CN105803568A - Preparation method of silk protein fibers - Google Patents

Abstract

The invention discloses a preparation method of silk protein fibers. The preparation method comprises the following steps of: (1) after peeling off cocoon shells into fragments, degumming a sodium carbonate solution with the mass percent of 3% for three times, and putting the fragments into a vacuum drying box at the temperature of 75 DEG C and drying; then dissolving dried silk protein into a 1.5wt% NaOH solution; (2) carrying out slicing treatment on tree raw materials, and boiling, finely selecting before bleaching, bleaching, finely selecting after bleaching, pulping, dehydrating and drying to prepare pulp; (3) filling the pulp and liquid-state NMMO (Methylmorpholine-N-Oxide) into a mixing kneading tank and heating the mixture at vacuum to 90 DEG C, so as to prepare a spinning solution with the cellulose concentration of 10%-25%; and (4) proportioning and commixing a silk protein solution in the step (1) and the spinning solution in the step (3), and adding a nano aromatic auxiliary agent and spinning by adopting a dry-wet-method process. The silk protein fibers provided by the invention have soft luster and a smooth and soft hand feeling of real silk, and also keep good moisture absorption and high fiber strength of natural silk; and the silk protein fibers are more skin-friendly and comfortable.

Description

A kind of preparation method of fibroin fiber

Technical field

The preparation method that the present invention relates to a kind of fiber, the preparation method being specifically related to a kind of fibroin fiber.

Background technology

Silkworm silk is one of native protein of utilizing the earliest of the mankind, enjoys the good reputation of " fiber queen ".At present, China is domestic silkworm silk and the maximum country of tussah silk yield in the world, and silkworm Raw Silk Production accounts for world's half.The silkworm silk of the overwhelming majority is all used as textile material all the time.The exploitation of silkworm silk gradually extend to the fields such as food, fermentation industry new material, bio-pharmaceuticals, clinical conditions, environmental conservation, utilization of energy, medical material and cosmetics.Fibroin has better Biodegradable and biocompatibility, is excellent natural biologic material, and along with constantly improving and ripe of process technology, fibroin will have broader practice prospect as new ep-type material.

Silkworm silk is made up of fibroin albumen (Fibroin) and sericin (Sericin) two parts.Fibroin albumen is the key component in silkworm silk, accounts for the 70% of quality, and sericin wraps in the outside of fibroin albumen, accounts for the 25% of quality, additionally contains the impurity of about 5%.Fibroin and sericin all contain 18 seed amino acids including essential amino acid.The main component of fibroin is glycine, alanine, tyrosine, serine；Sericin then contains substantial amounts of serine, aspartic acid, glutamic acid, next to that glycine, threonine and lysine etc..In sericin, hydrophilic aminoacid is more than hydrophobic aminoacid；And hydrophilic aminoacid is less than hydrophobic aminoacid in fibroin.Fibroin is also containing multiple inorganic elementss such as the potassium less than 0.7%, calcium, silicon, strontium, phosphorus, ferrum and copper.

Protein component in fiber and human body have the good compatibility, and its fiber and fabric have stronger leads wet, hygroscopicity, and the functions such as glossiness is good, uvioresistant, sense comfortable and easy to wear is strong.

Tencel is referred to as " 21st century green fiber ", absolutely natural material, manufacturing process environmental protection; allow life style with conservation of nature environment for this; cater to the demand of modern consumer completely, tencel is nontoxic, pollution-free, product use after bio-degradable, will not to environment.Tencel has concurrently outside the advantages such as the excellent hygroscopicity of plain edition viscose rayon, soft and smooth elegant property, comfortableness, overcomes common viscose fiber brute force low, and especially wet defect low by force, its brute force is almost close with terylene.

There is presently no a kind of can in conjunction with the fiber of both premium properties above-mentioned.

Summary of the invention

The present invention is to solve above-mentioned technical problem, thus the preparation method that a kind of fibroin fiber is provided.

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

The preparation method of a kind of fibroin fiber, comprises the steps:

(1) after silkworm cocoon stripping being fragmentated, with the sodium carbonate liquor degumming that mass fraction is 3% 3 times, boiling 30min in a water bath, bath raio remains 1:50 every time；Fully clean up with distilled water after degumming, be placed in the vacuum drying oven that temperature is 75 DEG C and dry, then the fibroin of drying is dissolved in the NaOH solution that mass fraction is 1.5%, is configured to the fibroin solutions that protein content is 13%；

(2) tree wood raw material is removed joint slicing treatment through peeling, then after bleaching selected before steaming and decocting drift is floated, make pulp after selected papermaking dewatered drying；

(3) being incorporated with together with liquid NMMO in screw rod and heatable mixer kneader tank by the pulp in step (2), heat under vacuo to 90 DEG C, heat time heating time is 3-4h, prepares the spinning solution that cellulose concentration is 10%-25%；

(4) by blended with the spinning solution proportioning in step (3) for the fibroin solutions in step (1), and add nanometer fragrant auxiliary agent, then adopt wet-dry change technique spinning, carry out washing cut-out post processing after spinning and dry packing.

In a preferred embodiment of the invention, described fibroin solutions is 10%-20%:90%-80% with the ratio of spinning solution.

In a preferred embodiment of the invention, described nanometer fragrant auxiliary agent proportion is 3%-5%.

In a preferred embodiment of the invention, the spinning process in step (4) is as follows:

Entering before coagulating bath the dry-spinning distance through 10-300mm through the silk of spinning ejection, unformed fiber thread is at this stage stretch orientation；After dry-spinning, fiber finer flows into molding in NMMO-H2O coagulating bath.

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

The feel of soft gloss and smooth softness as the existing real silk of the present invention, maintains again the good hygroscopicity of tencel and high-tenacity, and pro-skin is comfortable more.

The present invention can improve surrounding air environment, and helps for sleep, and improves sleep quality so that mood is happier, is greatly improved class and the added value of product.

Accompanying drawing explanation

In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.

Fig. 1 is the preparation flow figure of spinning solution；

Fig. 2 is the preparation flow figure of spinning process.

Detailed description of the invention

For the technological means making the present invention realize, creation characteristic, reach purpose and effect and be easy to understand, below in conjunction with being specifically illustrating, the present invention is expanded on further.

The preparation method of a kind of fibroin fiber provided by the invention, it comprises the steps:

(1) after silkworm cocoon stripping being fragmentated, with the sodium carbonate liquor degumming that mass fraction is 3% 3 times, boiling 30min in a water bath, bath raio remains 1:50 every time；Fully clean up with distilled water after degumming, be placed in the vacuum drying oven that temperature is 75 DEG C and dry, then the fibroin of drying is dissolved in the NaOH solution that mass fraction is 1.5%, is configured to the fibroin solutions that protein content is 13%；

(2) tree wood raw material is removed joint slicing treatment through peeling, then after bleaching selected before steaming and decocting drift is floated, make pulp after selected papermaking dewatered drying；

(3) pulp in step (2) is incorporated with together with liquid NMMO in screw rod and heatable mixer kneader tank, heat under vacuo to 90 DEG C, heat time heating time is 3-4h, prepares the spinning solution (referring to Fig. 1) that cellulose concentration is 10%-25%；

(4) by blended with the spinning solution proportioning in step (3) for the fibroin solutions in step (1), and add nanometer fragrant auxiliary agent, then adopt wet-dry change technique spinning, carry out washing (NMMO washing away in spinning) after spinning and cut off (by long fibre cutting short-forming fiber) post processing (chopped fiber after cutting off is carried out, bleaches and is oiled) dry (evaporation moisture content) packing (referring to Fig. 2).

Wherein, the ratio of fibroin solutions and spinning solution is 15%:85%, and nanometer fragrant auxiliary agent proportion is 4%, and the spinning process in step (4) is as follows:

Entering before coagulating bath the dry-spinning distance through 10-300mm through the silk of spinning ejection, unformed fiber thread is at this stage stretch orientation；After dry-spinning, fiber finer flows into molding in NMMO-H2O coagulating bath.

Referring to Fig. 2, due to the NMMO solvent in production process purified after can reclaim for dissolution process from spinning workshop section, the response rate of NMMO may be up to more than 99%, so can be recycled, and is greatly saved cost.

By the fibroin fiber that said method is made, its fabric made is adopted to reach:

Size changing rate: warp-wise-3.0%, broadwise-3.0%；

Powerful: >=250N；

Dyefastness: washable (variable color, staining) >=3 grades；

Rub resistance >=3 grade；

Content of formaldehyde: < 75mg/kg.

The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; described in above-described embodiment and description is that principles of the invention is described; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within the claimed scope of the invention.Claimed scope is defined by appending claims and equivalent thereof.

Claims (4)

1. the preparation method of a fibroin fiber, it is characterised in that comprise the steps:

(1) after silkworm cocoon stripping being fragmentated, with the sodium carbonate liquor degumming that mass fraction is 3% 3 times, boiling 30min in a water bath, bath raio remains 1:50 every time；Fully clean up with distilled water after degumming, be placed in the vacuum drying oven that temperature is 75 DEG C and dry, then the fibroin of drying is dissolved in the NaOH solution that mass fraction is 1.5%, is configured to the fibroin solutions that protein content is 13%；

(2) tree wood raw material is removed joint slicing treatment through peeling, then after bleaching selected before steaming and decocting drift is floated, make pulp after selected papermaking dewatered drying；

(3) being incorporated with together with liquid NMMO in screw rod and heatable mixer kneader tank by the pulp in step (2), heat under vacuo to 90 DEG C, heat time heating time is 3-4h, prepares the spinning solution that cellulose concentration is 10%-25%；

(4) by blended with the spinning solution proportioning in step (3) for the fibroin solutions in step (1), and add nanometer fragrant auxiliary agent, then adopt wet-dry change technique spinning, carry out washing cut-out post processing after spinning and dry packing.

2. the preparation method of a kind of fibroin fiber according to claim 1, it is characterised in that the ratio of described fibroin solutions and spinning solution is 10%-20%:90%-80%.

3. the preparation method of a kind of fibroin fiber according to claim 1, it is characterised in that described nanometer fragrant auxiliary agent proportion is 3%-5%.

4. the preparation method of a kind of fibroin fiber according to claim 1, it is characterised in that the spinning process in step (4) is as follows:

Entering before coagulating bath the dry-spinning distance through 10-300mm through the silk of spinning ejection, unformed fiber thread is at this stage stretch orientation；After dry-spinning, fiber finer flows into molding in NMMO-H2O coagulating bath.