CN106381562A

CN106381562A - Preparation method for silk protein microfibers

Info

Publication number: CN106381562A
Application number: CN201510447803.6A
Authority: CN
Inventors: 沈守兵; 陈秀苗; 陈园园
Original assignee: Shanghai Shuixing Home Textile Co Ltd
Current assignee: Shanghai Shuixing Home Textile Co Ltd
Priority date: 2015-07-27
Filing date: 2015-07-27
Publication date: 2017-02-08

Abstract

The invention discloses a preparation method for silk protein microfibers, wherein the preparation method comprises the following steps: firstly, removing impurities in silk protein raw material fibers by using a steaming pre-shrinking machine, carrying out lye degumming, washing and drying, dissolving in a lithium bromide solution, and fully hydrolyzing to obtain a silk protein-lithium bromide solution; continuing to concentrate, to obtain a saturated silk protein solution; carrying out a certain dialysis process of the solution, and removing lithium bromide in the solution, to obtain a silk protein auxiliary agent solution; and then performing by a spray-process or impregnation-process treatment process, drying, and shaping to obtain the silk protein microfibers. The prepared fibers contain multiple amino acids, minerals and vitamins and the like necessary for human bodies, and has the functions of protecting skin, beautifying feature, promoting sleeping and the like.

Description

A kind of preparation method of fibroin microfilament fiber

Technical field

The present invention relates to a kind of preparation method of microfilament fiber, particularly to a kind of fibroin microfilament fiber Preparation method.

Background technology

Nearly ten years, the requirement to dress for the people has a very large change, and is changed into by force from focusing on ruggedness Adjust comfortableness；Modern start be particular about quality of life, not only to dress with it, to living environment it is also proposed that Very high health care, environmental requirement；Take another look at and live closely related New textile material with us, such as Tencel Fiber, Model fiber, pupa protein fiber, soybean fiber, bamboo carbon fiber, coconut palm Carbon fibe etc., Also it is seen that, all close around environmental protection, comfortable, feature, this is big for the exploitation of family's woven material nearly ten years Theme.

Fibroin is mainly made up of fibroin albumen and sericin two parts；Fibroin albumen is the master of silkworm silk Want part, account for the 75% of total amount, remaining major part is that sericin there are about 25%；Fibroin contains 18 Plant aminoacid, wherein contain 8 kinds of aminoacid needed by human, the primary amino acid constituting fibroin albumen is Aminoacetic acid, alanine, serine and tyrosine；Serine in sericin, aspartic acid and sweet Histidine content is higher；The molecular weight of fibroin is from tens of thousands of to more than 30 ten thousand；There are some in silkworm silk has Functional group, has good chemosensitivity, can change into multiple Land use systems；Silkworm silk itself It is protein, there is the characteristics such as moisturizing, anti-ultraviolet and protection skin.

Therefore develop fibroin terylene --- microfilament fiber, prepared fiber contains some necessary to human body Plant aminoacid, mineral, vitamin etc., there is the functions such as cosmetology, hypnotic, this product Release, both filled up the blank in market, and met the purchasing demand of consumer again, and had good market prospect.

Content of the invention

The technical problem to be solved in the present invention is to provide a kind of preparation process is simple, convenient fibroin microfilament The preparation method of fiber.

For reaching above-mentioned purpose, technical scheme is as follows：

A kind of preparation method of fibroin microfilament fiber, described preparation method comprises the steps：

(1) pretreatment fibroin raw material：By 50/50 by the mixing silk fiber raw material of pelettes and cocoon Impurity in mixing silk fiber raw material is removed using steam-shrinkage machine；

(2) prepare fibroin compounding agent solution：The mixing silk fiber after the removal of impurity will be removed in step (1) Raw material is placed in the NaC03 aqueous solution of 0.6mol/L, wherein mixes silk fiber raw material：NaC03 is 1:1.3 Part by weight, then degumming 1.5 hours at a temperature of 85 DEG C, after the completion of degumming, silk fiber will be mixed Clean post-drying with water, and weigh；Then by the mixing silk fiber of degumming according to mixing silk fiber：Bromine Changing lithium is 1:0.6 part by weight, is dissolved in the lithium bromide water solution of 12mol/L, at a temperature of 40 DEG C Hydrolysis 5 hours, obtains fibroin lithium-bromide solution, dissolubility in water for the lithium bromide after the completion of hydrolysis Reduce with temperature and reduce, when solution is in saturation, solid brominated lithium crystallization precipitation obtains saturation silkworm silk Protein solution, this solution is loaded in dialysis sack, the lithium bromide in solution constantly carries out dialysis outside sack, Thus removing lithium bromide, being retained in dialysis sack is then fibroin compounding agent solution；

(3) postfinishing process of microfilament fiber：Carried out using spray process or infusion process handling process, its condition Be part by weight using silicone oil and water be 1:10, the weight of fibroin composite assistant solution and silicon oil solution Than for 1:9, spinning speed be 180m/min, in bath the dipping temperature of fibroin compounding agent solution be 35～ 45 DEG C, dip time is 40 minutes, is then dried, and the temperature of drying is 95～100 DEG C；The most laggard Row heat treatment, sizing in the case of 130 DEG C can be prepared by fibroin microfilament fiber for 30～40 seconds.

In one embodiment of the invention, in the fibroin compounding agent solution that described step (2) obtains The preservative of interpolation ratio and antiseptic and mite-proof agent and VE the or VC auxiliary agent of 1-2% can also be added.

By technique scheme, the invention has the beneficial effects as follows：

Preparation process is simple of the present invention, convenience, it is necessary that the fibroin microfilament fiber prepared contains human body institute Several aminoacid, mineral, vitamin etc., there is the functions such as cosmetology, hypnotic.

Specific embodiment

In order that technological means, creation characteristic, reached purpose and effect that the present invention realizes are easy to understand, The present invention is further elucidated below.

Embodiment 1

The invention discloses a kind of preparation method of fibroin microfilament fiber, preparation method includes walking as follows Suddenly：

(1) pretreatment fibroin raw material：Mixing silk fiber raw material by 50/50 pelettes and cocoon Impurity in mixing silk fiber raw material is removed using steam-shrinkage machine；

(2) prepare fibroin compounding agent solution：The mixing silk fiber after the removal of impurity will be removed in step (1) Raw material is placed in the NaC03 aqueous solution of 0.6mol/L, wherein mixes silk fiber raw material：NaC03 is 1:1.3 Part by weight, then degumming 1.5 hours at a temperature of 85 DEG C, after the completion of degumming, silk fiber will be mixed Clean post-drying with water, and weigh；Then by the mixing silk fiber of degumming according to mixing silk fiber：Bromine Changing lithium is 1:0.6 part by weight, is dissolved in the lithium bromide water solution of 12mol/L, at a temperature of 40 DEG C Hydrolysis 5 hours, obtains fibroin lithium-bromide solution, dissolubility in water for the lithium bromide after the completion of hydrolysis Reduce with temperature and reduce, when solution is in saturation, solid brominated lithium crystallization precipitation obtains saturation silkworm silk Protein solution, this solution is loaded in dialysis sack, the lithium bromide in solution constantly carries out dialysis outside sack, Thus removing lithium bromide, being retained in dialysis sack is then fibroin compounding agent solution；In order that product is not Apt to deteriorate, reach the useful life of regulation, the interpolation of 1-2% can be added in fibroin compounding agent solution The preservative of ratio and antiseptic and mite-proof agent and VE or VC auxiliary agent；

(3) postfinishing process of microfilament fiber：Carried out using spray process or infusion process handling process, its Part is the part by weight using silicone oil and water is 1:10, the weight ratio of fibroin compounding agent solution and silicon oil solution For 1:9, spinning speed is 180m/min, and in bath, the dipping temperature of fibroin compounding agent solution is 35 DEG C, Dip time is 40 minutes, is then dried, and the temperature of drying is 95 DEG C；Finally carry out heat treatment, In the case of 130 DEG C, sizing can be prepared by fibroin microfilament fiber for 30 seconds.

Embodiment 2

(2) prepare fibroin compounding agent solution：The mixing silk fiber after the removal of impurity will be removed in step (1) Raw material is placed on the NaC0 of 0.6mol/L₃In aqueous solution, wherein mix silk fiber raw material：NaC0₃For 1:1.3 Part by weight, then degumming 1.5 hours at a temperature of 85 DEG C, after the completion of degumming, silk fiber will be mixed Clean post-drying with water, and weigh；Then by the mixing silk fiber of degumming according to mixing silk fiber：Bromine Changing lithium is 1:0.6 part by weight, is dissolved in the lithium bromide water solution of 12mol/L, at a temperature of 40 DEG C Hydrolysis 5 hours, obtains fibroin lithium-bromide solution, dissolubility in water for the lithium bromide after the completion of hydrolysis Reduce with temperature and reduce, when solution is in saturation, solid brominated lithium crystallization precipitation obtains saturation silkworm silk Protein solution, this solution is loaded in dialysis sack, the lithium bromide in solution constantly carries out dialysis outside sack, Thus removing lithium bromide, being retained in dialysis sack is then fibroin compounding agent solution；In order that product is not Apt to deteriorate, reach the useful life of regulation, the interpolation of 1-2% can be added in fibroin compounding agent solution The preservative of ratio and antiseptic and mite-proof agent and VE or VC auxiliary agent；

(3) postfinishing process of microfilament fiber：Carried out using spray process or infusion process handling process, its Part is the part by weight using silicone oil and water is 1:10, the weight ratio of fibroin compounding agent solution and silicon oil solution For 1:9, spinning speed is 180m/min, and in bath, the dipping temperature of fibroin compounding agent solution is 45 DEG C, Dip time is 40 minutes, is then dried, and the temperature of drying is 100 DEG C；Finally carry out heat treatment, In the case of 130 DEG C, sizing can be prepared by fibroin microfilament fiber for 40 seconds.

If the fibroin microfilament fiber softening that the present invention prepares will not be tacky and necessary containing human body Dry kind of aminoacid, mineral, vitamin etc., have the functions such as cosmetology, hypnotic；And fiber Cost is greatly reduced, and meets the principle of cost efficiency, and the quality of product meets first to close and requires simultaneously.

Ultimate principle and principal character and the advantages of the present invention of the present invention have been shown and described above.The industry Technical staff it should be appreciated that the present invention is not restricted to the described embodiments, in above-described embodiment and description Describe merely illustrates the principles of the invention, without departing from the spirit and scope of the present invention, the present invention Also have various changes and modifications, these changes and improvements both fall within scope of the claimed invention.This The claimed scope of invention is by appending claims and its equivalent thereof.

Claims

1. a kind of preparation method of fibroin microfilament fiber it is characterised in that：Described preparation method include as Lower step：

(1) pretreatment fibroin raw material：Will be former for the mixing silk fiber of pelettes and cocoon by 50/50 Material removes the impurity in mixing silk fiber raw material using steam-shrinkage machine；

(2) prepare fibroin compounding agent solution：The mixing silk fiber after the removal of impurity will be removed in step (1) Raw material is placed on the NaC0 of 0.6mol/L₃In aqueous solution, wherein mix silk fiber raw material：NaC0₃For 1:1.3 Part by weight, then degumming 1.5 hours at a temperature of 85 DEG C, after the completion of degumming, silk fiber will be mixed Clean post-drying with water, and weigh；Then by the mixing silk fiber of degumming according to mixing silk fiber：Bromine Changing lithium is 1:0.6 part by weight, is dissolved in the lithium bromide water solution of 12mol/L, at a temperature of 40 DEG C Hydrolysis 5 hours, obtains fibroin lithium-bromide solution, dissolubility in water for the lithium bromide after the completion of hydrolysis Reduce with temperature and reduce, when solution is in saturation, solid brominated lithium crystallization precipitation obtains saturation silkworm silk Protein solution, this solution is loaded in dialysis sack, the lithium bromide in solution constantly carries out dialysis outside sack, Thus removing lithium bromide, being retained in dialysis sack is then fibroin compounding agent solution；

(3) postfinishing process of microfilament fiber：Carried out using spray process or infusion process handling process, its Part is the part by weight using silicone oil and water is 1:10, the weight ratio of fibroin compounding agent solution and silicon oil solution For 1:9, spinning speed be 180m/min, in bath the dipping temperature of fibroin compounding agent solution be 35～ 45 DEG C, dip time is 40 minutes, is then dried, and the temperature of drying is 95～100 DEG C；The most laggard Row heat treatment, sizing in the case of 130 DEG C can be prepared by fibroin microfilament fiber for 30～40 seconds.

2. the preparation method of a kind of fibroin microfilament fiber according to claim 1, its feature exists In：The interpolation of 1-2% can also be added in the fibroin composite assistant solution that described step (2) obtains The preservative of ratio and antiseptic and mite-proof agent and VE or VC auxiliary agent.