and particularly relates to the technical field of silk processing. The light resistance of the silk is improved from a silk preparation source, the silk is soaked by adding a protective agent after being boiled, then the silk reeling is carried out by adding a penetration auxiliary agent, and then a protective film is formed on the surface of the silk by adopting radiation polymerization reaction, so that the silk can keep good color, toughness and mechanical strength under the condition of ultraviolet accelerated destruction test, the change of breaking strength is lower than 5cN, the elongation at break is reduced within 5 percent, and the reduction of whiteness is within 5 percent.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of silk processing, in particular to high-light-resistance silk and a preparation method thereof.
[ background of the invention ]
The silk is continuous long fiber formed by solidifying silk liquid secreted by a mature silkworm during cocooning, is also called natural silk, is a natural protein fiber material, is one of the earliest animal fibers utilized by human beings, and is one of the main raw materials for producing high-grade light and thin garment fabrics in summer. Silk is a civilized product of ancient China, and the imperial concubine snail ancestor of Huangdi inherits the silkworm breeding, and the oracle has silk characters and silk side characters. According to archaeology, China has used silk to make silk threads, woven silk ribbons and simple silk fabrics about 4700 years ago, and silk fabrics such as lenos, silks, fine silk fabrics, yarns, crapes, silks, embroideries and the like which are woven by silk have appeared by the year of the week of commerce.
The silk has good moisture absorption, moisture release, heat dissipation and heat retention, and the woven fabric is comfortable to wear, smooth in hand feeling and soft in color, so that the silk enjoys the reputation of fibre queen. However, silk has a serious problem that yellowing, embrittlement, reduction of mechanical properties, and the like are caused when the silk is irradiated by sunlight in the using process. The GA solid gum technology that the quality of a Yangyi is makeed quality etc. published in 2014 35 th volume 3 rd phase's textile science newspaper influences the text of cocoon silk performance, indicate that adopt glutaraldehyde solid gum technology reducible sunlight, the air, sweat is to the erosion of silk, improve silk stability, but this method has leaded to the decline of silk whiteness degree to a certain extent, and adopted the hydrogen peroxide solution that has strong oxidizing property to carry out whiteness degree restoration processing, also cause the damage to the silk structure, mechanical properties and the light fastness promotion that has leaded to silk are not obvious.
Therefore, there is a need to develop a highly light-resistant silk that is less likely to discolor, embrittle, and break under long-term light irradiation.
[ summary of the invention ]
The invention aims to: aiming at the problems that the existing silk is easy to yellow, embrittle and reduce the mechanical property after being illuminated, the high-light-resistance silk and the preparation method thereof are provided. The silk keeps good color, toughness and mechanical strength under the condition of ultraviolet accelerated destruction test, so that the change of breaking strength is lower than 5cN, the elongation at break is reduced within 5 percent, and the reduction of whiteness is within 5 percent.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of silk with high light resistance comprises the following steps:
a. taking 19-35 parts of silkworm cocoon according to the weight part ratio, boiling the silkworm cocoon, adding 55-75 parts of protective agent, and soaking for 60-120 minutes under the conditions that the vacuum degree is 20-40kPa and the temperature is 40-50 ℃ to obtain a pretreated cocoon;
b. adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 13-23 parts of coix seed, 20-30 parts of poria cocos, 50-70 parts of water, 400 parts of rice washing water, 2-8 parts of glutaraldehyde, 15-25 parts of glutathione, 10-20 parts of 5-hydroxytryptamine and 1-5 parts of glucomannan;
c. taking silk fiber, and carrying out radiation polymerization reaction;
d. and (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
Preferably, the protective agent in the step a comprises the following raw materials in parts by weight: 6-10 parts of white carbon black, 140 parts of water 100-.
Further preferably, the preparation method of the protective agent comprises the following steps: according to the weight portion, adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer, homogenizing for 4-8 times under 80-120MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 3-5 times under 100-130MPa to obtain the protective agent.
More preferably, the radiation polymerization reaction in step c is performed by: gamma-ray is adopted for irradiation, the irradiation dose is 5-15kGy, and the irradiation time is 2-4 hours.
In a further preferred embodiment, the radiation polymerization in step c comprises: adopting electron beam irradiation, wherein the irradiation dose is 2-14kGy, and the irradiation time is 75-115 minutes.
Further preferably, the step b comprises 800mg of penetration assistant per 100ml of reeling soup.
Further preferably, the temperature of the reeling soup in the step b is 34-38 ℃, and the flow rate is 600-.
Still further preferably, the preparation method of the penetration aid in the step b comprises: soaking coix seeds, poria cocos and water at 60-80 ℃ for 90-120 minutes according to the weight part ratio, taking out the soaked coix seeds and poria cocos, adding the coix seeds and poria cocos into a high-pressure homogenizer, adding rice washing water, homogenizing for 2-4 times at 30-50MPa, taking out the coix seeds and the poria cocos, filtering, collecting an extracting solution, taking glutaraldehyde, glutathione, 5-hydroxytryptamine and the extracting solution, carrying out ultrasonic treatment for 20-30 minutes, adding glucomannan, and continuing ultrasonic treatment for 5-13 minutes to obtain the permeation aid.
A silk with high light resistance is prepared by the above method.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the light resistance of the silk is improved from a silk preparation source, the silk is soaked by adding a protective agent after being boiled, then the silk reeling is carried out by adding a penetration auxiliary agent, and then a protective film is formed on the surface of the silk by adopting radiation polymerization reaction, so that the silk can keep good color, toughness and mechanical strength under the condition of ultraviolet accelerated destruction test, the change of breaking strength is lower than 5cN, the elongation at break is reduced within 5 percent, and the reduction of whiteness is within 5 percent.
2. According to the invention, the white carbon black, water, dodecyl glucoside, zein, barium strontium titanate and sodium bicarbonate are adopted to prepare the protective agent, and the protective agent can be polymerized with the light-intolerant group of the silk, so that the whiteness, toughness and mechanical strength of the silk are well maintained, and the situations of yellowing, embrittlement and reduction of mechanical strength are not easy to occur under the illumination condition. Generally, the poor light resistance of silk is related to the existence of tryptophan and tyrosine side groups and the molecular chain structure of protein in silk, and under the illumination condition, ultraviolet rays in sunlight can oxidize the side groups and break the hydrogen bonds and the molecular chains of the protein, so that the silk is yellowed, embrittled and reduced in mechanical strength. According to the invention, zein and side groups of proteins in silk are polymerized, white carbon black and barium strontium titanate are used for effectively reflecting ultraviolet rays so as to reduce the absorption of the silk to the ultraviolet rays, dodecyl glucoside is added so that a protective agent forms a uniform suspension solution so as to increase the uniformity and the adhesiveness of the protective agent, and finally, substances in the protective agent form a protective film on the surface of the silk and are tightly adhered to the silk.
According to the ultraviolet-resistant white carbon black and the preparation method, both the white carbon black and the barium strontium titanate can reflect ultraviolet light, wherein the barium strontium titanate has a polyhedral structure, so that incident ultraviolet light can be reflected to form mutual interference to be offset, and the barium strontium titanate and the white carbon black have a synergistic effect when being mixed for use, and have a stronger ultraviolet-resistant effect than that when being used alone.
The diameter of the silk is usually about 10 mu m, the superfine surface is not easy to be adsorbed by large particle substances, and in order to enable the protective agent to be tightly adsorbed on the surface of the silk, the protective agent is prepared by adopting a high-pressure homogenization method, so that the protective agent can be fine and smooth in texture and form uniform particles with the particle size of less than 100 nm.
The white carbon black and the barium strontium titanate in the invention have certain hardness, are easy to cause abrasion to a high-pressure homogenizer, and have the conditions of incomplete partial thinning and large particles during homogenization. In order to fully refine the white carbon black and the barium strontium titanate, sodium bicarbonate is added during high-pressure homogenization, the sodium bicarbonate is rapidly decomposed under high pressure to generate carbon dioxide to form turbulence, so that the collision kinetic energy among the protective agent particles is increased, the crushing effect of the particles is enhanced, the particle size of the particles is further reduced, and meanwhile, a gasification film is formed between the protective agent particles and the inner wall of the homogenizer to reduce the abrasion of the inner wall of the homogenizer.
3. The penetration auxiliary agent is added in the silk reeling stage, so that the protective agent can be more tightly fixed on the surface of the silk, and the subsequent radiation polymerization reaction can be smoothly carried out. The penetration auxiliary agent contains 5-hydroxytryptamine which is used as neurotransmitter capable of combining with protein, and can enhance the affinity of the penetration auxiliary agent and the fibroin, so that the penetration auxiliary agent is easily combined with the fibroin. The invention uses rice washing water, coix seed and tuckahoe to prepare extracting solution, wherein the extracting solution contains starch, polysaccharide and other sticky particle components, and the fine particles and glutaraldehyde and glucomannan in the penetration auxiliary agent form substances with good adhesion, and the substances can be attached to the surface of silk, so that the protective agent and the silk are combined more tightly. The penetration aid also contains glutathione with oxidation resistance, can protect sulfydryl in silk protein molecules from being damaged by ultraviolet rays, and plays a role in preventing yellowing and embrittlement of silk and reduction of mechanical strength from the aspects except for protecting tryptophan and tyrosine side groups.
The preparation of the penetration aid also adopts a high-pressure homogenization method, and is also used for enabling large granular substances in the penetration aid to form uniform granules with fine texture and grain diameter below 100nm, and simultaneously, the cell walls of the coix seed and the tuckahoe can be cracked by a high-pressure method, wherein viscous components can be dissolved out into an extracting solution more completely, so that the uniform granules rich in the viscous components can enter the cocoon layer more easily, and the fixation effect of a protective agent on the surface of silk is favorably improved.
4. The invention adopts a radiation polymerization method to polymerize the zein and the side groups of the protein in the silk at normal temperature, which is different from the conventional high-temperature polymerization reaction which easily causes protein denaturation, and the radiation polymerization reaction used by the invention protects the molecular structure of the silk protein. The invention respectively adopts two methods of gamma ray irradiation and electron beam irradiation to realize the polymerization with tryptophan and tyrosine side groups in the silk, simultaneously further strengthens the molecular chain and hydrogen bond of the silk, and effectively enhances the light resistance of the silk.
5. According to the invention, the protective agent capable of polymerizing with the silk is added after the cocoon is boiled, and the radiation polymerization reaction is arranged after the silk reeling, so that each silk can be in full contact with the substances participating in the polymerization reaction, the condition that no residual tryptophan and tyrosine side groups exist is ensured, and the improvement of the light resistance of the silk is facilitated; and the silk fabric that uses among the prior art to make carries out radiation polymerization, because silk has been crossed and weaved, the silk thread for weaving is held in the arms for many silks and forms, can cause silk to fail like this and carry out abundant contact with the material of participating in polymerization, leads to partial tryptophan and tyrosine lateral group can not participate in the reaction, influences the promotion of silk light resistance greatly.
[ detailed description ] embodiments
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of silk with high light resistance comprises the following steps:
a. taking 19 parts of silkworm cocoon according to the weight part ratio, boiling the silkworm cocoon, adding 55 parts of protective agent, and soaking for 60 minutes under the conditions that the vacuum degree is 20Pa and the temperature is 40 ℃ to obtain a pretreated cocoon;
wherein, the protective agent comprises the following raw materials in parts by weight: 6 parts of white carbon black, 100 parts of water, 1 part of dodecyl glucoside, 12 parts of zein, 1 part of barium strontium titanate and 0.2 part of sodium bicarbonate.
The preparation method of the protective agent comprises the following steps: adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer according to the weight part ratio, homogenizing for 4 times under 80MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 3 times under 100MPa to obtain the protective agent.
b. Adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 13 parts of coix seeds, 20 parts of poria cocos, 50 parts of water, 300 parts of rice washing water, 2 parts of glutaraldehyde, 15 parts of glutathione, 10 parts of 5-hydroxytryptamine and 1 part of glucomannan;
wherein, every 100ml silk reeling soup contains 100mg penetration assistant.
c. Taking silk fiber, and carrying out radiation polymerization reaction;
the radiation polymerization reaction method comprises the following steps: gamma-ray is adopted for irradiation, the irradiation dose is 5kGy, and the irradiation time is 2 hours.
d. And (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
Example 2
A preparation method of silk with high light resistance comprises the following steps:
a. weighing 35 parts of silkworm cocoon according to the weight part ratio, boiling the silkworm cocoon, adding 75 parts of protective agent, and soaking for 120 minutes under the conditions that the vacuum degree is 40kPa and the temperature is 50 ℃ to obtain a pretreated cocoon;
wherein, the protective agent comprises the following raw materials in parts by weight: 10 parts of white carbon black, 140 parts of water, 3 parts of dodecyl glucoside, 16 parts of zein, 2 parts of barium strontium titanate and 1.2 parts of sodium bicarbonate.
The preparation method of the protective agent comprises the following steps: adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer according to the weight part ratio, homogenizing for 8 times under 120MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 5 times under 130MPa to obtain the protective agent.
b. Adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 23 parts of coix seeds, 30 parts of poria cocos, 70 parts of water, 400 parts of rice washing water, 8 parts of glutaraldehyde, 25 parts of glutathione, 20 parts of 5-hydroxytryptamine and 5 parts of glucomannan;
wherein, each 100ml silk reeling soup contains 800mg penetration assistant.
c. Taking silk fiber, and carrying out radiation polymerization reaction;
the radiation polymerization reaction method comprises the following steps: gamma-ray is adopted for irradiation, the irradiation dose is 15kGy, and the irradiation time is 4 hours.
d. And (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
Example 3
A preparation method of silk with high light resistance comprises the following steps:
a. taking 23 parts of silkworm cocoon according to the weight part ratio, boiling the silkworm cocoon, adding 60 parts of protective agent, and soaking for 75 minutes under the conditions that the vacuum degree is 25kPa and the temperature is 43 ℃ to obtain a pretreated cocoon;
wherein, the protective agent comprises the following raw materials in parts by weight: 7 parts of white carbon black, 110 parts of water, 1.5 parts of dodecyl glucoside, 13 parts of zein, 1.2 parts of barium strontium titanate and 0.5 part of sodium bicarbonate.
The preparation method of the protective agent comprises the following steps: according to the weight portion, adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer, homogenizing for 5 times under 90MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 4 times under 110MPa to obtain the protective agent.
b. Adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 15.5 parts of coix seeds, 22.5 parts of poria cocos, 55 parts of water, 325 parts of rice washing water, 3.5 parts of glutaraldehyde, 17 parts of glutathione, 13 parts of 5-hydroxytryptamine and 2 parts of glucomannan;
wherein, every 100ml silk reeling soup contains 300mg penetration assistant.
The temperature of the reeling soup is 34 deg.C, and the flow rate is 600 ml/min.
The preparation method of the penetration aid comprises the following steps: soaking coix seeds, poria cocos and water at 60 ℃ for 90 minutes according to the weight part ratio, taking out the soaked coix seeds and poria cocos, adding the coix seeds and poria cocos into a high-pressure homogenizer, adding rice washing water, homogenizing for 2 times under 30MPa, taking out the coix seeds and the poria cocos, filtering, collecting an extracting solution, taking glutaraldehyde, glutathione, 5-hydroxytryptamine and the extracting solution, carrying out ultrasonic treatment for 20 minutes, adding glucomannan, and continuing ultrasonic treatment for 5 minutes to obtain the penetration aid.
c. Taking silk fiber, and carrying out radiation polymerization reaction;
the radiation polymerization reaction method comprises the following steps: gamma-ray is adopted for irradiation, the irradiation dose is 10kGy, and the irradiation time is 3 hours.
d. And (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
Example 4
A preparation method of silk with high light resistance comprises the following steps:
a. taking 31 parts of silkworm cocoon according to the weight part ratio, boiling the silkworm cocoon, adding 70 parts of protective agent, and soaking for 105 minutes under the conditions that the vacuum degree is 35kPa and the temperature is 47 ℃ to obtain a pretreated cocoon;
wherein, the protective agent comprises the following raw materials in parts by weight: 9 parts of white carbon black, 130 parts of water, 2.5 parts of dodecyl glucoside, 15 parts of zein, 1.7 parts of barium strontium titanate and 1 part of sodium bicarbonate.
The preparation method of the protective agent comprises the following steps: adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer according to the weight part ratio, homogenizing for 7 times under 110MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 4 times under 120MPa to obtain the protective agent.
b. Adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 20 parts of coix seeds, 27 parts of poria cocos, 65 parts of water, 370 parts of rice washing water, 6.5 parts of glutaraldehyde, 23 parts of glutathione, 18 parts of 5-hydroxytryptamine and 4 parts of glucomannan;
wherein, every 100ml silk reeling soup contains 650mg penetration assistant.
The temperature of the reeling soup is 38 ℃, and the flow rate is 690 ml/min.
The preparation method of the penetration aid comprises the following steps: soaking coix seeds, poria cocos and water at 80 ℃ for 120 minutes according to the weight part ratio, taking out the soaked coix seeds and poria cocos, adding the coix seeds and poria cocos into a high-pressure homogenizer, adding rice washing water, homogenizing for 4 times at 50MPa, taking out the coix seeds and the poria cocos, filtering, collecting an extracting solution, taking glutaraldehyde, glutathione, 5-hydroxytryptamine and the extracting solution, carrying out ultrasonic treatment for 30 minutes, adding glucomannan, and continuing ultrasonic treatment for 13 minutes to obtain the penetration aid.
c. Taking silk fiber, and carrying out radiation polymerization reaction;
the radiation polymerization reaction method comprises the following steps: the electron beam irradiation is adopted, the irradiation dose is 2kGy, and the irradiation time is 75 minutes.
d. And (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
Example 5
A preparation method of silk with high light resistance comprises the following steps:
a. weighing 33 parts of silkworm cocoon according to the weight part ratio, boiling the silkworm cocoon, adding 73 parts of protective agent, and soaking for 112 minutes under the conditions that the vacuum degree is 37kPa and the temperature is 48 ℃ to obtain a pretreated cocoon;
wherein, the protective agent comprises the following raw materials in parts by weight: 9.5 parts of white carbon black, 135 parts of water, 2.7 parts of dodecyl glucoside, 15.5 parts of zein, 1.6 parts of barium strontium titanate and 1.1 parts of sodium bicarbonate.
The preparation method of the protective agent comprises the following steps: adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer according to the weight part ratio, homogenizing for 6 times under 115MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 4 times under 125MPa to obtain the protective agent.
b. Adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 21.5 parts of coix seeds, 28.5 parts of poria cocos, 68 parts of water, 385 parts of rice washing water, 7.5 parts of glutaraldehyde, 24 parts of glutathione, 17 parts of 5-hydroxytryptamine and 4.5 parts of glucomannan;
wherein, each 100ml silk reeling soup contains 750mg penetration assistant.
The temperature of the reeling soup is 35 deg.C, and the flow rate is 625 ml/min.
The preparation method of the penetration aid comprises the following steps: soaking coix seeds, poria cocos and water at 65 ℃ for 97 minutes according to the weight part ratio, taking out the soaked coix seeds and poria cocos, adding the coix seeds and poria cocos into a high-pressure homogenizer, adding rice washing water, homogenizing for 3 times at 35MPa, taking out the coix seeds and the poria cocos, filtering, collecting an extracting solution, taking glutaraldehyde, glutathione, 5-hydroxytryptamine and the extracting solution, carrying out ultrasonic treatment for 22 minutes, adding glucomannan, and continuing ultrasonic treatment for 7 minutes to obtain the penetration aid.
c. Taking silk fiber, and carrying out radiation polymerization reaction;
the radiation polymerization reaction method comprises the following steps: the electron beam irradiation is adopted, the irradiation dose is 14kGy, and the irradiation time is 115 minutes.
d. And (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
Example 6
A preparation method of silk with high light resistance comprises the following steps:
a. taking 27 parts of silkworm cocoons according to the weight part ratio, boiling the cocoons, adding 65 parts of protective agent, and soaking for 90 minutes under the conditions that the vacuum degree is 30kPa and the temperature is 45 ℃ to obtain pretreated cocoons;
wherein, the protective agent comprises the following raw materials in parts by weight: 8 parts of white carbon black, 120 parts of water, 2 parts of dodecyl glucoside, 14 parts of zein, 1.5 parts of barium strontium titanate and 0.7 part of sodium bicarbonate.
The preparation method of the protective agent comprises the following steps: according to the weight portion, adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer, homogenizing for 6 times under 100MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 4 times under 115MPa to obtain the protective agent.
b. Adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 18 parts of coix seeds, 25 parts of poria cocos, 60 parts of water, 350 parts of rice washing water, 5 parts of glutaraldehyde, 20 parts of glutathione, 15 parts of 5-hydroxytryptamine and 3 parts of glucomannan;
wherein, each 100ml silk reeling soup contains 450mg penetration assistant.
The temperature of the reeling soup is 37 deg.C, and the flow rate is 665 ml/min.
The preparation method of the penetration aid comprises the following steps: soaking coix seeds, poria cocos and water at 75 ℃ for 113 minutes according to the weight part ratio, taking out the soaked coix seeds and poria cocos, adding the coix seeds and poria cocos into a high-pressure homogenizer, adding rice washing water, homogenizing for 3 times at 45MPa, taking out the coix seeds and the poria cocos, filtering, collecting an extracting solution, taking glutaraldehyde, glutathione, 5-hydroxytryptamine and the extracting solution, carrying out ultrasonic treatment for 27 minutes, adding glucomannan, and continuing ultrasonic treatment for 11 minutes to obtain the penetration aid.
c. Taking silk fiber, and carrying out radiation polymerization reaction;
the radiation polymerization reaction method comprises the following steps: the electron beam irradiation is adopted, the irradiation dose is 8kGy, and the irradiation time is 95 minutes.
d. And (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
Example 7
The difference from example 6 is that barium strontium titanate is not added in the preparation of the protective agent in step a. The rest of the procedure was the same as in example 6.
Example 8
The difference from example 6 is that no sodium bicarbonate is added to prepare the protectant in step a. The rest of the procedure was the same as in example 6.
Example 9
The difference from example 6 is that the protective agent is prepared in step a by stirring and mixing instead of high-pressure homogenization. The rest of the procedure was the same as in example 6.
Example 10
The difference from example 6 is that instead of radiation polymerization, a reaction at a temperature of 90 ℃ for 30 minutes is used in step c. The rest of the procedure was the same as in example 6.
Example 11
The difference from example 6 is that no 5-hydroxytryptamine was added to the permeation aid. The rest of the procedure was the same as in example 6.
Example 12
The difference from example 6 is that glutathione was not added to the permeation aid. The rest of the procedure was the same as in example 6.
Example 13 comparison of effects
1. Preparation of test samples
The same batch of raw materials was selected and experimental samples 3, 5, 6-12 were prepared according to the methods of examples 3, 5, 6-12.
2. Evaluation method
Placing the experimental samples 3, 5, 6-12 in a sunshine climate tester for 180 hours to perform ultraviolet accelerated destruction test, setting the wavelength of the instrument to be 420nm, the temperature to be 35 ℃, the humidity to be 40 percent and the irradiance to be 1.10W/m2And/nm, measuring the whiteness of each experimental sample before and after breakage by using a whiteness meter, and measuring the breaking strength and the breaking elongation of each experimental sample before and after breakage by using a single fiber strength meter.
3. Evaluation results
TABLE 1 Silk Performance test results
4. Results of the experiment
As can be seen from table 1, the quality of the experimental samples 3, 5, 6 is better, with the best quality of the experimental sample 6.
In the experimental sample 7, barium strontium titanate is not added during the preparation of the protective agent, so that the ultraviolet ray resisting effect is poorer than that of the experimental samples 3, 5 and 6, and after an ultraviolet ray accelerated destruction test, the protective agent is easy to yellow, embrittle and deteriorate the mechanical property, so that the whiteness, the breaking strength and the breaking elongation are reduced.
In the experimental sample 8, sodium bicarbonate is not added when the protective agent is prepared, and in the experimental sample 9, high-pressure homogenization is replaced by stirring and mixing when the protective agent is prepared, so that the particles of the protective agent are not fine enough, the ultraviolet ray resisting effect is poorer than that of the experimental samples 3, 5 and 6, and after an ultraviolet ray accelerated destruction test, the protective agent is easy to yellow and embrittle and the mechanical property is poor, so that the whiteness, the breaking strength and the breaking elongation are all reduced.
In the experimental sample 10, the temperature is increased to 90 ℃ for 30 minutes instead of radiation polymerization reaction, so that the silk protein is denatured to a certain degree, the breaking strength and the breaking elongation of the prepared finished product are very low, the ultraviolet ray resisting effect is poorer than that of the experimental samples 3, 5 and 6, and after an ultraviolet ray accelerated destruction test, the finished product is easy to yellow, embrittle and have poor mechanical properties, so that the whiteness, the breaking strength and the breaking elongation are obviously reduced.
In the experimental sample 11, 5-hydroxytryptamine is not added in the penetration aid, so that the penetration aid and fibroin are not tightly combined, the ultraviolet ray resisting effect is poorer than that of the experimental samples 3, 5 and 6, and after an ultraviolet ray accelerated destruction test, yellowing, embrittlement and mechanical property deterioration are easy to occur, so that the whiteness, the breaking strength and the breaking elongation are reduced.
Glutathione is not added in the penetration auxiliary agent of the experimental sample 12, so that sulfydryl in the silk protein molecules is easily damaged by ultraviolet rays, the ultraviolet ray resisting effect is poorer than that of the experimental samples 3, 5 and 6, and after an ultraviolet ray accelerated damage test, the silk protein molecules are easily yellowed, embrittled and poor in mechanical property, so that the whiteness, the breaking strength and the breaking elongation are reduced.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (3)
1. The preparation method of the silk with high light resistance is characterized by comprising the following steps:
a. taking 19-35 parts of silkworm cocoon according to the weight part ratio, boiling the silkworm cocoon, adding 55-75 parts of protective agent, and soaking for 60-120 minutes under the conditions that the vacuum degree is 20-40kPa and the temperature is 40-50 ℃ to obtain a pretreated cocoon; the protective agent comprises the following raw materials in parts by weight: 6-10 parts of white carbon black, 140 parts of water 100-; the preparation method of the protective agent comprises the following steps: adding white carbon black, dodecyl glucoside and water into a high-pressure homogenizer according to the weight part ratio, homogenizing for 4-8 times under 80-120MPa, then adding zein, barium strontium titanate and sodium bicarbonate, and continuing homogenizing for 3-5 times under 100-130MPa to obtain a protective agent;
b. adding a penetration auxiliary agent into the silk reeling soup, and then adding the pretreated cocoons for silk reeling to obtain silk fibers; the penetration aid comprises the following raw materials in parts by weight: 13-23 parts of coix seed, 20-30 parts of poria cocos, 50-70 parts of water, 400 parts of rice washing water, 2-8 parts of glutaraldehyde, 15-25 parts of glutathione, 10-20 parts of 5-hydroxytryptamine and 1-5 parts of glucomannan; soaking coix seeds, poria cocos and water at 60-80 ℃ for 90-120 minutes according to the weight part ratio, taking out the soaked coix seeds and poria cocos, adding the coix seeds and poria cocos into a high-pressure homogenizer, adding rice washing water, homogenizing for 2-4 times at 30-50MPa, taking out the coix seeds and the poria cocos, filtering, collecting an extracting solution, taking glutaraldehyde, glutathione, 5-hydroxytryptamine and the extracting solution, carrying out ultrasonic treatment for 20-30 minutes, adding glucomannan, and continuing ultrasonic treatment for 5-13 minutes to obtain a penetration aid;
c. taking silk fiber, and carrying out radiation polymerization reaction at normal temperature to polymerize zein and side groups of protein in silk; the method for the radiation polymerization reaction comprises the following steps: irradiating by adopting electron beams, wherein the irradiation dose is 2-14kGy, and the irradiation time is 75-115 minutes;
d. and (3) re-shaking and finishing the silk fiber subjected to radiation polymerization to obtain the high-light-resistance silk.
2. The method for preparing silk with high light fastness according to claim 1, wherein the penetration assistant is 100-800mg per 100ml silk reeling soup in step b.
3. Highly lightfast silk obtained by the method according to any one of claims 1 to 2.
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| JPH0921013A (en) * | 1995-07-04 | 1997-01-21 | Aiko Soma | Floss |
| EP1712561A1 (en) * | 2004-01-13 | 2006-10-18 | Toray Industries, Inc. | Silk thread containing spider thread protein and silkworm producing the silk thread |
| CN104294374A (en) * | 2014-10-29 | 2015-01-21 | 广西隆林嘉利茧丝绸有限公司 | High-quality mulberry silk manufacturing technology |
| CN104631116A (en) * | 2013-11-14 | 2015-05-20 | 青岛鑫益发工贸有限公司 | Functional arrangement technology for silk fabrics |
| CN105970697A (en) * | 2016-06-02 | 2016-09-28 | 辽东学院 | Color fixing process method for natural dyeing of textiles |
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| JPH0921013A (en) * | 1995-07-04 | 1997-01-21 | Aiko Soma | Floss |
| EP1712561A1 (en) * | 2004-01-13 | 2006-10-18 | Toray Industries, Inc. | Silk thread containing spider thread protein and silkworm producing the silk thread |
| CN104631116A (en) * | 2013-11-14 | 2015-05-20 | 青岛鑫益发工贸有限公司 | Functional arrangement technology for silk fabrics |
| CN104294374A (en) * | 2014-10-29 | 2015-01-21 | 广西隆林嘉利茧丝绸有限公司 | High-quality mulberry silk manufacturing technology |
| CN105970697A (en) * | 2016-06-02 | 2016-09-28 | 辽东学院 | Color fixing process method for natural dyeing of textiles |
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