CN112680798A - Silkworm cocoon degumming process and application thereof in production of spunlace non-woven fabric - Google Patents

Silkworm cocoon degumming process and application thereof in production of spunlace non-woven fabric Download PDF

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CN112680798A
CN112680798A CN201910986550.8A CN201910986550A CN112680798A CN 112680798 A CN112680798 A CN 112680798A CN 201910986550 A CN201910986550 A CN 201910986550A CN 112680798 A CN112680798 A CN 112680798A
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enzymolysis
fibroin
degumming process
spunlace
aqueous solution
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李和伟
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Abstract

The invention discloses a silkworm cocoon degumming process and application thereof in production of spunlace non-woven fabrics. And sericin zymolyte such as sericin peptide aqueous solution can be completely recycled. The whole process avoids the generation of wastewater in the traditional silkworm cocoon degumming process, and the recycling of the recovered sericin peptide aqueous solution has unique value, so that higher-end spunlace non-woven fabrics can be produced. The spunlace non-woven fabric not only has high softness, but also can dissolve out sericin peptide after being used as a membrane cloth to be manufactured into a skin-care mask, and has better skin-care effect. The silkworm cocoon degumming process and the application technology thereof in the production of the spunlace nonwoven fabric fully consider environmental protection and resource recycling, the market value of the whole process is very high, and products with better quality, such as high-end spunlace nonwoven fabrics, high-end facial masks, silk peptide and the like, can be obtained.

Description

Silkworm cocoon degumming process and application thereof in production of spunlace non-woven fabric
Technical Field
The invention relates to the field of textiles, in particular to a silkworm cocoon degumming process and application thereof in production of spunlace non-woven fabrics.
Background
Silkworm breeding is a traditional industry in some areas of China, deep processing research on silkworm cocoons is a mature technology, and silk is the most widely used direction. The silk cocoon comprises sericin and fibroin, and the silk is sericin removed fibroin, so the common silk process is to remove sericin by alkaline water or a solvent method to obtain the fibroin, and the problem is that a large amount of sewage needs to be treated. Although some prior documents describe a treatment process for sericin or silk fibroin, the treatment process is a single substance and does not solve the problem of sewage in the source silkworm cocoon treatment.
In addition, the spunlace nonwoven fabric is a product with wide application, and the application of the spunlace nonwoven fabric relates to the subject fields of medical health, light industry, electronics, environmental protection and the like. The hydroentangling method, also known as hydroentangling method, hydroentangling method and spunlace method, utilizes the impact of high-speed and high-pressure water flow on the fiber web to promote the fibers to be mutually entangled and cohered to reinforce the fiber web, and is a relatively new non-woven fabric processing technology. The important energy consumption of the spunlace non-woven fabric processing technology is water resource, and the water mainly used at present is pure water. With the market demand upgrading, the functional requirements for the spunlace nonwoven fabric are also higher and higher, and a great deal of research technologies on the spunlace nonwoven fabric are also disclosed in the existing literature, such as the nonwoven fabric taking cotton linters as the raw material and the nonwoven fabric taking silk staple fibers as the raw material developed by Asahi, which mainly aim at the selection of the fiber raw material of the nonwoven fabric. However, no research on the water source of the spunlace nonwoven fabric is found at present.
Disclosure of Invention
The inventor of the invention aims at the problem that silk degumming in the prior art has a large amount of sewage and the high-end requirement problem of spunlace non-woven fabrics, carries out a large amount of conception and innovation, combines the two problems, develops a new technical scheme, can solve the technical problems in the two fields simultaneously, and obtains a new silk degumming technology and a new spunlace non-woven fabric product.
The invention firstly develops a silkworm cocoon degumming process, and performs enzymolysis control reaction on silkworm cocoons, so that an enzymolysis product contains sericin peptide aqueous solution, and fibroin is not subjected to enzymolysis.
The enzymolysis control reaction comprises the following steps: selecting alkaline protease, preferably alkaline protease such as papain, trypsin, and trypsin; adjusting pH of the solution to 8.5-9.5, preferably 8.5, and hydrolyzing at 50-60 deg.C (preferably 55 deg.C) for 40-55min (preferably 50 min); then adjusting pH of the hydrolysate to 7.0, heating to 70-90 deg.C (preferably 80 deg.C), maintaining the temperature for 20-30min (preferably 20min), and terminating the enzymolysis reaction.
The alkaline protease is added in an amount of 0.5-1.5 g/L.
The pH regulator in the enzymolysis control reaction is preferably NaHCO3The addition amount is 5-8 g/L.
A surfactant, such as soap liquid, is also added in the enzymolysis control reaction, and the addition amount is 1.0-2.0g/L, so that the degumming efficiency can be effectively improved.
The cocoon in the above cocoon degumming process is soaked in water, such as 30-50 times of 50-60 deg.C warm water for 3-5 hr, preferably 30-50 times of 50 deg.C warm water for 3 hr.
After the enzymolysis control reaction is ended, cooling the hydrolysate to room temperature for centrifugation, centrifuging at 10000-. The recovered sericin peptide aqueous solution can be used as a spunlace water source in the production of spunlace non-woven fabrics. The fibroin obtained by separation can be subjected to subsequent treatment to obtain fibroin peptide used as raw materials of medical dressing, skin care and hair care, health food and the like; the specific treatment steps are as follows:
1) washing the separated silk fibroin with deionized water for many times until clean silk fibroin is obtained;
2) enzymolysis of silk fibroin: taking clean silk fibroin to ensure that the concentration of a silk fibroin aqueous solution is 5-8%, adding 0.5-1g/L protease, reacting at 50-70 ℃, preferably 60 ℃, and the pH value of the reaction is 8.5-9, and reacting for 3-5h, preferably 4 h;
3) and (3) terminating the enzymolysis of the silk fibroin: adjusting pH of the fibroin hydrolysate to 7.0, heating to 70-90 deg.C, preferably 80 deg.C, maintaining the temperature for 20-30min, preferably 20min, and terminating the enzymolysis reaction;
4) extracting silk peptide: after the fibroin hydrolysate is cooled to room temperature, centrifuging at 10000-.
The protease in the silk enzymolysis can be selected from alkaline protease such as trypsin, etc.
The sericin peptide aqueous solution recovered in the silkworm cocoon degumming process can be used as a spunlace water source in the production of spunlace non-woven fabrics, so the invention also relates to a novel spunlace non-woven fabric product and a production method thereof. The spunlace non-woven fabric is prepared by the method, the fibers of the non-woven fabric can be selected from silk or other common fibers, and the non-woven fabric product with very high softness can be obtained after the spunlace treatment by the sericin peptide aqueous solution, so that the selection threshold and the cost of the raw materials of the spunlace non-woven fabric are reduced.
The reaction is controlled by enzymolysis in the silkworm cocoon degumming process, so that the enzymolysis of sericin and fibroin is effectively isolated, the reaction is carried out towards the expected direction, and sericin zymolyte such as a sericin peptide aqueous solution can be completely recycled. The whole process avoids the generation of wastewater in the traditional silkworm cocoon degumming process, and the recycling of the recovered sericin peptide aqueous solution has unique value, so that higher-end spunlace non-woven fabrics can be produced. The spunlace non-woven fabric not only has high softness, but also can dissolve out sericin peptide after being used as a membrane cloth to be manufactured into a skin-care mask, and has better skin-care effect. In addition, fibroin can be treated in the whole process to obtain high-quality fibroin peptide which can be used for manufacturing medical dressings, raw materials for skin care and hair care, health-care food and the like.
The silkworm cocoon degumming process and the application technology thereof in the production of the spunlace nonwoven fabric fully consider environmental protection and resource recycling, the market value of the whole process is very high, and products with better quality, such as high-end spunlace nonwoven fabrics, high-end facial masks, silk peptide and the like, can be obtained.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1: silkworm cocoon degumming process
1. Soaking silkworm cocoon
The silkworm cocoon is soaked in warm water with the mass of 30 times and the temperature of 50 ℃ for 3 hours.
2. Enzymolysis degumming
Adding papain into the silkworm cocoon soaking mixture, wherein the addition amount is 0.5 g/L; adding NaHCO3 in an amount of 5 g/L; surfactant was added in an amount of 1.0 g/L. Stirring, adjusting pH to 8.5, and hydrolyzing at 50 deg.C for 40 min.
3. Terminating the enzymolysis
Adjusting the pH value of the hydrolysate to 7.0, heating to 70 ℃, and keeping the temperature for 20min to terminate the enzymolysis reaction. The enzymolysis product contains sericin peptide aqueous solution, and the fibroin is not subjected to enzymolysis.
4. Silk separation
And after the hydrolysate is cooled to room temperature, centrifuging at 10000rpm for 20min, removing the sericin peptide aqueous solution, and washing the fibroin for multiple times by deionized water until clean fibroin is obtained.
5. Hydrolysis of fibroin
Taking clean silk fibroin to ensure that the concentration of the silk fibroin aqueous solution is 5 percent, adding 0.5g/L of enzyme, reacting at the temperature of 50 ℃, and reacting for 3 hours, wherein the reaction pH value is 8.5.
6. Terminating the enzymolysis of the fibroin
Adjusting the pH value of the fibroin hydrolysate to 7.0, heating to 70 ℃, and keeping the temperature for 20min to terminate the enzymolysis reaction.
7. Extraction of silk peptide
And after the fibroin hydrolysate is cooled to room temperature, centrifuging at 10000rpm for 20min, removing inactivated alkaline protease and unhydrolyzed complete fibroin, and taking supernatant to obtain the fibroin peptide solution.
Example 2: silkworm cocoon degumming process 2
1. Soaking silkworm cocoon
The silkworm cocoon is soaked in 40 times of warm water with the mass of 55 ℃ for 4 hours.
2. Enzymolysis degumming
Adding trypsin into the silkworm cocoon soaking mixture, wherein the addition amount is 1 g/L; adding NaHCO3 in an amount of 6 g/L; surfactant was added in an amount of 1.5 g/L. Stirring, adjusting pH to 9, and hydrolyzing at 55 deg.C for 50 min.
3. Terminating the enzymolysis
Adjusting the pH value of the hydrolysate to 7.0, heating to 80 ℃, and keeping the temperature for 25min to terminate the enzymolysis reaction. The enzymolysis product contains sericin peptide aqueous solution, and the fibroin is not subjected to enzymolysis.
4. Silk separation
And after the hydrolysate is cooled to room temperature, centrifuging at the speed of 15000rpm for 25min, removing the sericin peptide aqueous solution, and washing the fibroin for multiple times by deionized water until clean fibroin is obtained.
5. Hydrolysis of fibroin
Taking clean silk fibroin, ensuring that the concentration of a silk fibroin aqueous solution is 6 percent, adding 0.8g/L of enzyme, reacting at the temperature of 60 ℃, and reacting for 4 hours, wherein the reaction pH value is 8.5.
6. Terminating the enzymolysis of the fibroin
Adjusting the pH value of the fibroin hydrolysate to 7.0, heating to 80 ℃, and keeping the temperature for 25min to terminate the enzymolysis reaction.
7. Extraction of silk peptide
And after the fibroin hydrolysate is cooled to room temperature, centrifuging at the speed of 15000rpm for 25min, removing inactivated alkaline protease and unhydrolyzed complete fibroin protein, and taking supernatant to obtain the fibroin peptide solution.
Example 3: silkworm cocoon degumming process III
1. Soaking silkworm cocoon
The silkworm cocoon is soaked in 50 times of 60 ℃ warm water for 5 hours.
2. Enzymolysis degumming
Adding trypsin into the silkworm cocoon soaking mixture, wherein the addition amount of the trypsin is 1.5 g/L; adding NaHCO3 in an amount of 8 g/L; the surfactant was added in an amount of 2.0 g/L. Stirring, adjusting pH to 9.5, and hydrolyzing at 60 deg.C for 55 min.
3. Terminating the enzymolysis
Adjusting the pH value of the hydrolysate to 7.0, heating to 90 ℃, and keeping the temperature for 30min to terminate the enzymolysis reaction. The enzymolysis product contains sericin peptide aqueous solution, and the fibroin is not subjected to enzymolysis.
4. Silk separation
And after the hydrolysate is cooled to room temperature, centrifuging at 20000rpm for 30min, removing sericin peptide aqueous solution, and washing the fibroin for multiple times by deionized water until clean fibroin is obtained.
5. Hydrolysis of fibroin
Taking clean silk fibroin to ensure that the concentration of the silk fibroin aqueous solution is 8 percent, the enzyme adding amount is 1g/L, the reaction temperature is 70 ℃, the reaction pH value is 9, and the reaction time is 5 hours.
6. Terminating the enzymolysis of the fibroin
Adjusting the pH value of the fibroin hydrolysate to 7.0, heating to 90 ℃, and keeping the temperature for 30min to terminate the enzymolysis reaction.
7. Extraction of silk peptide
And after the fibroin hydrolysate is cooled to room temperature, centrifuging at the speed of 2000rpm for 30min, removing inactivated alkaline protease and unhydrolyzed complete fibroin protein, and taking supernatant to obtain the fibroin peptide solution.
Example 4: production of spunlace nonwoven fabric
The production of the spunlace nonwoven fabric adopts a conventional spunlace nonwoven fabric production process, and the basic process flow is as follows: web forming, prewetting, multi-channel spunlace reinforcement on the front and back surfaces, pattern spunlace, dewatering, predrying, after finishing, drying qualitative, slitting, winding and packaging. The spunlace water source selects the sericin peptide aqueous solution recovered in the examples 1-3 to carry out spunlace treatment, and a spunlace nonwoven fabric 1, a spunlace nonwoven fabric 2 and a spunlace nonwoven fabric 3 are respectively obtained.
Example 5: detection of spunlace nonwoven fabric
Using a model YT-RR 1000 softness instrument, according to the standard: measurement of softness of GB/T8942-2016 paper the hydroentangled nonwoven fabrics prepared in the above examples were tested for softness with the following results:
softness
Water-jet non-woven fabric 1 15mN (milliNewton)
Water-jet non-woven fabric 2 17mN (milliNewton)
Water-jet non-woven fabric 3 10mN (milliNewton)
Ordinary spunlace nonwoven fabric 45mN (milliNewton)
Note: the source of the common spunlace non-woven fabric is as follows: the lyocell/cuprammonium fiber blended viscose non-woven fabric.
As can be seen from the softness results, the nonwoven fabrics hydroentangled with the recovered sericin peptide aqueous solutions of examples 1 to 3 of the present invention had much better softness than the conventional hydroentangled nonwoven fabrics.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (13)

1. A silkworm cocoon degumming process is characterized in that: carrying out enzymolysis control reaction on the silkworm cocoon to ensure that an enzymolysis product contains sericin peptide aqueous solution and the fibroin is not subjected to enzymolysis.
2. The cocoon degumming process according to claim 1, wherein: the enzymolysis control reaction is as follows: selecting alkaline protease, adjusting pH to 8.5-9.5, and hydrolyzing at 50-60 deg.C for 40-55 min; then adjusting pH of the hydrolysate to 7.0, heating to 70-90 deg.C, maintaining the temperature for 20-30min, and terminating the enzymolysis reaction.
3. The cocoon degumming process according to claim 2, wherein: the addition amount of the alkaline protease is 0.5-1.5g/L, and the alkaline protease is preferably papain or trypsin.
4. The cocoon degumming process according to claim 2, wherein: the pH value regulator in the enzymolysis control reaction is NaHCO3The addition amount is 5-8 g/L.
5. The cocoon degumming process according to claim 2, wherein: and a surfactant is also added in the enzymolysis control reaction, and the addition amount is 1.0-2.0 g/L.
6. The cocoon degumming process according to claim 1, wherein: the silkworm cocoon is a soaking product of the silkworm cocoon in water.
7. The cocoon degumming process according to claim 2, wherein: and after the enzymolysis control reaction is ended, cooling the hydrolysate to room temperature, centrifuging, and recovering to obtain sericin peptide aqueous solution and separated fibroin.
8. The cocoon degumming process according to claim 7, wherein: the sericin peptide aqueous solution is used as a spunlace water source in the production of spunlace non-woven fabrics.
9. The cocoon degumming process according to claim 7, wherein: the subsequent processing steps of the separated fibroin are as follows:
1) washing the separated silk fibroin with deionized water for many times until clean silk fibroin is obtained;
2) enzymolysis of silk fibroin: taking clean silk fibroin to ensure that the concentration of a silk fibroin aqueous solution is 5-8%, adding 0.5-1g/L protease, reacting at 50-70 ℃, and reacting for 3-5h, wherein the reaction pH value is 8.5-9;
3) and (3) terminating the enzymolysis of the silk fibroin: adjusting the pH value of the fibroin hydrolysate to 7.0, heating to 70-90 ℃, and keeping the temperature for 20-30min to terminate the enzymolysis reaction;
4) extracting silk peptide: after the fibroin hydrolysate is cooled to room temperature, centrifuging at 10000-.
10. The cocoon degumming process according to claim 9, wherein: the silk peptide is used as raw materials of medical dressing, skin care and hair care and health food.
11. A spunlace nonwoven fabric is characterized in that: the sericin peptide aqueous solution according to claim 1 or 7 is selected as a water source for spunlace production.
12. A production process of spunlace non-woven fabric is characterized by comprising the following steps: an aqueous solution of the sericin peptide as defined in claim 1 or 7 is selected as a source of water for the water-jet.
13. A mask made from a spunlace nonwoven fabric of claim 11 as a base mask.
CN201910986550.8A 2019-10-17 2019-10-17 Silkworm cocoon degumming process and application thereof in production of spunlace non-woven fabric Pending CN112680798A (en)

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CN113403752A (en) * 2021-07-20 2021-09-17 江苏华佳丝绸股份有限公司 Preparation method of sericin reinforced silk non-woven fabric

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Publication number Priority date Publication date Assignee Title
CN113403752A (en) * 2021-07-20 2021-09-17 江苏华佳丝绸股份有限公司 Preparation method of sericin reinforced silk non-woven fabric

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Application publication date: 20210420