CN105671663B - A kind of preparation method and applications of nettle extract protein compound additive - Google Patents

Abstract

The invention belongs to the technical field of functional fibers, and relates to a method for preparing a hemp extract protein composite additive, which is used to prepare cellulose fibers with both silk and hemp functions. Dextrin is stirred and adsorbed to obtain hemp extract-cyclodextrin powder; add hemp extract-cyclodextrin powder to the protein aqueous solution, stir evenly, and adjust the pH value, then cool down, and add transglutaminase And adjust the pH, filter after the reaction to get the hemp extract-cyclodextrin as the core material, and the protein as the microcapsule of the wall material; Foaming agent to prepare composite additives; protein and hemp extract are used as functional components to make cellulose fiber have both silk and hemp functions, and at the same time, the effect of imitating hemp structure is achieved by adding foaming agent. The effective components in the fiber The amount of loss during spinning and post-processing is reduced.

Description

Preparation method and application of a kind of hemp extract protein compound additive

technical field

The invention belongs to the technical field of functional fibers, and in particular relates to a method for preparing a hemp extract protein compound additive, which is used for the preparation of cellulose fibers with both silk and hemp functional characteristics.

Background technique

Today, when people are returning to nature and advocating green textiles, people not only put forward higher requirements for the comfort and beauty of textiles, but also prefer to use natural textiles. Therefore, middle and high-grade natural protein fiber and hemp fiber fabrics are getting more and more attention. . However, due to the limited output and high price of natural protein fibers such as silk and cashmere, it is difficult for the general public to accept; the hemp fiber is rough and hard, so it is not suitable to be directly used as raw materials for textiles. It needs to be processed by various processes, which increases the cost and increases the output. Slow and unable to meet actual needs.

Regenerated cellulose fiber has the characteristics of moisture absorption, good air permeability and comfortable wearing, and has been widely used. At the same time, due to the reduction of cultivated land and the depletion of oil resources, the production of natural fibers and synthetic fibers will be more and more restricted, so the application of regenerated cellulose fibers has obtained an unprecedented development opportunity.

In view of this, on the basis of the production and modification of regenerated cellulose fibers, the development of protein-modified cellulose fibers and hemp-modified cellulose fibers has entered a stage of rapid development and achieved certain results.

The Chinese patent No. ZL02138823.7 discloses a manufacturing method of soybean protein viscose fiber, which is to add soybean protein extracted from soybean meal to an aqueous solution of sodium hydroxide at a certain temperature and concentration to obtain a soybean protein liquid, and then press It is blended with viscose in a certain proportion, and after being molded in a coagulation bath in the form of injection before spinning, the silk cake is then hydroformylated to obtain soybean protein fiber; Chinese patent application number 200410010327.3 discloses a manufacturing method of soybean protein cellulose fiber It is produced by dissolving the isolated and purified soybean protein from soybeans in 1-5% sodium hydroxide aqueous solution at 40-60°C, adding an initiator and acrylamide for reaction, and then adding it to cellulose xanthate in proportion Soybean protein cellulose viscose filament and viscose short fiber; the Chinese patent No. ZL200610016426.1 discloses a modified viscose fiber and its manufacturing method, which is prepared silk protein solution, hydroxyethyl It is prepared by blending and spinning chitosan xanthate viscous solution and viscose; Chinese patent No. ZL200710097723.8 discloses a method for producing protein viscose fiber from animal protein and plant fiber, using animal hair, skin, etc. Make protein liquid as raw material, extract animal protein and co-spin with plant fiber. The Chinese patent with the patent number ZL200810136626.X discloses a method for manufacturing protein cellulose fibers. First, a protein solution is prepared, the protein solution is mixed with a viscose solution, and finally wet spinning is used. The Chinese patent No. ZL200810163379.2 discloses a milk protein viscose yarn and a preparation method thereof. The preparation method adopts the conventional wet spinning process and production equipment of viscose rayon, wherein the preparation of spinning comprises the following steps: a. Extract milk protein; b, dilute and purify the milk protein, adjust the pH value, put it into an electric mill or rubber mill for grinding; c, filter and concentrate the ground milk protein solution, and dry it to make milk protein powder, d, Adjust the pH value of the obtained milk protein powder solution water or the milk protein liquid obtained in step b, filter, and then fully mix with viscose liquid; Chinese patent No. 200810302306.7 discloses a protein viscose fiber and its The preparation method, the preparation method of the protein fiber comprises the following steps: A. degreasing, decolorizing and deodorizing animal and vegetable protein raw materials to obtain animal and vegetable protein powder; B. alkalization; dissolving the animal and vegetable protein powder in lye , to obtain a protein alkali solution; C, adding a cross-linking agent to the protein alkali solution to obtain a protein spinning solution; D, blending and spinning the protein spinning solution and viscose to obtain a protein filament; E, using a peroxidized The product solution is washed, upstream, and dried to obtain protein fibers; the Chinese patent application number 200710168521.8 discloses a soybean protein isolate/cellulose mixed solution and its preparation method and use, which is to disperse the soybean protein isolate in sodium hydroxide In the combined aqueous solution of soybean protein and urea, a soybean protein isolate solution is obtained, and then the protein solution is pre-cooled to a certain temperature, cellulose is added, stirred and dissolved to obtain a soybean protein isolate/cellulose mixed solution, and related applications are carried out. Chinese patent application number 200910048098.7 discloses a method for preparing soybean protein/cellulose composite fiber with high protein retention. In this method, a high-concentration cellulose solution is prepared by dissolving cellulose by using a mixed aqueous solution of sodium hydroxide/thiourea/urea as a solvent, and the soybean protein isolate is pretreated by a mixed aqueous solution of thiourea/urea and added to the obtained suspension The sodium hydroxide is directly dissolved to obtain the soybean protein solution; the composite solution obtained by mixing the cellulose solution and the soybean protein solution according to the proportion is degassed, spinned by a spinning machine, coagulated, drawn, washed, dried, and oiled. Soybean protein/cellulose composite fibers with excellent mechanical properties and high protein retention were prepared by winding. The Chinese patent with the application number 201110170688.4 discloses a collagen/cellulose composite fiber and its preparation method. It is to add the collagen solution to the cellulose viscose collagen solution, blend evenly and spin to obtain collagen/cellulose Plain composite fiber; Chinese patent application number 200910172139.3 discloses a peanut protein cellulose blended composite fiber and a preparation method thereof, including peanut protein isolate and cellulose. Its preparation method is as follows: (1) preparing peanut protein solution; (2) preparing cellulose solution; (3) fully mixing peanut protein solution and cellulose solution in proportion, then filtering through a plate and frame filter press, and vacuum static dehydration. After soaking, peanut protein cellulose blended fibers are prepared by wet spinning in a coagulation bath at room temperature; (4) the blended fibers are subjected to desulfurization, water washing, dehydration, acetal treatment, water washing, oiling, drying and compacting, Curl, style gets. The Chinese patent application number 200910154855.9 discloses a production method of regenerated silk protein fibers, which includes the following steps: washing and drying silk raw materials, then putting the above silk materials into lye, hydrolyzing the regenerated silk protein stock solution, drying After drying, the regenerated silk protein powder is obtained; the regenerated silk protein powder is added with water and stirred to obtain a saturated liquid of regenerated silk protein; the saturated liquid of regenerated silk protein: regenerated collagen liquid: auxiliary agent according to 10-50%: 85-45%: The ratio of 5% is mixed, and the regenerated silk protein fiber is obtained by spinning after mixing evenly. The Chinese patent whose patent number is ZL201110206559.6 discloses a kind of chicken feather regenerated protein viscose fiber and its preparation method and application. It is blended with viscose collagen liquid and spun by wet spinning technology; Chinese patent application number 201010184697.4 discloses milk protein blended regenerated cellulose fiber and its preparation process. It also dissolves milk casein into lye containing a cross-linking agent; Chinese patent No. ZL201110329457.3 discloses a preparation method of silk protein composite cellulose fiber, which is degummed waste silk Add it into the lithium bromide solution to prepare the silk protein solution, then add it to the sodium hydroxide solution of cellulose sulfonate to prepare the blend solution of silk protein and cellulose, and finally go through coagulation bath molding and post-treatment to obtain Silk protein composite cellulose fiber; the Chinese patent No. ZL200710097723.8 discloses a method for producing protein viscose fiber from animal protein and plant fiber. First, the leftovers of cow hair, pig hair or chicken feather are processed to obtain denatured protein Liquid, the denatured protein liquid is added to the mixing process of viscose fiber for production, and then it is cured by chromium salt treatment to obtain the finished product. The Chinese patent No. ZL201210033741.0 discloses a production process of wool protein composite viscose fiber. The present invention provides a production process of wool protein composite viscose fiber, which belongs to the field of viscose fiber. The wool protein viscose fiber is obtained through the preparation of the wool protein spinning solution, the blending of the wool protein solution and the viscose spinning solution, spinning, coagulation and solidification, and post-treatment procedures. The Chinese patent with the patent number ZL201210304512.8 discloses a preparation method of pupae protein cellulose composite viscose staple fiber spinning liquid, which is to dissolve pupae protein powder in sodium hydroxide solution, add protein denaturation aid after filtering Obtain pupal protein spinning solution, and then blend with viscose collagen solution for spinning; the Chinese patent No. ZL201220387021.4 discloses a preparation method of silk protein blended regenerated cellulose fiber, and the specific process is: (1) Degumming, swelling, drying and pulverizing the silk waste to obtain silk protein powder with a particle size of 0.1-0.5 microns, (2) dispersing the silk protein powder with sodium hydroxide solution, adding a dispersant and crosslinking (3) blending the mother liquor with cellulose viscose to obtain a blend glue, spinning and post-processing to obtain a silk protein blended regenerated cellulose fiber.

The Chinese patent application number 201110400581.4 discloses a regenerated animal micropowder protein cellulose fiber and its preparation method. The present invention discloses a regenerated animal micropowder protein cellulose fiber and its preparation method. The preparation includes the following steps: Add animal micropowder protein into the dispersant solution, stir evenly, and obtain 20-35wt% animal micropowder protein liquid after filtration; prepare viscose with cellulose pulp as raw material, and add denaturant in the dissolving step to obtain denatured viscose , the animal micropowder protein liquid is added to the denatured viscose according to the ratio of the animal micropowder to 1-30wt% of the weight of the finished fiber, and stirred evenly to prepare the animal micropowder blended viscose, which is introduced into the coagulation bath after defoaming and filtering Spinning and forming, and then the animal micropowder protein viscose fiber is obtained through filament drawing and post-processing steps. Chinese patent No. ZL200910153053.6 discloses silk protein blended regenerated cellulose fiber and its preparation process. The process of the present invention includes the following steps: (1) preparation of nano-scale silk protein powder; (2) preparation of cellulose fiber . Compared with the prior art, the present invention has the following beneficial effects: the present invention overcomes the difficulty of pulverizing and ultrafine silk protein powder, adopts self-developed nano-crushing equipment, and produces silk protein powder with a particle size within 50-100 nanometers up to 100%.

The above-mentioned patents mainly use protein to modify cellulose fibers. Combining the production technologies of these patents, there are mainly two production methods: (1) first dissolve animal or vegetable protein to obtain protein liquid, and then add it to traditional Wet spinning is carried out in the fiber production process; (2) Animal or vegetable protein is pretreated or pulverized and refined first, and then made into nano or micron protein powder by grinding, and then added to the viscous powder by blending modification. Glue for wet spinning molding. The method of dissolving protein into protein solution in production method (1) will completely destroy the original cavity structure of protein fibers. Combined treatment will inevitably use aldehydes for acetalization or heavy metals for denaturation and curing, which not only affects the quality of protein fibers, but also such toxic substances will cause serious environmental pollution. In the production method (2), the method of adding nano- or micron-shaped protein powder is adopted. Although the problems in the production method (1) are avoided, the protein powder still has swelling fibers in the viscose collagen solution, which affects the quality of the blend. Filtration performance seriously even affects the strength index and feel of the fiber.

The Chinese patent with the application number CN200610068481.5 discloses a method for preparing hemp viscose fiber using hemp plant as raw material and the hemp viscose fiber prepared by this method, the steps include the production steps of material preparation, cooking, beating and bleaching , impregnation, yellowing, spinning, etc., to obtain hemp viscose fiber. The patent number is ZL201010265600.2 Chinese patent discloses a preparation method of hemp viscose fiber, including: soaking hemp pulp, pressing and pulverizing to obtain alkali cellulose, the average degree of polymerization of the hemp pulp is 400-450; the alkali cellulose is yellowed, dissolved and filtered to obtain a spinning dope; the spinning dope is spun to obtain hemp viscose fiber. The Chinese patent No. ZL201310084726.3 discloses a preparation method of hemp stalk viscose fiber and its application. The preparation method of hemp stalk viscose fiber includes material preparation, dipping and pressing, crushing, aging, yellowing, Dissolving, filtering, defoaming, pre-spinning filtration, drawing and post-processing steps. The Chinese patent No. ZL201310084738.6 discloses a preparation method of ramie stalk antibacterial viscose fiber and its application. The preparation method of ramie stalk antibacterial viscose fiber includes pressing, crushing, soaking, degumming, acid-base treatment , cooking, pulping, post-processing and other steps. The Chinese patent with the patent number ZL200410004397.8 discloses a method for preparing hemp viscose pulp and functional fibers. The present invention relates to a process for producing viscose pulp and functional fibers using hemp. The directions include: Hemp material preparation→cutting→screening→washing→pretreatment→cooking→extruding→decompressing→desanding, concentrating→chlorination→alkali refining→bleaching→acid treatment→desanding, concentrating→copying→dipping→pressing→crushing → Aging → Yellowing → Grinding → Dissolving → Mixing → Pre-filtering → Filtration → Degassing → Filtration → Spinning → Drawing → Cutting → Post-processing → Drying → Packing to obtain functional viscose fibers. The Chinese patent with the patent number ZL200710130606.7 discloses a viscose fiber and a preparation method thereof. The present invention provides a viscose fiber prepared from industrial hemp as a raw material and a preparation method thereof. The method includes: preparing materials, cutting Material, flash explosion, pre-hydrolysis, cooking, selection, chlorination, bleaching, acid treatment, refining, copying, rubbing, impregnation, pressing, crushing, aging, yellowing, dissolution, mixing, filtration, defoaming, filtration, Spinning, cutting, refining, drying, and packaging to obtain viscose fibers prepared from industrial hemp. The Chinese patent application number 200810037072.8 discloses a method for producing viscose fiber from sisal leaves, which includes the following steps: (1) sorting sisal leaves; Scraping off the mesophyll gum of sisal leaves by shredding, washing with water to obtain rough sisal leaf cellulose fibers; (3) fermentation treatment in microbial mold solution, and hydrogen peroxide treatment to remove residual gum; (4) alkali cellulose Preparation; (5) yellowing and dissolving alkali cellulose to prepare spinning slurry; (6) defoaming spinning slurry; (7) wet spinning to obtain viscose fiber. The Chinese patent application number 201510176587.6 discloses a preparation method of viscose fiber containing Apocynum extract, comprising the following steps: preparation of antibacterial agent solution (adding Apocynum extract powder to water at a temperature of 25±1°C , the addition amount is 120g/1000ml water, stir fully until the powder is completely dissolved to make an antibacterial agent solution), add a dispersant, add sodium carboxymethylcellulose, blend with the spinning stock solution, spin, and post-treat to obtain Viscose with hemp extract. The Chinese patent with application number 201510433580.8 discloses a preparation method of hemp viscose mint fiber and socks, including: soaking hemp pulp, pressing and pulverizing to obtain alkali cellulose, and the average polymerization of hemp pulp The degree is 400-450; the alkali cellulose is subjected to yellowing treatment, then bamboo charcoal mint emulsion is added, and after dissolving and filtering, a spinning solution is obtained; the spinning solution is spun to obtain hemp viscose fiber. The Chinese patent with the patent number ZL201110066533.6 discloses a hemp viscose short fiber and its preparation method, which uses hemp as raw material to make hemp pulp, and then uses this pulp to produce viscose fiber to prepare The methods include pretreatment, water washing, cooking, washing, beating, sand removal, concentration, alkali refining, bleaching, acid treatment, washing, post-selection sand removal, concentration, copying, dipping, pressing, crushing, aging, yellowing, Grinding, dissolving, filtering, defoaming, filtering, spinning, drawing, cutting, post-processing, drying and packing, etc., to obtain hemp viscose staple fiber.

The above-mentioned patent is a production technology for preparing hemp modified cellulose fibers. It can be seen from these technologies that the preparation of the hemp modified cellulose fiber is mainly to prepare the hemp pulp first, and then use the hemp pulp to prepare the hemp viscose collagen solution by the viscose preparation process, and then spin. In the process of making hemp pulp or preparing hemp viscose collagen solution from hemp first, it needs to go through the process of concentrated alkali and high temperature, and the effective ingredients of hemp are too little, which seriously affects the performance of the fiber.

The foregoing patents only carry out a single modification to cellulose fibers, that is, either only protein modification or hemp modification. With the improvement of people's requirements for fabric comfort, more and more attention has been paid to the simultaneous modification of cellulose fibers with protein and hemp.

The Chinese patent with the application number 201410380285.6 discloses a silk and hemp cellulose fiber and its preparation method. The specific process includes: preparation of hemp pulp viscose spinning stock solution, preparation of protein dispersion emulsion, hemp pulp protein modified spinning stock solution preparation and post-spinning treatment, etc. Among them, the preparation of hemp pulp viscose spinning stock solution is hot and full of viscose technology, which uses strong alkali and takes a long time, which greatly damages the active ingredients in hemp pulp and affects the performance. At the same time, as an organic substance, the effect of using lye treatment, ceramic rollers, and star ball mills to grind and disperse protein is relatively poor.

Contents of the invention

The purpose of the present invention is to overcome the shortcoming that prior art exists, seek to design a kind of preparation method of hemp extract protein composite additive, the prepared hemp extract protein composite additive is used for preparing the cellulose fiber with silk, hemp function, The prepared cellulose fiber has the functions of silk and hemp in terms of functional components and structure, and reduces the loss of effective components in the fiber during the spinning process and post-treatment process.

In order to achieve the above object, the technical scheme adopted in the present invention is: a preparation method of hemp extract protein composite additive, comprising the following steps:

Step 1: Prepare hemp extract-cyclodextrin powder

Dissolve hemp extract at 40-60°C, prepare an aqueous solution of hemp extract with a mass fraction of 10%-20%, add cyclodextrin to the aqueous solution of hemp extract for stirring and adsorption, and the weight ratio of hemp extract to cyclodextrin The ratio is 2~5:1, the adsorption time is 20~50min, and then the solution is dried to obtain hemp extract-cyclodextrin powder;

Preferably, the hemp extract is from one or more of ramie, jute, flax, apocynum and kenaf, and is purchased from the market.

Step 2: Preparation of microcapsules with hemp extract-cyclodextrin as the core material and protein as the wall material

Prepare a protein aqueous solution with a mass fraction of 10.0% to 18.0%, and add the hemp extract-cyclodextrin powder prepared in step 1 to the protein aqueous solution, wherein the mass ratio of the hemp extract to the protein is 1 to 2:1 to 2. Stir evenly, and adjust the pH value to 3.5, then lower the temperature to 2.0°C, add transglutaminase and adjust the pH value to 8.0, and filter after 2 hours of reaction, that is, the hemp extract-cyclodextrin is used as the core material, and the protein Microcapsules as wall materials;

Preferably, the protein is one or more of gelatin, soybean protein isolate, wool protein or silk protein;

Preferably, the particle size D97 of the microcapsules with hemp extract-cyclodextrin as the core material and protein as the wall material is ≤ 3.000 μm.

Step 3: Prepare hemp extract protein complex additive

Add a foaming agent to the microcapsules prepared in step 2 with the hemp extract-cyclodextrin as the core material and the protein as the wall material to prepare a composite additive. The quality of the foaming agent is 1.0% of the quality of the hemp extract ~4.0%.

Preferably, the foaming agent is one of carbonate or bicarbonate;

Preferably, the blowing agent is one of sodium carbonate or sodium bicarbonate.

A preparation method of cellulose fibers with silk and hemp functions, comprising the following steps:

Step a: Preparation of blended spinning dope

Using cellulose pulp as raw material, through the known viscose preparation process, the viscose collagen solution is obtained. The content of cellulose A in the viscose collagen solution is 7.8%-9.2%; the pre-spinning injection equipment is used to add the viscose collagen solution. The hemp extract protein compound additive, the quality of the hemp extract and protein in the hemp extract protein compound additive is 4.0% to 12.0% of the quality of the first cellulose, and the blended spinning stock solution is prepared;

Step b: spinning and post-processing

The blended spinning stock solution is spun through an adjusted coagulation bath, and the as-spun tow is drawn to obtain a formed tow; the obtained formed tow is cut, eased desulfurization process, oiled bath, washed and dried, A cellulose fiber with both silk and hemp functions is obtained.

Preferably, the coagulation bath is 80-105 g/L of sulfuric acid and 260-295 g/L of sodium sulfate.

Preferably, the desulfurization bath: Na ₂ SO ₃ 2.0-8.0g/L, oil bath: 1.0-5.0g/L, no bleaching, drying temperature: 100-120°C, drying time 40-60min.

A cellulose fiber with silk and hemp functions, containing 2.0-5.0 wt% of protein and 2.0-5.0 wt% of hemp extract.

The beneficial effects of the present invention are:

(1) Using protein and hemp extract as functional components, the cellulose fiber has both silk and hemp functions, and at the same time, by adding a foaming agent, the fiber forms a hollow structure during the molding process to achieve a hemp-like structure The effect is that the prepared cellulose fiber has the functional characteristics of silk and hemp in terms of functional components and structure.

(2) Through the adsorption of cyclodextrin, microencapsulation and cross-linking and solidification of wall material protein, the loss of the effective components in the fiber - hemp extract and protein in the spinning process and post-processing process is reduced, The prepared functional viscose fiber has both the functional characteristics of silk and hemp.

(3) Compared with conventional viscose fiber, its bacteriostatic rate to Staphylococcus aureus ≥ 85.0%, the bacteriostatic rate to Escherichia coli ≥ 85.0%, the bacteriostatic rate to Candida albicans ≥ 80.0%, the fiber contains A variety of amino acids and trace elements have good hand feeling and skin care functions. The main physical indicators of the product can meet the requirements of first-class products in GB/T14463-2008 "Viscose Staple Fiber".

detailed description

The present invention will be further described below by specific embodiment:

Example 1

The preparation method of the hemp extract protein composite additive of the present embodiment comprises the following steps:

Step 1: Preparation of ramie extract-cyclodextrin powder

Dissolve the ramie extract at 40°C, prepare a ramie extract aqueous solution with a mass fraction of 10%, add cyclodextrin to the ramie extract aqueous solution for stirring and adsorption, and the weight ratio of ramie extract to cyclodextrin is 2:1, The adsorption time is 50min, and then the solution is dried to obtain ramie extract-cyclodextrin powder;

Step 2: Prepare microcapsules with ramie extract-cyclodextrin as core material and gelatin protein as wall material

Prepare a gelatin protein aqueous solution with a mass fraction of 10.0%, add the ramie extract-cyclodextrin powder prepared in step 1 into the gelatin protein aqueous solution, wherein the mass ratio of the ramie extract to the gelatin protein is 1:1, and stir evenly , and adjust the pH value to 3.5, then lower the temperature to 2.0°C, add transglutaminase and adjust the pH to 8.0, react for 2 hours and then filter, that is, the ramie extract-cyclodextrin is used as the core material, and the gelatin protein is used as the wall material The microcapsules; the particle size of the microcapsules with ramie extract-cyclodextrin as the core material and gelatin protein as the wall material is D97≤1.027μm.

Step 3: Prepare ramie extract gelatin protein compound additive

To the microcapsules prepared in step 2 with ramie extract-cyclodextrin as the core material and gelatin protein as the wall material, add foaming agent sodium carbonate to prepare a composite additive. The quality of the foaming agent sodium carbonate is extracted from ramie 1.0% by mass of substance.

A preparation method of cellulose fibers with silk and hemp functions, comprising the following steps:

Step a: Preparation of blended spinning dope

Using cellulose pulp as raw material, through the known viscose preparation process, the viscose solution is obtained, the content of cellulose A in the viscose solution is 9.2%; the ramie is added to the viscose solution by using pre-spinning injection equipment to extract Compound gelatin protein additive, the quality of ramie extract and gelatin protein in the ramie extract gelatin protein compound additive is 4.0% of the quality of a kind of cellulose, and prepares blended spinning stock solution;

Step b: spinning and post-processing

The blended spinning stock solution is spun through an adjusted coagulation bath, and the as-spun tow is drawn to obtain a formed tow; the obtained formed tow is cut, eased desulfurization process, oiled bath, washed and dried, Obtain cellulose fiber with both silk and hemp functions; coagulation bath is sulfuric acid 80g/L, sodium sulfate 260g/L; desulfurization bath: Na ₂ SO ₃ 2.0g/L, oil bath: 1.0g/L, without bleaching, drying Drying temperature: 100°C, drying time is 60min.

Embodiment 1 makes the cellulose fiber that specification is 1.11dtex * 38mm and has silk, hemp function concurrently, compared with conventional viscose fiber, its antibacterial rate to Staphylococcus aureus is 85.0%, and the antibacterial rate to Escherichia coli The rate is 85.0%, and the inhibition rate to Candida albicans is 80.0%. The fiber contains a variety of amino acid trace elements, and has a quasi-hollow structure, with good hand feeling and skin care function.

Example 2

The preparation method of the hemp extract protein composite additive of the present embodiment comprises the following steps:

Step 1: Preparation of Jute Extract-Cyclodextrin Powder

Dissolve jute extract at 45°C, prepare a jute extract aqueous solution with a mass fraction of 12%, add cyclodextrin to the jute extract aqueous solution for stirring and adsorption, the weight ratio of jute extract to cyclodextrin is 2:1, The adsorption time is 42min, and then the solution is dried to obtain jute extract-cyclodextrin powder;

Step 2: Preparation of microcapsules with jute extract-cyclodextrin as the core material and soybean protein isolate as the wall material

Preparation mass fraction is 12.2% soybean protein isolate aqueous solution, the jute extract-cyclodextrin powder that step 1 makes is added in soybean protein isolate solution, wherein the mass ratio of jute extract and soybean protein isolate is 1:2 , stir evenly, and adjust the pH value to 3.5, then lower the temperature to 2.0°C, add transglutaminase and adjust the pH value to 8.0, and filter after 2 hours of reaction, that is, jute extract-cyclodextrin is used as the core material, and soybeans are separated The microcapsule with protein as the wall material; the microcapsule with jute extract-cyclodextrin as the core material and soybean protein isolate as the wall material has a particle size D97≤1.236 μm.

Step 3: Prepare Jute Extract Soy Protein Isolate Complex Supplement

Take the jute extract-cyclodextrin prepared in step 2 as core material, add foaming agent sodium bicarbonate in the microcapsule of wall material, prepare composite additive, the quality of described foaming agent sodium bicarbonate 1.5% of the mass of jute extract.

A preparation method of cellulose fibers with silk and hemp functions, comprising the following steps:

Step a: Preparation of blended spinning dope

Using cellulose pulp as raw material, through the known viscose preparation process, the viscose solution is prepared, the content of cellulose A in the viscose solution is 8.8%; the jute extract is added to the viscose solution by using pre-spinning injection equipment Soybean protein isolate compound additive, the total mass of jute extract and soybean protein isolate compound additive in the jute extract soybean protein isolate compound additive is 5.5% of the A cellulose quality, and the blended spinning stock solution is prepared;

Step b: spinning and post-processing

The blended spinning stock solution is spun through an adjusted coagulation bath, and the as-spun tow is drawn to obtain a formed tow; the obtained formed tow is cut, eased desulfurization process, oiled bath, washed and dried, Obtain cellulose fiber with both silk and hemp functions; coagulation bath is sulfuric acid 86g/L, sodium sulfate 271g/L; desulfurization bath: Na ₂ SO ₃ 2.9g/L, oil bath: 1.6g/L, without bleaching, drying Drying temperature: 105°C, drying time is 55min.

Embodiment 2 makes the cellulose fiber that specification is 1.33dtex * 38mm concurrently with silk, fiber crops function, compared with conventional viscose fiber, its bacteriostatic rate to Staphylococcus aureus is 89.2%, to the bacteriostatic rate of Escherichia coli The rate is 90.1%, and the inhibition rate to Candida albicans is 86.5%. The fiber contains a variety of amino acid trace elements, and has a quasi-hollow structure, with good hand feeling and skin care function.

Example 3

The preparation method of the hemp extract wool protein composite additive of the present embodiment comprises the following steps:

Step 1: Preparation of Jute Extract-Cyclodextrin Powder

Dissolve hemp extract at 51°C, prepare an aqueous solution of hemp extract with a mass fraction of 14.5%, add cyclodextrin to the aqueous solution of hemp extract for stirring and adsorption, and the weight ratio of hemp extract to cyclodextrin is 3:1, The adsorption time is 35 minutes, and then the solution is dried to obtain hemp extract-cyclodextrin powder; the hemp extract is a combination of kenaf extract and flax extract in any proportion;

Step 2: Preparation of microcapsules with hemp extract-cyclodextrin as the core material and wool protein as the wall material

Prepare a wool protein aqueous solution with a mass fraction of 13.5%, add the hemp extract-cyclodextrin powder prepared in step 1 into the wool protein aqueous solution, wherein the mass ratio of the hemp extract to wool protein is 2:1, and stir evenly , and adjust the pH value to 3.5, then lower the temperature to 2.0°C, add transglutaminase and adjust the pH to 8.0, react for 2 hours and then filter, that is to say, hemp extract-cyclodextrin is used as the core material, and wool white matter is used as the wall material microcapsules; the particle size of the microcapsules with hemp extract-cyclodextrin as the core material and wool protein as the wall material is D97≤1.578μm.

Step 3: Prepare hemp extract wool protein complex additive

To the microcapsules prepared in step 2 with hemp extract-cyclodextrin as core material and wool protein as wall material, add foaming agent sodium bicarbonate to prepare composite additives. The quality of the foaming agent sodium bicarbonate is 2.1% by mass of hemp extract.

A preparation method of cellulose fibers with silk and hemp functions, comprising the following steps:

Step a: Preparation of blended spinning dope

Using cellulose pulp as raw material, through the known viscose preparation process, the viscose solution is obtained, the content of cellulose A in the viscose solution is 8.2%; the hemp is added to the viscose solution by pre-spinning injection equipment to extract Wool protein composite additive, the total mass of hemp extract and wool protein in the hemp extract wool protein composite additive is 8.2% of the first cellulose quality, and the blended spinning stock solution is prepared;

Step b: spinning and post-processing

The blended spinning stock solution is spun through an adjusted coagulation bath, and the as-spun tow is drawn to obtain a formed tow; the obtained formed tow is cut, eased desulfurization process, oiled bath, washed and dried, Obtain cellulose fiber with both silk and hemp functions; coagulation bath is sulfuric acid 91g/L, sodium sulfate 278g/L; desulfurization bath: Na ₂ SO ₃ 4.2g/L, oil bath: 2.7g/L, do not bleach, dry Drying temperature: 110°C, drying time is 51 minutes.

Embodiment 3 makes the cellulose fiber that specification is 1.56dtex * 38mm concurrently with silk, fiber crops function, compared with conventional viscose fiber, its bacteriostatic rate to Staphylococcus aureus is 93.2%, to the bacteriostatic rate of Escherichia coli The rate is 93.8%, and the inhibition rate to Candida albicans is 90.2%. The fiber contains a variety of amino acid trace elements, and has a quasi-hollow structure, with good hand feeling and skin care function.

Example 4

The preparation method of the apocynum extract silk protein composite additive of the present embodiment comprises the following steps:

Step 1: Prepare Apocynum extract-cyclodextrin powder

Dissolve the Apocynum apocynum extract at 55°C, prepare an aqueous solution of the Apocynum apocynum extract with a mass fraction of 18%, add cyclodextrin to the aqueous solution of the Apocynum apocynum extract and carry out stirring and adsorption, and the weight ratio of the apocynum apocynum extract to the cyclodextrin is 4:1, the adsorption time is 27min, and then the solution is dried to obtain Apocynum extract-cyclodextrin powder;

Step 2: Prepare microcapsules with Apocynum extract-cyclodextrin as the core material and silk protein as the wall material

Prepare a silk protein aqueous solution with a mass fraction of 15.9%, add the Apocynum extract-cyclodextrin powder prepared in step 1 into the silk protein aqueous solution, wherein the mass ratio of the Apocynum extract to silk protein is 1:1, Stir evenly, and adjust the pH value to 3.5, then lower the temperature to 2.0°C, add transglutaminase and adjust the pH value to 8.0, and filter after 2 hours of reaction, that is to say, Apocynum extract-cyclodextrin is used as the core material, silk protein The microcapsules are wall materials; the microcapsules with Apocynum extract-cyclodextrin as the core material and silk protein as the wall material have a particle size D97≤1.925 μm.

Step 3: Prepare apocynum extract silk protein compound additive

To the microcapsules prepared in step 2 with Apocynum extract-cyclodextrin as core material and silk protein as wall material, add foaming agent sodium bicarbonate to prepare composite additives, the quality of the foaming agent sodium bicarbonate It is 2.9% of the quality of Apocynum apocynum extract.

A preparation method of cellulose fibers with silk and hemp functions, comprising the following steps:

Step a: Preparation of blended spinning dope

Using cellulose pulp as raw material, through the known viscose preparation process, the viscose solution is obtained, the content of cellulose A in the viscose solution is 7.8%; the pre-spinning injection equipment is used to add the apocynum to the viscose solution Extract silk protein compound additive, the total mass of Apocynum extract and silk protein in the compound additive of Apocynum extract and silk protein is 10.3% of the mass of A cellulose, and prepare the blended spinning stock solution;

Step b: spinning and post-processing

The blended spinning stock solution is spun through an adjusted coagulation bath, and the as-spun tow is drawn to obtain a formed tow; the obtained formed tow is cut, eased desulfurization process, oiled bath, washed and dried, Obtain cellulose fiber with both silk and hemp functions; coagulation bath is sulfuric acid 99g/L, sodium sulfate 286g/L; desulfurization bath: Na ₂ SO ₃ 5.9g/L, oil bath: 4.2g/L, do not bleach, dry Drying temperature: 116°C, drying time is 45 minutes.

Embodiment 4 makes the cellulose fiber that specification is 1.67dtex * 38mm concurrently with silk, hemp function, compared with conventional viscose fiber, its bacteriostatic rate to Staphylococcus aureus is 96.8%, to the bacteriostatic rate of Escherichia coli The rate is 97.2%, and the inhibition rate to Candida albicans is 95.3%. The fiber contains a variety of amino acid trace elements, and has a quasi-hollow structure, with good hand feeling and skin care function.

Example 5

The preparation method of the kenaf extract protein composite additive of the present embodiment may further comprise the steps:

The preparation method of the kenaf extract silk protein composite additive of the present embodiment comprises the following steps:

Step 1: Preparation of kenaf extract-cyclodextrin powder

Dissolve kenaf extract at 60°C, prepare an aqueous solution of kenaf extract with a mass fraction of 20%, add cyclodextrin to the aqueous solution of kenaf extract for stirring and adsorption, and the weight ratio of kenaf extract to cyclodextrin is 5:1, the adsorption time is 20min, and then the solution is dried to obtain kenaf extract-cyclodextrin powder;

Step 2: Preparation of microcapsules with kenaf extract-cyclodextrin as core material and silk protein as wall material

Preparation mass fraction is 18% silk protein aqueous solution, the kenaf extract-cyclodextrin powder that step 1 makes is added in the silk protein aqueous solution, wherein the mass ratio of kenaf extract and silk protein is 2:1, Stir evenly, and adjust the pH value to 3.5, then lower the temperature to 2.0°C, add transglutaminase and adjust the pH value to 8.0, react for 2 hours and then filter to obtain kenaf extract-cyclodextrin as the core material and silk protein The microcapsule is a wall material; the microcapsule with kenaf extract-cyclodextrin as a core material and silk protein as a wall material has a particle size D97≤2.328 μm.

Step 3: Prepare kenaf extract and silk protein compound additive

To the microcapsules prepared in step 2 with kenaf extract-cyclodextrin as the core material and silk protein as the wall material, add foaming agent sodium bicarbonate to prepare a composite additive. The quality of the foaming agent sodium bicarbonate It is 4.0% of the quality of kenaf extract.

A preparation method of cellulose fibers with silk and hemp functions, comprising the following steps:

Step a: Preparation of blended spinning dope

Using cellulose pulp as raw material, through the known viscose preparation process, the viscose solution is prepared, the content of cellulose A in the viscose solution is 8.9%; the kenaf is added to the viscose solution by using pre-spinning injection equipment Extract silk protein composite additive, the total mass of kenaf extract and silk protein in the kenaf extract silk protein composite additive is 12% of the quality of the first cellulose, and prepare the blended spinning stock solution;

Step b: spinning and post-processing

The blended spinning stock solution is spun through an adjusted coagulation bath, and the as-spun tow is drawn to obtain a formed tow; the obtained formed tow is cut, eased desulfurization process, oiled bath, washed and dried, Obtain cellulose fiber with both silk and hemp functions; coagulation bath is sulfuric acid 105g/L, sodium sulfate 295g/L; desulfurization bath: Na ₂ SO ₃ 8.0g/L, oil bath: 5.0g/L, without bleaching, drying Drying temperature: 120°C, drying time is 40min.

Embodiment 4 makes the cellulose fiber that specification is 2.22dtex * 56mm concurrently with silk, fiber crops function, compared with conventional viscose fiber, its bacteriostatic rate to Staphylococcus aureus is 99.1%, to the bacteriostatic rate of Escherichia coli The rate is 99.0%, and the inhibition rate to Candida albicans is 98.5%. The fiber contains a variety of amino acid trace elements, and has a hollow structure, with good hand feeling and skin care function.

Claims (7)

1. A kind of 1. preparation method with silk, the cellulose fibre of numb function, it is characterised in that：Including preparing nettle extract albumen Matter compound additive；It is described to prepare nettle extract protein compound additive, comprise the following steps：

   Step 1：Prepare nettle extract-cyclodextrin powder

   Nettle extract is dissolved at 40~60 DEG C, the nettle extract aqueous solution that mass fraction is 10%-20% is prepared, is extracted to fiber crops Cyclodextrin is added in the thing aqueous solution and is stirred absorption, the weight ratio of nettle extract and cyclodextrin is 2~5：1, adsorption time is 20~50min, then the solution is dried, obtain nettle extract-cyclodextrin powder；

   Step 2：Prepare using nettle extract-cyclodextrin as core, protein is the microcapsules of wall material

   The protein aqueous solution that mass fraction is 10.0%~18.0% is prepared, by nettle extract-cyclodextrin powder made from step 1 Body is added in protein aqueous solution, and wherein the mass ratio of nettle extract and protein is 1~2:1~2, stir, and adjust It is 3.5 to save pH value, is then cooled to 2.0 DEG C, and it is 8.0 to add transglutaminase and adjust pH, is filtered after reacting 2h, i.e., It is core to be able to nettle extract-cyclodextrin, and protein is the microcapsules of wall material；

   Step 3：Prepare nettle extract protein compound additive

   To step 2 preparation using nettle extract-cyclodextrin as core, protein is made to add foaming agent in the microcapsules of wall material For compound additive is gone out, the quality of the foaming agent is the 1.0%~4.0% of nettle extract quality；

   Described foaming agent is one kind in carbonate or bicarbonate；

   The preparation method, including prepare co-blended spinning stoste, spinning and post processing；

   Described to prepare co-blended spinning stoste, the quality of nettle extract and protein is first in nettle extract protein compound additive The 4.0%~12.0% of kind cellulose quality；

   The spinning, coagulating bath are 80~105g/L of sulfuric acid, 260~295g/L of sodium sulphate.
2. 2. the preparation method according to claim 1 with silk, the cellulose fibre of numb function, it is characterised in that：It is described Nettle extract comes from the one or several kinds in ramie, jute, flax, bluish dogbane and bluish dogbane.
3. 3. the preparation method according to claim 1 with silk, the cellulose fibre of numb function, it is characterised in that：It is described Protein be one or more of in gelatin, soybean protein isolate, wool protein or fibroin.
4. 4. the preparation method according to claim 1 with silk, the cellulose fibre of numb function, it is characterised in that：It is described Using nettle extract-cyclodextrin as core, protein for wall material microcapsules particle diameter D97≤3.000 μm.
5. 5. the preparation method according to claim 1 with silk, the cellulose fibre of numb function, it is characterised in that including Following steps：

   Step a：Prepare co-blended spinning stoste

   Using cellulose pulp as raw material, by known viscose glue preparation section, viscose glue stoste is made, alpha cellulose in viscose glue stoste Content be 7.8%-9.2%；Nettle extract as claimed in claim 1 is added into viscose glue stoste using injection device before spinning Protein compound additive, co-blended spinning stoste is made；

   Step b：Spinning and post processing

   The co-blended spinning stoste is subjected to spinning by the coagulating bath adjusted, nascent tow obtains shaping silk after drawing-off Beam；Gained is molded tow after cutting off, relaxing sulfur removal technology, finish application bath, washing and drying, obtains having silk, numb function concurrently Cellulose fibre.
6. 6. the preparation method according to claim 5 with silk, the cellulose fibre of numb function, it is characterised in that described Desulfurization is bathed：Na₂SO₃2.0~8.0g/L, oil bath：1.0~5.0g/L, do not bleach, drying temperature：100~120 DEG C, drying time For 40~60min.
7. 7. it is a kind of it is as claimed in claim 1 with silk, the cellulose fibre of numb function preparation method prepared by with silk, The cellulose fibre of numb function, it is characterised in that：Protein containing 2.0~5.0wt%, 2.0~5.0wt% fiber crops extraction Thing.