CN105671663A - Preparation method and application of hemp extract and protein composite additive - Google Patents
Preparation method and application of hemp extract and protein composite additive Download PDFInfo
- Publication number
- CN105671663A CN105671663A CN201610070489.9A CN201610070489A CN105671663A CN 105671663 A CN105671663 A CN 105671663A CN 201610070489 A CN201610070489 A CN 201610070489A CN 105671663 A CN105671663 A CN 105671663A
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- protein
- preparation
- nettle extract
- extract
- cyclodextrin
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- 230000000996 additive effect Effects 0.000 title claims abstract description 47
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/20—Composition of the spinning solution or the bath for the manufacture of hollow threads
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the technical field of functional fibers and relates to a preparation method of a hemp extract and protein composite additive. The preparation method is used for preparing cellulosic fiber with functions of silk and hemp; firstly, a hemp extract water solution is prepared, cyclodextrin is added to the hemp extract water solution to be stirred for absorption, and hemp extract-cyclodextrin powder is obtained; the hemp extract-cyclodextrin powder is added to a protein water solution, the mixture is uniformly stirred, the pH value is adjusted, the mixture is cooled, transglutaminase is added, the pH is adjusted, the mixture is filtered after reaction, and a microcapsule with hemp extract-cyclodextrin as a core material and protein as a wall material is obtained; a foaming agent is added to the microcapsule with hemp extract-cyclodextrin as the core material and protein as the wall material, and the composite additive is prepared; the protein and the hemp extract are taken as functional components, so that the cellulosic fiber has functions of silk and hemp; besides, the foaming agent is added, the effect of a hemp-simulating structure is obtained, and the loss quantity of effective components in the fiber is reduced in the spinning process and aftertreatment process.
Description
Technical field
The invention belongs to functional fibre technical field, specifically, it relates to the preparation method of a kind of Nettle extract protein composite additive, for having the preparation of the cellulosic fibre of silk, fiber crops functional character concurrently.
Background technology
At people's back to nature, advocate today of green textiles, the comfortable aesthetic property of textiles is not only had higher requirement by people, and prefers to use natural fabric, and therefore medium-to-high grade natural protein fiber and flaxen fiber fabric are more and more subject to people's attention. But owing to natural protein fiber is as limited in silk, cashmere equal yield line, and expensive so that ordinary populace is difficult to accept; Flaxen fiber quality is thick and stiff, should not directly take the raw material of weaving, it is necessary to carry out kinds of processes process, increases cost, and output increases slowly, can not practical requirement.
Regenerated cellulose fibre has moisture absorption, good permeability, and feature comfortable and easy to wear, obtains a wide range of applications. Simultaneously due to the minimizing in arable land and the day by day exhausted of petroleum resources, the restriction that the output of natural fiber, synthon will be got more and more, therefore the application of regenerated cellulose fibre has obtained a unprecedented opportunity to develop.
Given this, regenerated cellulose fibre produce and modification basis on, the exploitation of protein modified cellulose fibre and fiber crops modified cellulose fibre is entered stage of high speed development by people, and achieves certain achievement.
The patent No. is the manufacture method that the Chinese patent of ZL02138823.7 discloses a kind of soybean protein viscose fiber, it be by from dregs of beans extract soy-protein join certain temperature, the aqueous sodium hydroxide solution of concentration obtain soybean protein solution, then carry out blended with viscose glue by a certain percentage, employing spin front injection form precipitation bath shaping after, spinning cake again through hydroformylation process obtain soybean fiber; Application number be 200410010327.3 Chinese patent disclose the manufacture method of a kind of soybean fiber cellulose fiber, it be the soy-protein being separated purification in soybean is dissolved in 40-60 DEG C, concentration be 1-5% aqueous sodium hydroxide solution in, add initiator and acrylamide react after add in proportion in cellulose xanthate and produce soybean fiber cellulose viscose filament and viscose staple fibre;The Chinese patent that the patent No. is ZL200610016426.1 discloses a kind of modified viscose fiber and manufacture method thereof, and it is prepared from obtained fibroin solution, hydroxyethyl chitosan xanthate viscous soln and viscose glue blending spinning; The Chinese patent that the patent No. is ZL200710097723.8 discloses a kind of animal proteinum and vegetable fibre manufacture protein cellulose viscose method, utilizes animal wool, skin etc. to make protein liquid as raw material, and extraction animal protein and vegetable fibre spin altogether. The patent No. is the manufacture method that the Chinese patent of ZL200810136626.X discloses a kind of protein cellulose fiber, first produces protein soln, is mixed with viscose solution by described protein soln, finally adopts wet-spinning and becomes. The Chinese patent that the patent No. is ZL200810163379.2 discloses a kind of cow milk protein viscose and its preparation method, its preparation method adopts the conventional wet spinning process of viscose rayon and production unit, and wherein the preparation of spinning comprises the following steps: a, extraction cow's milk protein; Cow's milk protein after b, dilution purification, adjust ph, puts into electric mill machine or rubber mill grinding; C, by grinding after milk protein liquid filtering and concentrating, cow's milk protein powder is made in drying, d, by obtained cow's milk protein powder solution water or adopt b step gained milk protein liquid, adjust ph, filter, then fully mix with viscose; The patent No. be 200810302306.7 Chinese patent disclose a kind of protein cellulose viscose and its preparation method, the preparation method of this thiozell comprises the following steps: A, by animal and plant protein raw materials degreasing, decolouring, deodorizing, obtain animal and plant protein powder; B, alkalization; Animal and plant protein powder is dissolved in alkali lye, obtains albumen alkaline solution; C, in albumen alkaline solution, add linking agent, obtain albumen spinning solution; D, by albumen spinning solution and viscose glue blending spinning, obtain Protein filament; E, by Protein filament peroxide solutions washing, upstream, oven dry, obtain thiozell; Application number be 200710168521.8 Chinese patent disclose a kind of soybean separation protein/cellulose mixed and its production and use, it is scattered in by soybean protein isolate in the combination solution of sodium hydroxide and urea, obtain soybean protein isolate solution, then this protein liquid is pre-chilled to certain temperature, add Mierocrystalline cellulose, stirring and dissolving obtains the mixing solutions of soybean protein isolate/Mierocrystalline cellulose, thus carries out related application. Application number be 200910048098.7 Chinese patent disclose a kind of protein recoverable amount high soybean protein/cellulose composite fiber preparation method. By adopting, sodium hydroxide/thiocarbamide/urea mixed aqueous solution carrys out, as solvent, the cellulose solution that dissolving cellulos prepares high density to the method, and adds sodium hydroxide after soybean protein isolate being carried out pre-treatment by thiocarbamide/urea mixed aqueous solution in gained suspension and directly dissolve and obtain soy bean proteinous soln; Cellulose solution and soy bean proteinous soln are proportionally uniformly mixed the composite solution that obtains again through deaeration, spinning-drawing machine spray silk, solidify, drawing-off, washing, drying, prepare, through winding, soybean protein/cellulose composite fiber that mechanical property is excellent, protein recoverable amount is high after oiling process. Application number be 201110170688.4 Chinese patent disclose a kind of collagen protein/cellulose composite fiber and its preparation method, it is joined by collagen solution in Mierocrystalline cellulose viscose glue stoste, blended evenly after carry out spinning and obtain collagen protein/cellulose composite fiber;Application number be 200910172139.3 Chinese patent disclose a kind of blend composite fiber of peanut protein cellulose and preparation method, comprise peanut protein isolate and Mierocrystalline cellulose. Its preparation method is: (1) preparation Semen arachidis hypogaeae protein solution; (2) cellulose solution is prepared; (3) by fully mixed even in proportion to Semen arachidis hypogaeae protein solution and cellulose solution, then filter through plate-and-frame filter press, after vacuum discontinuous degassing, under room temperature, in precipitation bath, prepare peanut protein cellulose blended fiber by wet spinning process; (4) blended fiber process through desulfurization, washing, dehydration, acetal, wash, oil, dry fine and close, curling, shaping obtains. Application number be 200910154855.9 Chinese patent disclose the production method of a kind of regenerated fibroin fiber, comprise the following steps: silk raw material is washed post-drying, then above-mentioned silk material is put into alkali lye, it is hydrolyzed to obtain regenerated fibroin stoste, obtained regenerated fibroin powder after oven dry; The stirring that obtained regenerated fibroin powder added water obtains the saturated liquid of regenerated fibroin; By saturated for regenerated fibroin liquid: reclaimed rubber stoste: auxiliary agent mixes in the ratio of 10-50%:85-45%:5%, mix the obtained regenerated fibroin fiber of rear spinning. The Chinese patent that the patent No. is ZL201110206559.6 discloses a kind of chicken feather regenerated protein viscose fiber and its preparation method and application, it is by useless chicken feather pre-treatment (comprise sig water hydrolysis or make hydrolysis chicken feather protein powder), then with viscose glue dope blending, wet spinning technology is utilized to carry out spinning; Application number be 201010184697.4 Chinese patent disclose milk protein blending regenerating cellulose fiber and preparation technology thereof. It is also add milk casein food grade in the alkali lye containing linking agent to dissolve; The patent No. is the preparation method that the Chinese patent of ZL201110329457.3 discloses a kind of fibroin composite cellulose fiber, it is joined after degumming process in lithium-bromide solution by waste and old silk, prepare fibroin solution, then joined in the sodium hydroxide solution of Mierocrystalline cellulose sulfonate, the blend solution of obtained fibroin and Mierocrystalline cellulose,, aftertreatment shaping finally by precipitation bath, obtains fibroin composite cellulose fiber; The Chinese patent that the patent No. is ZL200710097723.8 discloses a kind of animal proteinum and the method for vegetable fibre manufacture protein cellulose viscose, first metaprotein liquid is obtained after being processed by the tankage of ox hair, pig hair or chicken feather, metaprotein liquid is joined in the mixed processes of viscose fiber and produces, after through chromic salts process be cured after obtain finished product. The patent No. is the production technique that the Chinese patent of ZL201210033741.0 discloses a kind of wool protein compound viscose fiber, and the present invention provides the production technique of a kind of wool protein compound viscose fiber, belongs to field of viscose fiber. , spinning blended by the preparation of wool protein spinning solution, wool protein liquid and rayon spinning liquid, solidify and solidification and postprocessing working procedures, obtain wool protein viscose fiber. The patent No. is the preparation method that the Chinese patent of ZL201210304512.8 discloses a kind of pupa protein fiber element compound short rayon fiber spinning solution, it is dissolved in sodium hydroxide solution by pupa protein powder, add protein denaturation auxiliary agent after filtration and obtain pupa albumen spinning solution, then carry out spinning with viscose glue dope blending; The patent No. is the preparation method that the Chinese patent of ZL201220387021.4 discloses a kind of fibroin blending regeneration cellulose fiber, concrete technique is: (1) by silk offcut through coming unstuck, obtain the silk fibroin powder body that particle diameter is 0.1-0.5 micron after swelling, dry and broken powder, (2) after using sodium hydroxide solution to disperse silk fibroin powder body, add dispersion agent and linking agent fatty acid alkyl alcohol amide, obtain fibroin dispersion mother liquor;(3) this mother liquor and Mierocrystalline cellulose viscose glue blending are obtained Blend rubber, after spinning moulding and aftertreatment, obtain fibroin blending regeneration cellulose fiber.
Application number be 201110400581.4 Chinese patent disclose a kind of regenerated animal micropowder protein cellulose fiber and its preparation method, the present invention discloses a kind of regenerated animal micropowder protein cellulose fiber and its preparation method, preparation comprises the following steps: join in dispersant solution by micro-for nano level animal amyloid proteins, stir evenly, after filtration, obtain the micro-amyloid proteins liquid of animal of 20～35wt%; It is that viscose glue prepared by raw material taking cellulose pulp, in dissolving step, add the obtained sex change viscose glue of denaturing agent, micro-for animal amyloid proteins liquid is accounted in the micro-powder of animal wherein the ratio of finished fiber weight 1～30wt%, join in sex change viscose glue and stir evenly, being prepared into the animal blended viscose glue of micro-powder, introduce precipitation bath spinning moulding after deaeration, filtration, then the drawing-off of organizine bar and post-processing step obtain the micro-amyloid proteins viscose fiber of animal. The Chinese patent that the patent No. is ZL200910153053.6 discloses fibroin blending regeneration cellulose fiber and preparation technology thereof, and technique of the present invention comprises the steps: the preparation of (1) nano-grade silk protein powder; (2) preparation of cellulosic fibre. Compared with prior art, the present invention has following useful effect: instant invention overcomes the problem that silk fibroin powder pulverizes super-refinement difficulty, adopts nanometer broken equipment researched and developed voluntarily, and the silk fibroin powder particle diameter of production reaches 100% within 50～100 nanometers.
Above-mentioned patent mainly utilizes protein that cellulosic fibre is carried out modification, the production technology of these patents comprehensive, its production method mainly contains two kinds: animal or plant albumen is first carried out dissolution process and obtains protein liquid by (1), and then joins and carry out wet-spinning in traditional fibre manufacturing technique; (2) first being undertaken animal or plant albumen being made nanometer or micron protein powder by grinding after pre-treatment or dispersion and fining process, then adopting the mode of blending and modifying to add, to carry out wet-spinning in viscose glue shaping. The mode that protein is dissolved in production method (1) protein liquid can destroy the original cavity structure of protein fibre completely, if not taking by crosslinking Treatment, runs off serious in spinning moulding or last handling process; Aldehyde material will certainly be used to carry out acetalation or use heavy metal to carry out sex change solidification according to crosslinking Treatment, not only have influence on the quality of thiozell, and this kind of poisonous material also can cause serious environmental pollution. Production method (2) adopts interpolation nanometer or micron shape protein powder mode, although avoiding Problems existing in production method (1), but also can there is swollen fiber in viscose glue stoste in protein powder, affect the strainability of Blend rubber, seriously even have influence on powerful index and the feel of fiber.
Application number is that the Chinese patent of CN200610068481.5 discloses and a kind of adopts fiber crops material plant to be the numb material viscose fiber that the method for fiber crops material viscose fiber prepare by raw material and prepared by employing the method, step comprises that production stage is got the raw materials ready, boiling, making beating, bleaching, dipping, yellow, spinning etc., thus obtain fiber crops material viscose fiber. The patent No. is the preparation method that ZL201010265600.2 Chinese patent discloses a kind of jute viscose, comprising: by hemp dissolving pulp after dipping, squeezing and pulverization process, obtaining soda cellulose, the mean polymerisation degree of described hemp dissolving pulp is 400～450;By described soda cellulose after yellow, dissolving and filtration treatment, obtain spinning glue liquid, described spinning glue liquid is carried out spinning, obtains jute viscose. the patent No. is preparation method and the application thereof that the Chinese patent of ZL201310084726.3 discloses a kind of hemp stalk viscose fiber, and the preparation method of described hemp stalk viscose fiber comprises and gets the raw materials ready, dipping squeezing, pulverizing, experienced, yellow, dissolving, filtration, deaeration, spins front filtration, wire drawing and post-treating and other steps. the patent No. is preparation method and the application thereof that the Chinese patent of ZL201310084738.6 discloses a kind of ramie stalk antibacterial viscose fiber, the preparation method of described ramie stalk antibacterial viscose fiber comprises squeezing, pulverizes, soaks, comes unstuck, acid-alkali treatment, boiling, the slurrying dregs of rice, post-treating and other steps. the Chinese patent that the patent No. is ZL200410004397.8 discloses a kind of fiber crops material cellulose viscose pulp and functional fibre preparation method, the present invention relates to the Technology utilizing fiber crops material to produce cellulose viscose pulp and functional fibre, described direction comprises: fiber crops material gets the raw materials ready → blank → screen → wash material → pre-treatment → boiling → extrude → discongest → desanding, concentrated → chlorination → soda finishing → bleaching → acid treatment → desanding, concentrate → manufacture paper with pulp → flood → squeeze → pulverize → experienced → yellow → grinding → dissolving → mixing → pre-filtering → filtration → deaeration → filtration → spinning → drawing-off → cut-out → aftertreatment → drying → packing, obtain with functional viscose fiber. the Chinese patent that the patent No. is ZL200710130606.7 discloses a kind of viscose fiber and its preparation method, the present invention provide a kind of utilize industrial hemp to prepare for raw material viscose fiber and its preparation method, described method comprises: get the raw materials ready, blank, sudden strain of a muscle are quick-fried, prehydrolysis, boiling, selected, chlorination, bleaching, acid treatment, refine, manufacture paper with pulp, rub mill, dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing, filtration, deaeration, filtration, spinning, cut-out, refining, drying, packing with the hands, thus obtain taking industrial hemp as viscose fiber prepared by raw material. application number be 200810037072.8 Chinese patent disclose a kind of method that sisal leaves produces viscose fiber, comprise the following steps: (1) sorting sisal leaves, (2) adopting machinery to knock or roll compacting, the mesophyll colloid of sisal leaves struck off through carding method sub-wire, washing obtains thick sisal leaves cellulosic fibre, (3) fermentative processing in microorganism mould solution, and hydrogen peroxide treatment is de-except residual colloid, (4) soda cellulose is produced, (5) soda cellulose yellow, dissolving spinning slurry processed, (6) spinning slurry deaeration, (7) wet-spinning, obtains viscose fiber. application number be 201510176587.6 Chinese patent disclose the preparation method of a kind of viscose fiber containing Herba Apocyni veneti extract, comprise the following steps: Herba Apocyni veneti extract powder (is joined in the water that temperature is 25 ± 1 DEG C by the preparation of antimicrobial, add-on is 120g/1000ml water, be stirred well to powder dissolve completely make antimicrobial), add dispersion agent, add Xylo-Mucine, blended with spinning solution, spinning, aftertreatment, obtains the viscose fiber containing Herba Apocyni veneti extract. application number be 201510433580.8 Chinese patent disclose a kind of fiber crops preparation method of viscose glue mint fibers and socks, comprise: by hemp dissolving pulp after dipping, squeezing and pulverization process, obtaining soda cellulose, the mean polymerisation degree of described hemp dissolving pulp is 400～450,Described soda cellulose is carried out yellow process, then adds bamboo charcoal mint emulsion, then through dissolving and after filtration treatment, obtain spinning solution, described spinning solution is carried out spinning, obtains jute viscose. the Chinese patent that the patent No. is ZL201110066533.6 discloses a kind of fiber crops material viscose staple fibre and its preparation method, fiber crops material is adopted to be that hemp dissolving pulp made by raw material, the viscose fiber produced with this kind of slurry dregs of rice again, preparation method comprises pre-treatment, washing, boiling, wash material, making beating, desanding, concentrated, soda finishing, bleaching, acid treatment, washing, rear selected desanding, concentrated, manufacture paper with pulp, dipping, squeezing, pulverize, experienced, yellow, grinding, dissolve, filter, deaeration, filter, spinning, drawing-off, cut off, aftertreatment, the steps such as drying and packing, obtain fiber crops material viscose staple fibre.
Above-mentioned patent is the production technology of preparation fiber crops modified cellulose fibre. It may be seen that hemp dissolving pulp is mainly first prepared in the preparation of fiber crops modified cellulose fibre from these technology, then hemp dissolving pulp utilizes viscose preparation technology carry out the preparation of fiber crops viscose glue stoste, then carries out spinning. Fiber crops are first made in the process of hemp dissolving pulp or preparation fiber crops viscose glue stoste, will handle dense alkali, pyroprocess, and the effective ingredient of fiber crops retains very few, seriously affects the performance of fiber.
Namely or just protein-modified or numb modification cellulosic fibre is just carried out single modification by patent noted earlier. Along with the raising that comfort of fabric is required by people, the while of protein and fiber crops, modified cellulose fibre is more and more paid attention to.
Application number be 201410380285.6 Chinese patent disclose a kind of silk flaxen fiber cellulose fiber and its preparation method, concrete technique comprises: the preparation of the preparation of fiber crops slurry rayon spinning stoste, the preparation of protein dispersion and emulsion liquid, the fiber crops protein modified spinning solution of slurry and spinning aftertreatment etc. Wherein the preparation abundant employing adhering process of heat of fiber crops slurry rayon spinning stoste, uses highly basic, and length consuming time, the effective constituent in hemp dissolving pulp is destroyed relatively big, affects performance. Protein is as organic substance simultaneously, it may also be useful to the effect that base extraction and pottery roller, star type ball mill carry out grinding distribution is poor.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art existence, seek to design the preparation method of a kind of Nettle extract protein composite additive, by prepared Nettle extract protein composite additive for the preparation of the cellulosic fibre with silk, fiber crops function, make prepared cellulosic fibre all have the function of silk, fiber crops from functional group of part and structure two aspect, make the number of dropouts minimizing of the active princlple in fiber in spinning process and last handling process.
In order to realize above-mentioned purpose, the technical solution used in the present invention is: the preparation method of a kind of Nettle extract protein composite additive, comprises the following steps:
Step 1: prepare Nettle extract-cyclodextrin powder body
Nettle extract is dissolved at 40～60 DEG C, preparation massfraction is the Nettle extract aqueous solution of 10%-20%, in the Nettle extract aqueous solution, add cyclodextrin carry out whip attachment, the weight ratio of Nettle extract and cyclodextrin is 2～5:1, adsorption time is 20～50min, then this solution is dried, obtain Nettle extract-cyclodextrin powder body;
Preferably, described Nettle extract comes from one or several in ramie, jute, flax, kendir and bluish dogbane, buys by market and obtains.
Step 2: preparation is taking Nettle extract-cyclodextrin as core, and protein is the microcapsule of wall material
Preparation massfraction is the protein water soln of 10.0%～18.0%, Nettle extract-cyclodextrin powder body that step 1 is obtained is joined in protein water soln, wherein the mass ratio of Nettle extract and protein is 1～2:1～2, stir evenly, and adjust ph is 3.5, is then cooled to 2.0 DEG C, add trans-glutaminases and regulate pH to be 8.0, filtering after reaction 2h, being namely able to Nettle extract-cyclodextrin is core, and protein is the microcapsule of wall material;
Preferably, described protein is one or more in gelatin, soybean protein isolate, wool protein or fibroin;
Preferably, described taking Nettle extract-cyclodextrin as core, protein is particle diameter D97≤3.000 μm of the microcapsule of wall material.
Step 3: prepare Nettle extract protein composite additive
To step 2 prepare taking Nettle extract-cyclodextrin as core, protein be wall material microcapsule in add whipping agent, prepare composite additive, the quality of described whipping agent is the 1.0%～4.0% of Nettle extract quality.
Preferably, described whipping agent is the one in carbonate or supercarbonate;
Preferably, described whipping agent is the one in sodium carbonate or sodium bicarbonate.
A preparation method with the cellulosic fibre of silk, fiber crops function, comprises the following steps:
Step a: prepare co-blended spinning stoste
Taking cellulose pulp as raw material, know viscose glue preparation section through public affairs, obtained viscose glue stoste, in viscose glue stoste, the content of alpha cellulose is 7.8%-9.2%; Utilization is spun front injection device and is added described Nettle extract protein composite additive in viscose glue stoste, and in Nettle extract protein composite additive, the quality of Nettle extract and protein is the 4.0%～12.0% of alpha cellulose quality, prepares co-blended spinning stoste;
Step b: spinning and aftertreatment
By the precipitation bath adjusted, described co-blended spinning stoste is carried out spinning, and nascent tow obtains shaping tow after drawing-off; The shaping tow of gained, after cutting off, relax sulfur removal technology, finish application bath, washing and drying, obtains having concurrently the cellulosic fibre of silk, fiber crops function.
Preferably, described precipitation bath is sulfuric acid 80～105g/L, sodium sulfate 260～295g/L.
Preferably, described desulfurization is bathed: Na2SO32.0～8.0g/L, oil bath: 1.0～5.0g/L, does not bleach, bake out temperature: 100～120 DEG C, and drying time is 40～60min.
A cellulosic fibre with silk, fiber crops function, the protein containing 2.0～5.0wt%, the Nettle extract of 2.0～5.0wt%.
The useful effect of the present invention is:
(1) using protein, Nettle extract as functional group of part, cellulosic fibre is made to have silk and fiber crops function concurrently, simultaneously by adding whipping agent, fiber is made to form class hollow structure in moulding process, to reach the effect of imitative fiber crops structure, prepared cellulosic fibre is made all to have the functional character of silk, fiber crops from functional group of part and structure two aspect.
(2) by the crosslinking curing of the adsorption of cyclodextrin, micro encapsulation and wall material protein, make the number of dropouts minimizing in spinning process and last handling process of the active princlple Nettle extract in fiber and protein, prepare the functional character that the functional viscose fiber has silk, fiber crops concurrently.
(3) compared with conventional viscose fiber, its bacteriostasis rate >=85.0% to streptococcus aureus, bacteriostasis rate >=85.0% to intestinal bacteria, inhibiting rate >=80.0% to Candida albicans, containing multiple amino acids trace element in fiber, having good feel and skin-protecting function, product main physical indexes can reach the requirement of GB/T14463-2008 " viscose staple fibre " acceptable end product.
Embodiment
Below by specific embodiment, the invention will be further described:
Embodiment 1
The preparation method of the Nettle extract protein composite additive of the present embodiment, comprises the following steps:
Step 1: preparation ramie extract-cyclodextrin powder body
Ramie extract is dissolved at 40 DEG C, preparation massfraction is the ramie solution of extract of 10%, in ramie solution of extract, add cyclodextrin carry out whip attachment, the weight ratio of ramie extract and cyclodextrin is 2:1, adsorption time is 50min, then this solution is dried, obtain ramie extract-cyclodextrin powder body;
Step 2: preparation is taking ramie extract-cyclodextrin as core, and gelatin protein is the microcapsule of wall material
Preparation massfraction is the gelatin protein aqueous solution of 10.0%, ramie extract-cyclodextrin powder body that step 1 is obtained is joined in the gelatin protein aqueous solution, wherein the mass ratio of ramie extract and gelatin protein is 1:1, stir evenly, and adjust ph is 3.5, is then cooled to 2.0 DEG C, add trans-glutaminases and regulate pH to be 8.0, filtering after reaction 2h, being namely able to ramie extract-cyclodextrin is core, and gelatin protein is the microcapsule of wall material; Taking ramie extract-cyclodextrin as core, gelatin protein is particle diameter D97≤1.027 μm of the microcapsule of wall material.
Step 3: preparation ramie extract gelatin protein composite additive
To step 2 prepare taking ramie extract-cyclodextrin as core, gelatin protein be wall material microcapsule in add whipping agent sodium carbonate, prepare composite additive, the quality of described whipping agent sodium carbonate is the 1.0% of ramie extract quality.
A preparation method with the cellulosic fibre of silk, fiber crops function, comprises the following steps:
Step a: prepare co-blended spinning stoste
Taking cellulose pulp as raw material, know viscose glue preparation section through public affairs, obtained viscose glue stoste, in viscose glue stoste, the content of alpha cellulose is 9.2%; Utilization is spun front injection device and is added described ramie extract gelatin protein composite additive in viscose glue stoste, in ramie extract gelatin protein composite additive, the quality of ramie extract and gelatin protein is the 4.0% of alpha cellulose quality, prepares co-blended spinning stoste;
Step b: spinning and aftertreatment
By the precipitation bath adjusted, described co-blended spinning stoste is carried out spinning, and nascent tow obtains shaping tow after drawing-off; The shaping tow of gained, after cutting off, relax sulfur removal technology, finish application bath, washing and drying, obtains having concurrently the cellulosic fibre of silk, fiber crops function; Precipitation bath is sulfuric acid 80g/L, sodium sulfate 260g/L; Desulfurization is bathed: Na2SO32.0g/L, oil bath: 1.0g/L, does not bleach, bake out temperature: 100 DEG C, and drying time is 60min.
Embodiment 1 obtains the cellulosic fibre having silk, fiber crops function concurrently that specification is 1.11dtex × 38mm, compared with conventional viscose fiber, its bacteriostasis rate 85.0% to streptococcus aureus, the bacteriostasis rate 85.0% to intestinal bacteria, inhibiting rate 80.0% to Candida albicans, containing multiple amino acids trace element in fiber, and there is class hollow structure, feel and skin-protecting function are good.
Embodiment 2
The preparation method of the Nettle extract protein composite additive of the present embodiment, comprises the following steps:
Step 1: preparation jute extract-cyclodextrin powder body
Jute extract is dissolved at 45 DEG C, preparation massfraction is the jute solution of extract of 12%, in jute solution of extract, add cyclodextrin carry out whip attachment, the weight ratio of jute extract and cyclodextrin is 2:1, adsorption time is 42min, then this solution is dried, obtain jute extract-cyclodextrin powder body;
Step 2: preparation is taking jute extract-cyclodextrin as core, and soybean protein isolates is the microcapsule of wall material
Preparation massfraction is the soybean protein isolates aqueous solution of 12.2%, jute extract-cyclodextrin powder body that step 1 is obtained is joined in the soybean protein isolates aqueous solution, wherein the mass ratio of jute extract and soybean protein isolates is 1:2, stir evenly, and adjust ph is 3.5, is then cooled to 2.0 DEG C, add trans-glutaminases and regulate pH to be 8.0, filtering after reaction 2h, being namely able to jute extract-cyclodextrin is core, and soybean protein isolates is the microcapsule of wall material;Taking jute extract-cyclodextrin as core, soybean protein isolates is particle diameter D97≤1.236 μm of the microcapsule of wall material.
Step 3: preparation jute extract soybean protein isolates composite additive
To step 2 prepare taking jute extract-cyclodextrin as core, soybean protein isolates be wall material microcapsule in add whipping agent sodium bicarbonate, prepare composite additive, the quality of described whipping agent sodium bicarbonate is the 1.5% of jute extract quality.
A preparation method with the cellulosic fibre of silk, fiber crops function, comprises the following steps:
Step a: prepare co-blended spinning stoste
Taking cellulose pulp as raw material, know viscose glue preparation section through public affairs, obtained viscose glue stoste, in viscose glue stoste, the content of alpha cellulose is 8.8%; Utilization is spun front injection device and is added described jute extract soybean protein isolates composite additive in viscose glue stoste, in jute extract soybean protein isolates composite additive, the total mass of jute extract and soybean protein isolates is the 5.5% of alpha cellulose quality, prepares co-blended spinning stoste;
Step b: spinning and aftertreatment
By the precipitation bath adjusted, described co-blended spinning stoste is carried out spinning, and nascent tow obtains shaping tow after drawing-off; The shaping tow of gained, after cutting off, relax sulfur removal technology, finish application bath, washing and drying, obtains having concurrently the cellulosic fibre of silk, fiber crops function; Precipitation bath is sulfuric acid 86g/L, sodium sulfate 271g/L; Desulfurization is bathed: Na2SO32.9g/L, oil bath: 1.6g/L, does not bleach, bake out temperature: 105 DEG C, and drying time is 55min.
Embodiment 2 obtains the cellulosic fibre having silk, fiber crops function concurrently that specification is 1.33dtex × 38mm, compared with conventional viscose fiber, its bacteriostasis rate 89.2% to streptococcus aureus, the bacteriostasis rate 90.1% to intestinal bacteria, inhibiting rate 86.5% to Candida albicans, containing multiple amino acids trace element in fiber, and there is class hollow structure, feel and skin-protecting function are good.
Embodiment 3
The preparation method of the Nettle extract wool protein composite additive of the present embodiment, comprises the following steps:
Step 1: preparation jute extract-cyclodextrin powder body
Nettle extract is dissolved at 51 DEG C, preparation massfraction is the Nettle extract aqueous solution of 14.5%, in the Nettle extract aqueous solution, add cyclodextrin carry out whip attachment, the weight ratio of Nettle extract and cyclodextrin is 3:1, adsorption time is 35min, then this solution is dried, obtain Nettle extract-cyclodextrin powder body; Nettle extract is that bluish dogbane extract and flax extract combine by any proportioning;
Step 2: preparation is taking Nettle extract-cyclodextrin as core, and wool protein is the microcapsule of wall material
Preparation massfraction is the wool protein aqueous solution of 13.5%, Nettle extract-cyclodextrin powder body that step 1 is obtained is joined in the wool protein aqueous solution, wherein the mass ratio of Nettle extract and wool protein is 2:1, stir evenly, and adjust ph is 3.5, is then cooled to 2.0 DEG C, add trans-glutaminases and regulate pH to be 8.0, filtering after reaction 2h, being namely able to Nettle extract-cyclodextrin is core, and wool white matter is the microcapsule of wall material; Taking Nettle extract-cyclodextrin as core, wool protein is particle diameter D97≤1.578 μm of the microcapsule of wall material.
Step 3: prepare Nettle extract wool protein composite additive
To step 2 prepare taking Nettle extract-cyclodextrin as core, wool protein be wall material microcapsule in add whipping agent sodium bicarbonate, prepare composite additive, the quality of described whipping agent sodium bicarbonate is the 2.1% of Nettle extract quality.
A preparation method with the cellulosic fibre of silk, fiber crops function, comprises the following steps:
Step a: prepare co-blended spinning stoste
Taking cellulose pulp as raw material, know viscose glue preparation section through public affairs, obtained viscose glue stoste, in viscose glue stoste, the content of alpha cellulose is 8.2%; Utilization is spun front injection device and is added described Nettle extract wool protein composite additive in viscose glue stoste, in Nettle extract wool protein composite additive, the total mass of Nettle extract and wool protein is the 8.2% of alpha cellulose quality, prepares co-blended spinning stoste;
Step b: spinning and aftertreatment
By the precipitation bath adjusted, described co-blended spinning stoste is carried out spinning, and nascent tow obtains shaping tow after drawing-off; The shaping tow of gained, after cutting off, relax sulfur removal technology, finish application bath, washing and drying, obtains having concurrently the cellulosic fibre of silk, fiber crops function; Precipitation bath is sulfuric acid 91g/L, sodium sulfate 278g/L; Desulfurization is bathed: Na2SO34.2g/L, oil bath: 2.7g/L, does not bleach, bake out temperature: 110 DEG C, and drying time is 51min.
Embodiment 3 obtains the cellulosic fibre having silk, fiber crops function concurrently that specification is 1.56dtex × 38mm, compared with conventional viscose fiber, its bacteriostasis rate 93.2% to streptococcus aureus, the bacteriostasis rate 93.8% to intestinal bacteria, inhibiting rate 90.2% to Candida albicans, containing multiple amino acids trace element in fiber, and there is class hollow structure, feel and skin-protecting function are good.
Embodiment 4
The preparation method of the Herba Apocyni veneti extract silk protein composite additive of the present embodiment, comprises the following steps:
Step 1: prepare Herba Apocyni veneti extract-cyclodextrin powder body
Herba Apocyni veneti extract is dissolved at 55 DEG C, preparation massfraction is the Herba Apocyni veneti extract aqueous solution of 18%, in the Herba Apocyni veneti extract aqueous solution, add cyclodextrin carry out whip attachment, the weight ratio of Herba Apocyni veneti extract and cyclodextrin is 4:1, adsorption time is 27min, then this solution is dried, obtain Herba Apocyni veneti extract-cyclodextrin powder body;
Step 2: preparation is taking Herba Apocyni veneti extract-cyclodextrin as core, and silk protein is the microcapsule of wall material
Preparation massfraction is the silk protein aqueous solution of 15.9%, Herba Apocyni veneti extract-cyclodextrin powder body that step 1 is obtained is joined in the silk protein aqueous solution, wherein the mass ratio of Herba Apocyni veneti extract and silk protein is 1:1, stir evenly, and adjust ph is 3.5, is then cooled to 2.0 DEG C, add trans-glutaminases and regulate pH to be 8.0, filtering after reaction 2h, being namely able to Herba Apocyni veneti extract-cyclodextrin is core, and silk protein is the microcapsule of wall material; Taking Herba Apocyni veneti extract-cyclodextrin as core, silk protein is particle diameter D97≤1.925 μm of the microcapsule of wall material.
Step 3: prepare Herba Apocyni veneti extract silk protein composite additive
To step 2 prepare taking Herba Apocyni veneti extract-cyclodextrin as core, silk protein be wall material microcapsule in add whipping agent sodium bicarbonate, prepare composite additive, the quality of described whipping agent sodium bicarbonate is the 2.9% of Herba Apocyni veneti extract quality.
A preparation method with the cellulosic fibre of silk, fiber crops function, comprises the following steps:
Step a: prepare co-blended spinning stoste
Taking cellulose pulp as raw material, know viscose glue preparation section through public affairs, obtained viscose glue stoste, in viscose glue stoste, the content of alpha cellulose is 7.8%;Utilization is spun front injection device and is added described Herba Apocyni veneti extract silk protein composite additive in viscose glue stoste, in Herba Apocyni veneti extract silk protein composite additive, the total mass of Herba Apocyni veneti extract and silk protein is the 10.3% of alpha cellulose quality, prepares co-blended spinning stoste;
Step b: spinning and aftertreatment
By the precipitation bath adjusted, described co-blended spinning stoste is carried out spinning, and nascent tow obtains shaping tow after drawing-off; The shaping tow of gained, after cutting off, relax sulfur removal technology, finish application bath, washing and drying, obtains having concurrently the cellulosic fibre of silk, fiber crops function; Precipitation bath is sulfuric acid 99g/L, sodium sulfate 286g/L; Desulfurization is bathed: Na2SO35.9g/L, oil bath: 4.2g/L, does not bleach, bake out temperature: 116 DEG C, and drying time is 45min.
Embodiment 4 obtains the cellulosic fibre having silk, fiber crops function concurrently that specification is 1.67dtex × 38mm, compared with conventional viscose fiber, its bacteriostasis rate 96.8% to streptococcus aureus, the bacteriostasis rate 97.2% to intestinal bacteria, inhibiting rate 95.3% to Candida albicans, containing multiple amino acids trace element in fiber, and there is class hollow structure, feel and skin-protecting function are good.
Embodiment 5
The preparation method of the bluish dogbane extract protein composite additive of the present embodiment, comprises the following steps:
The preparation method of the bluish dogbane extract silk protein composite additive of the present embodiment, comprises the following steps:
Step 1: preparation bluish dogbane extract-cyclodextrin powder body
Bluish dogbane extract is dissolved at 60 DEG C, preparation massfraction is the bluish dogbane solution of extract of 20%, in bluish dogbane solution of extract, add cyclodextrin carry out whip attachment, the weight ratio of bluish dogbane extract and cyclodextrin is 5:1, adsorption time is 20min, then this solution is dried, obtain bluish dogbane extract-cyclodextrin powder body;
Step 2: preparation is taking bluish dogbane extract-cyclodextrin as core, and silk protein is the microcapsule of wall material
Preparation massfraction is the silk protein aqueous solution of 18%, bluish dogbane extract-cyclodextrin powder body that step 1 is obtained is joined in the silk protein aqueous solution, wherein the mass ratio of bluish dogbane extract and silk protein is 2:1, stir evenly, and adjust ph is 3.5, is then cooled to 2.0 DEG C, add trans-glutaminases and regulate pH to be 8.0, filtering after reaction 2h, being namely able to bluish dogbane extract-cyclodextrin is core, and silk protein is the microcapsule of wall material; Taking bluish dogbane extract-cyclodextrin as core, silk protein is particle diameter D97≤2.328 μm of the microcapsule of wall material.
Step 3: preparation bluish dogbane extract silk protein composite additive
To step 2 prepare taking bluish dogbane extract-cyclodextrin as core, silk protein be wall material microcapsule in add whipping agent sodium bicarbonate, prepare composite additive, the quality of described whipping agent sodium bicarbonate is the 4.0% of bluish dogbane extract quality.
A preparation method with the cellulosic fibre of silk, fiber crops function, comprises the following steps:
Step a: prepare co-blended spinning stoste
Taking cellulose pulp as raw material, know viscose glue preparation section through public affairs, obtained viscose glue stoste, in viscose glue stoste, the content of alpha cellulose is 8.9%; Utilization is spun front injection device and is added described bluish dogbane extract silk protein composite additive in viscose glue stoste, in bluish dogbane extract silk protein composite additive, the total mass of bluish dogbane extract and silk protein is the 12% of alpha cellulose quality, prepares co-blended spinning stoste;
Step b: spinning and aftertreatment
By the precipitation bath adjusted, described co-blended spinning stoste is carried out spinning, and nascent tow obtains shaping tow after drawing-off; The shaping tow of gained, after cutting off, relax sulfur removal technology, finish application bath, washing and drying, obtains having concurrently the cellulosic fibre of silk, fiber crops function; Precipitation bath is sulfuric acid 105g/L, sodium sulfate 295g/L; Desulfurization is bathed: Na2SO38.0g/L, oil bath: 5.0g/L, does not bleach, bake out temperature: 120 DEG C, and drying time is 40min.
Embodiment 4 obtains the cellulosic fibre having silk, fiber crops function concurrently that specification is 2.22dtex × 56mm, compared with conventional viscose fiber, its bacteriostasis rate 99.1% to streptococcus aureus, the bacteriostasis rate 99.0% to intestinal bacteria, inhibiting rate 98.5% to Candida albicans, containing multiple amino acids trace element in fiber, and there is class hollow structure, feel and skin-protecting function are good.
Claims (9)
1. the preparation method of a Nettle extract protein composite additive, it is characterised in that comprise the following steps:
Step 1: prepare Nettle extract-cyclodextrin powder body
Nettle extract is dissolved at 40～60 DEG C, preparation massfraction is the Nettle extract aqueous solution of 10%-20%, in the Nettle extract aqueous solution, add cyclodextrin carry out whip attachment, the weight ratio of Nettle extract and cyclodextrin is 2～5:1, adsorption time is 20～50min, then this solution is dried, obtain Nettle extract-cyclodextrin powder body;
Step 2: preparation is taking Nettle extract-cyclodextrin as core, and protein is the microcapsule of wall material
Preparation massfraction is the protein water soln of 10.0%～18.0%, Nettle extract-cyclodextrin powder body that step 1 is obtained is joined in protein water soln, wherein the mass ratio of Nettle extract and protein is 1～2:1～2, stir evenly, and adjust ph is 3.5, is then cooled to 2.0 DEG C, add trans-glutaminases and regulate pH to be 8.0, filtering after reaction 2h, being namely able to Nettle extract-cyclodextrin is core, and protein is the microcapsule of wall material;
Step 3: prepare Nettle extract protein composite additive
To step 2 prepare taking Nettle extract-cyclodextrin as core, protein be wall material microcapsule in add whipping agent, prepare composite additive, the quality of described whipping agent is the 1.0%～4.0% of Nettle extract quality.
2. the preparation method of Nettle extract protein composite additive according to claim 1, it is characterised in that: described Nettle extract comes from one or several in ramie, jute, flax, kendir and bluish dogbane.
3. the preparation method of Nettle extract protein composite additive according to claim 1, it is characterised in that: described protein is one or more in gelatin, soybean protein isolate, wool protein or fibroin.
4. the preparation method of Nettle extract protein composite additive according to claim 1, it is characterised in that: described taking Nettle extract-cyclodextrin as core, protein is particle diameter D97≤3.000 μm of the microcapsule of wall material.
5. the preparation method of Nettle extract protein composite additive according to claim 1, it is characterised in that: described whipping agent is the one in carbonate or supercarbonate.
6. one kind has the preparation method of the cellulosic fibre of silk, fiber crops function, it is characterised in that, comprise the following steps:
Step a: prepare co-blended spinning stoste
Taking cellulose pulp as raw material, know viscose glue preparation section through public affairs, obtained viscose glue stoste, in viscose glue stoste, the content of alpha cellulose is 7.8%-9.2%;Utilization is spun front injection device and is added Nettle extract protein composite additive as claimed in claim 1 in viscose glue stoste, in Nettle extract protein composite additive, the quality of Nettle extract and protein is the 4.0%～12.0% of alpha cellulose quality, obtained co-blended spinning stoste;
Step b: spinning and aftertreatment
By the precipitation bath adjusted, described co-blended spinning stoste is carried out spinning, and nascent tow obtains shaping tow after drawing-off; The shaping tow of gained, after cutting off, relax sulfur removal technology, finish application bath, washing and drying, obtains having concurrently the cellulosic fibre of silk, fiber crops function.
7. the preparation method of the cellulosic fibre with silk, fiber crops function according to claim 6, it is characterised in that, described precipitation bath is sulfuric acid 80～105g/L, sodium sulfate 260～295g/L.
8. the preparation method of the cellulosic fibre with silk, fiber crops function according to claim 6, it is characterised in that, described desulfurization is bathed: Na2SO32.0～8.0g/L, oil bath: 1.0～5.0g/L, does not bleach, bake out temperature: 100～120 DEG C, and drying time is 40～60min.
9. one kind have as claimed in claim 6 silk, fiber crops function cellulosic fibre preparation method prepared by have silk, fiber crops function cellulosic fibre, it is characterised in that: the protein containing 2.0～5.0wt%, the Nettle extract of 2.0～5.0wt%.
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