CN1217041C - Protein synthetic fiber and its production method - Google Patents
Protein synthetic fiber and its production method Download PDFInfo
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- CN1217041C CN1217041C CN 03111814 CN03111814A CN1217041C CN 1217041 C CN1217041 C CN 1217041C CN 03111814 CN03111814 CN 03111814 CN 03111814 A CN03111814 A CN 03111814A CN 1217041 C CN1217041 C CN 1217041C
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Abstract
The present invention discloses a protein synthetic fiber which is composed of plant protein, animal protein and polyvinyl alcohol, wherein the total quantity of both kinds of the protein accounts for 1% to smaller than 20% or accounts for 20% to 40%, or accounts for larger than 40% to 99% in the fiber quantity, and the rest is polyvinyl alcohol; when the total quantity of both kinds of the protein accounts for 20% to 40% in the fiber quantity, the quantity of one kind of the protein accounts for 1% to 25%, or accounts for 75% to 99% in the total amount of the protein. The present invention also discloses a making method of the fiber. The fiber has good ventilation performance and moisture conducting performance, and has the softness performance and good skin compatible performance of pashm. The preparation of spinning stock solutions in the prepare invention is simple and is easy to implement, which not only can not damage the quality of protein, but also can increase the intersolubility of protein and polyvinyl alcohol, and can enhance the quality of products.
Description
Technical field
The invention belongs to textile material, relating in particular to by phytoprotein and animal protein and polyvinyl alcohol is the synthetic fiber of component, also relates to the manufacture method of this synthetic fiber simultaneously.
Background technology
The known fiber of protein that contains is except that natural silk, Japan once disclosed a kind of information of isolating the synthetic silk of protein production with milk in the publication of celloglobulin chemistry, this product has enlarged the source of producd fibers, in order further to enlarge the production of fiber, and on the basis that guarantees the fiber product superperformance, the inventor once disclosed a kind of manufacture method by plant protein synthetic fiber and this fiber in patent " 99116636.1 ", disclosed a kind of synthetic fiber and the manufacture method thereof different with phytoprotein content in preceding application again in application number is 02109966.9 patent application document, these fibers all have feel as the silk and good performance.
A kind of protein synthetic fibre spinning solution production method is disclosed again in number of patent application is 02101961.4 application documents, in this application, contain phytoprotein and animal protein in the spinning solution, it has increased new raw material for the resource of producd fibers, but only be a kind of spinning solution disclosed in this file, it is the intermediate products of producd fibers, can not become can be for the direct fiber that utilizes of people, though and in this solution, contain two kinds of protein and polyvinyl alcohol, but because two kinds of protein batching narrow range, the natural resources of making fiber are made full use of, the proportioning of phytoprotein and animal protein must be close in this application in addition, and in the process of making spinning solution, be that two kinds of protein and polyvinyl alcohol are dissolved respectively, make solution again, and then they blend, and need add multiple additives, this has increased trouble not only for the work of system liquid, improved cost, and can be because of the residual product quality that impairs of additive wherein, because being used for the solution of solubilising protein in this application mainly is sodium sulfite aqueous solution, therefore this spinning solution is when adopting the spinning technique of vinylon, have partially protein and be lost in the coagulation bath, thereby can't guarantee quality of fiber.
Summary of the invention
Purpose of the present invention just is to provide a kind of synthetic fiber that animal protein and phytoprotein and the multiple proportioning of polyvinyl alcohol are arranged, and the manufacture method of these synthetic fiber is provided simultaneously.
The present invention seeks to be achieved through the following technical solutions: a kind of soylon, form by phytoprotein, animal protein and polyvinyl alcohol, the ratio that the total amount of two kinds of protein accounts for fibre weight is: from 1% to less than 20% or from 20% to 40% or from greater than 40% to 99%, surplus is a polyvinyl alcohol, the ratio that accounts for fibre weight when the total amount of two kinds of protein is for from 20% to 40% the time, and the ratio that wherein a kind of protein accounts for total protein is from 1% to 25% or from 75% to 99%; Described animal protein is at least a in the isolated protein of glue protein, glycoprotein or slender cell space animal.
Described phytoprotein also comprises the isolated protein and the various proteinaceous fruit direct isolated protein that extracts after fragmentation that extract in the maize germ cake after oil expression except that adopting the isolated protein that separation and Extraction goes out from the dregs of rice of soybean or peanut or cottonseed or rapeseed.
Described glue protein is glutin, shellac albumen or gelatine albumen.
The method of making described soylon is:
A, the raw material of animal protein and phytoprotein is immersed in PH respectively is in 7.4～8.4 or 9.5～14 or 0.1～3.5 the aqueous solution, and stir, in temperature is that 28 ℃～29.5 ℃ or 36 ℃～37 ℃ separate after through 40～360 minutes and remove waste residue, transfer the isoelectric point of leachate, must separate protein;
B, isolated protein is dissolved in 1≤PH≤4 or aqueous solution PH 〉=7.3, that contain triethanolamine, perhaps isolated protein is dissolved in the aqueous solution that contains triethanolamine and washing agent, make the protein solution that concentration is As, 4%≤As＜14% or 15%＜As＜22% then, solution temperature is 30 ℃～95 ℃;
C, the polyvinyl alcohol of having washed is directly added in the protein solution, make their blend copolymerization, its temperature should be controlled at 60 ℃～100 ℃, and modulation becomes, and to contain protein and polyvinyl alcohol concentration be 8%～38% spinning solution;
D, add boric acid or borax in the solution that contains protein and polyvinyl alcohol, make spinning solution through stirring, the viscosity of this stoste adopts the test of gravity flow viscosimeter to should be 70～400 seconds;
E, spinning solution after filtration after the deaeration, enter the spinning program again, in this program, adopt the spinning technique of wet spinning technology or dry-jet wet-spinning to make soylon.
Among the described step a, be that animal protein and vegetable protein raw material are immersed in respectively in the alkaline solution, after branch is left away waste residue, transfer the leachate isoelectric point, must separate protein with acid.
Among the described step a, be that animal protein and vegetable protein raw material are immersed in respectively in the acid solution, after branch is left away waste residue, transfer the leachate isoelectric point, must separate protein with alkali.
Among the described step c, the concentration of spinning solution is 20%～38%, adopts dry-jet wet spinning process among the described step e, and spinning solution enters in the coagulation bath and does the wet method drawing-off through the silk of shower nozzle ejection is advanced 5～250mm in air after.
Among the described step b, isolated protein is dissolved in the aqueous solution 1≤PH≤4, that contain triethanolamine, in the spinning program, coagulation bath should be alkalescence.
Among the described step b, isolated protein is dissolved in aqueous solution PH 〉=7.3, that contain triethanolamine, in the spinning program, it is acid that coagulation bath should be.
Among the described step b, isolated protein is dissolved in the aqueous solution that contains triethanolamine and washing agent, in the spinning program, it is acid that coagulation bath should be.
Being used to transfer the acid of leachate isoelectric point is hydrochloric acid, sulfuric acid, boric acid or phosphoric acid.
Being used to transfer the alkali of leachate isoelectric point is NaOH or potassium hydroxide.
The synthetic fiber of making according to the method among the present invention, ventilative lead moist good and have the softness of cashmere and a skin-friendly preferably, and in the present invention, phytoprotein, animal protein and polyvinyl alcohol have adopted multiple different proportioning, and different concentration of dope and different spinning techniques have been adopted, made the fiber of multiple performance, this can adapt to various industries and consumer's needs.The preparation of spinning solution is simple among the present invention, not only can not damage the quality of protein, and increased the intersolubility of protein and polyvinyl alcohol, can improve the quality of product, multiple spinning process also is provided among the present invention, and these are the utilization of resource and the production and the development of synthetic fiber provides good condition.
The specific embodiment
Embodiment 1: it is 9.6 alkaline solution that the soya bean that grinds with wet method through water logging bubble is added pH value, be to dissolve under 29 ℃ the condition in temperature, material-water ratio is 1: 15, dissolution time is 180 minutes, it is 9.6 alkaline solution that gelatin is added pH value, be to dissolve under 28 ℃ the condition in temperature, material-water ratio is for being 1: 40, course of dissolution is 240 minutes, course of dissolution should stir, and then leaves standstill, separates and remove waste residue, gets leachate, in leachate, add hydrochloric acid, transfer the leachate isoelectric point must separate protein; Admittedly to measure weight ratio be that to be dissolved in pH value at 1: 29 be in 12 the aqueous solution that contains triethanolamine by doing the plant separation protein matter that makes and animal isolated protein, the initial temperature of dissolving is 30 ℃ and then is heated to 91 ℃, make temperature rise to 95 ℃ again, and under 95 ℃ temperature conditions, kept 20 minutes, make concentration As and be 4% protein solution; Directly add the polyvinyl alcohol of having washed (PVA) in the protein solution, under 95 ℃ temperature, make its blend copolymerization, then be warming up to 98 ℃ and kept 100 minutes, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 8%, and the weight ratio that solution includes the dried solid amount of phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol is 1: 29: 70, and adding boric acid stirs and makes spinning solution in this solution again.
The spinning solution of making, standing and defoaming under normal pressure enters the spinning way preface through the spinning solution after the deaeration after refiltering, and when the viscosity of spinning solution was measured as if usefulness " gravity flow viscosimeter ", its viscosity should be 80 seconds.Present embodiment adopts wet spinning technology, and the silk that sprays through spray silk machine shower nozzle enters in the coagulation bath, and this coagulation bath is salt and aqueous acid, and its salt adopts sodium sulphate, and acid is sulfuric acid.The contains sodium sulfate amount is 400～420 grams per liters in this body lotion, sulfuric acid amount is 0.22 grams per liter, bath temperature is 30 ℃～36 ℃, in air, carry out air draft through the tow behind the coagulation bath, degree of draft is 2 times, tow after air draft enters and does the wet method drawing-off in the fluid groove, body lotion is the aqueous solution that contains sodium sulphate in the groove, sodium sulphate content is 440 grams per liters in this solution, solution temperature is 90 ℃, the wet degree of draft of tow is 1.5 times in the groove, tow enters dry heat drafting and HEAT SETTING step after the wet method drawing-off, the tow surface temperature is 121 ℃ in a hot case, it is 211 ℃ in the two hot casees, it is 228 ℃ in the three hot casees, it is 240 ℃ in the four hot casees, it is 230 ℃ in the five hot casees, tow carries out dry heat drafting between two hot casees and three hot casees, its traction rate is 2 times, three times total draft reaches 6 times, after dry heat drafting and HEAT SETTING step, promptly become semi-finished product, semi-finished product are finished product through arrangement and acetalation again, should do curling earlier in the arrangement process, cut off, carry out acetalation again, the acetalation temperature in the present embodiment is between 40 ℃～64 ℃, the solution of acetalation adopts glyoxal, the solution of sulfuric acid and ammonium sulfate, its glyoxal content is 5～32 grams per liters, and sulfuric acid content is 150～200 grams per liters, and ammonium sulfate content is 119.9 grams per liters.Tow after acetalation cleans once more, and after becomes the finished product of soylon after oiling, drying and can pack and dispatch from the factory.
Embodiment 2: through fragmentation, it is 7.8 solution that the soya bean of degreasing and milk casein are put into pH value respectively, be to dissolve under 28 ℃ the condition in temperature, dissolution time is 120 minutes, course of dissolution should stir, then leave standstill, separate and remove waste residue, get leachate, add phosphoric acid and transfer isoelectric point in leachate, must separate protein, it is in 1.5 the solution that contains triethanolamine that two kinds of isolated proteins are dissolved in pH value with 5: 21 ratio, the initial temperature of dissolving is 40 ℃, then be heated to 95 ℃, and under 95 ℃ temperature conditions, kept 20 minutes, make concentration As and be 5% protein solution; The polyvinyl alcohol of having washed (PVA) is added in the protein solution, under 95 ℃ temperature, make its blend copolymerization, be warmed up to 98 ℃ and kept 60 minutes, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 10%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 5: 21: 74, adding boric acid stirs and makes spinning solution in this solution again, this stoste enters the spinning way preface after the deaeration after filtration, and the viscosity of spinning solution adopts the gravity flow viscosimeter to be measured as 70 seconds.
Adopt wet spinning technology in the spinning program, the silk of shower nozzle ejection enters in the coagulation bath, and this coagulation bath is an alkalescence, and it is the aqueous solution of salt and alkali, and salt adopts sodium sulphate, and alkali is potassium hydroxide.The pH value of this coagulation bath is 9～12, bath temperature is 36 ℃～38 ℃, tow behind supersolidification solution carries out drawing-off in air, degree of draft is 2.5 times, tow after air draft enters and does the wet method drawing-off in the fluid groove, body lotion is the aqueous solution that contains sodium sulphate in the groove, sodium sulphate content is 400 grams per liters in this solution, solution temperature is 38 ℃～80 ℃, the wet degree of draft of tow is 2 times in the groove, tow enters dry heat drafting and HEAT SETTING program after the wet drawing-off, the tow surface temperature is 141 ℃～180 ℃ in a hot case, in the two hot casees be 231 ℃～250 ℃, in the three hot casees be 251 ℃～260 ℃, in the four hot casees be 251 ℃～260 ℃, in the five hot casees be 241 ℃～250 ℃, tow carries out dry heat drafting between two hot casees and three hot casees, its traction rate is 1.5 times, and three times total draft reaches 7.5 times, the semi-finished product after dry heat drafting and HEAT SETTING step, clean acetalation, acetalation temperature in the present embodiment is 60 ℃, and in the solution of this acetalation, its content of formaldehyde is 30 grams per liters, sulfuric acid content is 230 grams per liters, anhydrous slufuric acid sodium content 135 grams per liters.Tow after acetalation cleans once more, and after oils, dries, curls, finalizes the design and be cut to finished product and can pack and dispatch from the factory.
Embodiment 3: put into pH value through the cottonseed meal of degreasing is 9.5 solution, be to dissolve under 29.5 ℃ the condition in temperature, material-water ratio is 1: 15, and dissolution time is 70 minutes, course of dissolution should stir, then leave standstill, separate and remove waste residue, get leachate, in leachate, add phosphoric acid and transfer isoelectric point, plant separation protein matter, it is that material-water ratio is 1: 15 in 10 the alkaline solution that shellac is added pH value, be to dissolve under 29.5 ℃ the condition in temperature, dissolution time is 100 minutes, and course of dissolution should stir, and then leaves standstill, separate and remove waste residue, get leachate, in leachate, add phosphoric acid, transfer the leachate isoelectric point to get the animal isolated protein; It is in 3 the solution that contains triethanolamine that plant separation protein matter and animal isolated protein are dissolved in pH value in 0.2: 19.8 ratio, the initial temperature of dissolving is 30 ℃, then be heated to 95 ℃, and under 95 ℃ temperature conditions, kept 20 minutes, make concentration As and be 8% protein solution; The polyvinyl alcohol of having washed (PVA) is added in the protein solution, under 94 ℃ temperature, make its blend copolymerization, then be warming up to 100 ℃ and kept 80 minutes, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 15.3%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 0.2: 19.8: 80, adding boric acid stirs and makes spinning solution in this solution again, it is 170 seconds that this spinning solution adopts its viscosity of gravity flow viscosity measurement, spinning solution is 50 ℃ in temperature, under the normal pressure through 3.5 hours standing and defoaming or 40 ℃ of vacuum defoamations, spinning solution after deaeration, enter wet-spinning frame more after filtration and adopt wet spinning, the spray silk enters in the coagulation bath, this coagulation bath is the aqueous solution of salt and alkali, its salt adopts sodium sulphate, and alkali is potassium hydroxide, and bath temperature is 36 ℃～37.9 ℃, pH value is 10.In air, carry out air draft through the tow behind the coagulation bath, degree of draft is 2 times, tow after air draft enters and does the wet method drawing-off in the fluid groove, body lotion is the solution that contains ammonium sulfate in the groove, ammonium sulfate content is 380 grams per liters in this solution, solution temperature is 35 ℃～38 ℃, the wet degree of draft of tow is 2.5 times in the groove, tow enters dry heat drafting and HEAT SETTING step after the wet drawing-off, the tow surface temperature is 181 ℃～200 ℃ in a hot case, be 251 ℃～260 ℃ in the two hot casees, is 261 ℃ in the three hot casees, in the four hot casees be 254 ℃～258 ℃, be 245 ℃ in the five hot casees, tow carries out dry heat drafting between two hot casees and three hot casees, and its traction rate is 1.6 times, three times total draft reaches 8 times, and the step of each behind dry heat drafting is made fiber again.
Embodiment 4: it is 3 the solution that contains triethanolamine that the maize germ cake after oil expression is put into pH value, be to dissolve under 36 ℃ the condition in temperature, dissolution time is 40 minutes, course of dissolution should stir, then leave standstill, separate and remove waste residue, get leachate, in leachate, add NaOH and transfer isoelectric point, get plant separation protein matter.It is 14 solution that shellac is put into pH value, be to dissolve under 36 ℃ the condition in temperature, dissolution time is 50 minutes, course of dissolution should stir, and adds sodium peroxide, then adds triethanolamine, separate and remove waste residue, get leachate, in leachate, add sulfuric acid, transfer the leachate isoelectric point to get the animal isolated protein.Again plant separation protein matter and animal isolated protein being dissolved in pH value in 18: 3 ratio is in 2 the solution that contains triethanolamine, the initial temperature of dissolving is 30 ℃ then makes temperature rise to 95 ℃, and under 95 ℃ temperature conditions, kept 25 minutes, make concentration As and be 12% protein solution; The polyvinyl alcohol of having washed (PVA) is added in the protein solution, under 60 ℃ temperature, make its blend copolymerization, then be warming up to 98 ℃ and kept 90 minutes, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 25%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 18: 3: 79, adding boric acid stirs and makes spinning solution in this solution again, the viscosity of spinning solution should be 280 seconds when adopting the gravity flow viscosimeter to measure, spinning solution discontinuous degassing under the normal pressure in 200 minutes time, or under 35 ℃ temperature, carry out vacuum defoamation, spinning solution after deaeration enters the spinning program more after filtration, in this program, adopt the spinning technique of dry-jet wet-spinning to make fiber, shower nozzle is 5mm apart from the distance of coagulation bath in this spinning technique, silk through the shower nozzle ejection is advanced in air earlier, then enter coagulation bath, body lotion is the aqueous solution of salt and alkali, its salt adopts sodium sulphate, and alkali is NaOH.The contains sodium sulfate amount is 430 grams per liters in this body lotion, amount of sodium hydroxide is 35 grams per liters, spinning solution is done wet drawing-off from the shower nozzle ejection after air enters in the fluid groove in this embodiment, enter again in the hot case and do dry heat drafting, behind dry heat drafting again through HEAT SETTING, cleaning, acetalation, clean once more, oil, dry, curl, step such as typing makes finished product.Tow is identical with embodiment 2 with technological parameter to the procedure of processing that becomes between the finished product from entering behind the fluid groove.
Embodiment 5: it is 11 the solution that contains triethanolamine that the maize germ cake after oil expression and proteinaceous slender cell space animal are put into pH value respectively, its material-water ratio is 1: 16, be to dissolve under 36.5 ℃ the condition in temperature, dissolution time is 120 minutes, and course of dissolution should stir, and then leaves standstill, separate and remove waste residue, get leachate, in leachate, add phosphoric acid and transfer isoelectric point, must separate protein.Again plant separation protein matter and animal isolated protein being dissolved in pH value in 13: 4 ratio is in 3.5 the solution that contains triethanolamine, the initial temperature of dissolving is 45 ℃ then makes temperature rise to 95 ℃, and under 95 ℃ temperature conditions, kept 25 minutes, make concentration As and be 18% protein solution; The polyvinyl alcohol of having washed (PVA) is added in the protein solution, under 70 ℃ temperature, make its blend copolymerization, then be warming up to 95 ℃ and kept 60 minutes, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 28%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 13: 4: 83, adding boric acid stirs and makes spinning solution in this solution again, the viscosity of spinning solution should be 300 seconds when adopting the gravity flow viscosimeter to measure, spinning solution carries out vacuum defoamation under 35 ℃ temperature, or under 80 ℃ of normal pressures discontinuous degassing, spinning solution after deaeration enters the spinning program more after filtration, in this program, adopt the spinning technique of dry-jet wet-spinning to make fiber, shower nozzle is 130mm apart from the distance of coagulation bath in this spinning technique, the spray silk enters coagulation bath behind air, this body lotion is the aqueous solution of salt and alkali.Tow is done wet drawing-off in fluid groove, enter again in the hot case and do dry heat drafting, behind dry heat drafting again through HEAT SETTING, cleaning, acetalation, clean once more, oil, dry, curl, step such as typing makes long filament or staple fibre, wherein tow from enter behind the fluid groove technological parameter in steps identical with embodiment 2.
In embodiment 6, the present embodiment, contain in the spinning solution of animals and plants isolated protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 39.6: 0.4: 60, solution concentration is 20%, and the viscosity of the spinning solution of making is 200 seconds, and other program is identical with embodiment 5 with technological parameter.
Embodiment 7, earlier any proteinaceous fruit fragmentation, and and gelatine to immerse pH value respectively be 3.2, contain in the acid solution of triethanolamine, material-water ratio is 1: 15, solution temperature is 29.5 ℃, after 90 minutes, solution is separated the impurity elimination of removing slag, get leachate, transfer the isoelectric point of protein with NaOH after, must separate protein, again plant separation protein matter and animal isolated protein being dissolved in PH in 35: 35 ratio is 4, temperature is the interior dissolving of 35 ℃ the solution that contains triethanolamine, slowly be warmed up to 90 ℃ again, be warmed up to 95 ℃ again, kept 18 minutes, make concentration As and be 13% the protein solution that contains, when this solution temperature is 60 ℃, in this solution, add polyvinyl alcohol through washing, and stir, then this solution is warmed up to 98 ℃, kept 70 minutes, make and contain, the spinning solution of phytoprotein and polyvinyl alcohol, and this solution is transferred to concentration is 32%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 35: 35: 30, add borax within it, make viscosity and be 259 seconds spinning solution (mensuration of former fluid viscosity adopts " gravity flow viscosimeter ").The spinning solution temperature is added to 110 ℃, adopt the spinning technique of dry-jet wet-spinning to carry out spinning, body lotion adopts alkaline body lotion, and tow is advanced in air, and 200mm is laggard to go into body lotion, and other programs are identical with embodiment 4 in the spinning.
Embodiment 8, rapeseed dregs and hide glue gelatine are immersed pH value respectively is that solution temperature is 37 ℃ in 12.5 the alkaline solution, and material-water ratio is 1: 16, dissolves 190 minutes, separates slagging-off, adds hydrochloric acid and transfer isoelectric point in the leachate of gained, makes isolated protein; It is that temperature is 30 ℃ in 10.5 the solution that contains triethanolamine that plant separation protein matter and animal isolated protein are dissolved in PH in 9: 8 ratio, slowly is warmed up under 95 ℃ the condition, makes concentration and be 15.2% solution.Pure polyvinyl alcohol is added in the above-mentioned protein solution, blend copolymerization under 70 ℃ temperature, then temperature is raised to 100 ℃ again, and kept 60 minutes, make the spinning solution that contains animal and plant protein and polyvinyl alcohol, and this solution is transferred to concentration is 38%, and the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount in the solution is 9: 8: 83, add borax and make spinning solution in solution, former fluid viscosity is 400 seconds; Then adopt the spinning technique of dry-jet wet-spinning to make fiber, in the throwing program, shower nozzle is apart from coagulation bath 230mm, and body lotion adopts acid solution, and tow is identical with embodiment 1 with technological parameter to the procedure of processing that becomes between the finished product from entering behind the fluid groove.
Embodiment 9, the rapeseed dregs of rice after oil expression and the albumen that contains compound sugar, adopt among the embodiment 1 and prepare method of separating protein, make plant separation protein matter and animal isolated protein, so two kinds of isolated proteins being dissolved in temperature jointly is 15 ℃, in the aqueous solution of making by triethanolamine and washing agent, dissolution time is 3～4 hours, they are fully dissolved, make concentration and be 18%～20% the protein solution that contains, the direct polyvinyl alcohol washed of adding in proteinaceous solution then, and make solution temperature slowly rise to 98 ℃ by 60 ℃, rose under 100 ℃ the condition blend copolymerization again 3～4 hours, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 35%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 12: 38: 50, in solution, add borax and stir, make spinning solution, making its viscosity is 380 seconds, and this spinning solution enters the spinning way preface after deaeration is filtered.In this program, adopt the spinning technique of dry-jet wet-spinning to carry out spinning, shower nozzle is 250mm apart from coagulation bath, tow is introduced into the air after the shower nozzle ejection, enter again in salt and the sour coagulation bath of making, through the wet method drawing-off, enter again do in the hot case dry heat drafting again through HEAT SETTING, cleaning, acetalation, clean once more, oil, dry, curl, step such as typing makes long filament or staple fibre.
Embodiment 10, it is 8.4 that soybean meal is immersed in pH value, material-water ratio is 1: 15, temperature is in 28 ℃～28.5 ℃ the alkaline solution, proteinaceous slender cell space animal water is cleaned, then putting into pH value is 3.5, material-water ratio is 1: 20, temperature is in 29 ℃～29.5 ℃ the aqueous solution that contains triethanolamine, extract phytoprotein and animal protein respectively, when they soak dissolving respectively after 180 minutes and 200 minutes in different solution, respectively through slagging-off, get leachate, transfer the isoelectric point of two kinds of protein leachates more respectively, get plant separation protein matter and animal isolated protein, it is 3.1 that two kinds of isolated proteins all are dissolved in PH, temperature is in 18 ℃ the solution that contains triethanolamine, make solution temperature rise to 86 ℃ again, make concentration and be 13.5%～13.9% protein solution, then the polyvinyl alcohol through washing is added in the above-mentioned protein solution, make their blend copolymerization, and stir, make temperature rise to 99 ℃, kept 1 hour, transfer the solution that contains protein and polyvinyl alcohol again, making its concentration is 12%, and solution includes phytoprotein, the ratio of animal protein and polyvinyl alcohol is 3: 7: 90, and program is made fiber by the method described in the embodiment 2 thereafter.
Embodiment 11, it is 8.5 that soybean meal is immersed in pH value, material-water ratio is 1: 14, temperature is in 28 ℃～28.5 ℃ the alkaline solution, it is 0.1 that gelatine is put into pH value, material-water ratio is 1: 19, temperature is in 28 ℃ the aqueous solution, extract phytoprotein and animal protein respectively, when they soak dissolving respectively after 130 minutes and 45 minutes in different solution, respectively through slagging-off, get leachate, transfer the isoelectric point of two kinds of protein leachates more respectively, get plant separation protein matter and animal isolated protein, it is 7.4 that two kinds of isolated proteins are dissolved in PH, temperature is in 20 ℃ the triethanolamine solution, make solution temperature rise to 88 ℃ again, make concentration and be 13.9% protein solution, then the polyvinyl alcohol through washing is added in the above-mentioned protein solution, make their blend copolymerization, and stir, make temperature rise to 95 ℃, transfer the spinning solution that contains protein and polyvinyl alcohol again, making its concentration is 21.9%, and solution includes phytoprotein, the ratio of animal protein and polyvinyl alcohol is 6: 6: 88, and program is made fiber by the method described in the embodiment 8 thereafter.
Embodiment 12, preparing method of separating protein among peanut meal and the gelatin employing embodiment 1, make plant separation protein matter and animal isolated protein, so two kinds of isolated proteins being dissolved in temperature jointly is 25 ℃, pH value 9.8, in the aqueous solution of making by triethanolamine and washing agent, temperature slowly rises to 93 ℃, dissolution time is 3 hours, they are fully dissolved, make concentration and be 18% the protein solution that contains, the direct polyvinyl alcohol washed of adding in proteinaceous solution then, and make solution temperature slowly rise to 98 ℃ by 60 ℃, rose under 100 ℃ the condition blend copolymerization again 3 hours, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 23%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 94: 5: 1, in solution, add borax and stir, make spinning solution, making its viscosity is 100 seconds, and this spinning solution uses the technology identical with embodiment 1 to make long filament or staple fibre.
Embodiment 13, preparing method of separating protein among peanut meal and the gelatin employing embodiment 1, make plant separation protein matter and animal isolated protein, so two kinds of isolated proteins being dissolved in temperature jointly is 28 ℃, pH value 10.1, in the aqueous solution of making by triethanolamine and washing agent, dissolution time is 3 hours, they are fully dissolved, make concentration and be 17% the protein solution that contains, the direct polyvinyl alcohol washed of adding in proteinaceous solution then, and make solution temperature slowly rise to 98 ℃ by 60 ℃, rose under 100 ℃ the condition blend copolymerization again 3 hours, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 17%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 0.5: 0.5: 99, in solution, add borax and stir, make spinning solution, making its viscosity is 210 seconds, and this spinning solution uses the technology identical with embodiment 1 to make long filament or staple fibre.
Embodiment 14, preparing method of separating protein among peanut meal and the gelatin employing embodiment 1, make plant separation protein matter and animal isolated protein, so two kinds of isolated proteins being dissolved in temperature jointly is 25 ℃, pH value 7.3, in the aqueous solution of making by triethanolamine and washing agent, dissolution time is 3 hours, slowly be warming up to 81 ℃, they are fully dissolved, make concentration and be 18% the protein solution that contains, the direct polyvinyl alcohol washed of adding in proteinaceous solution then, and make solution temperature slowly rise to 98 ℃ by 60 ℃, rose under 100 ℃ the condition blend copolymerization again 3 hours, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 23%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 94: 5: 1, in solution, add borax and stir, make spinning solution, making its viscosity is 100 seconds, uses the technology identical with embodiment 1 that this spinning solution is made long filament or staple fibre at last.
Embodiment 15, preparing method of separating protein among cottonseed meal and the shellac employing embodiment 1, make plant separation protein matter and animal isolated protein, so two kinds of isolated proteins being dissolved in temperature jointly is 55 ℃, pH value 7.9, in the aqueous solution of making by triethanolamine and washing agent, slowly be warming up to 83 ℃, dissolution time is 90 minutes, make concentration and be 21% the protein solution that contains, the direct polyvinyl alcohol washed of adding in proteinaceous solution then, and make solution temperature slowly rise to 98 ℃ by 60 ℃, rose under 100 ℃ the condition blend copolymerization again 3 hours, make the spinning solution that contains plant animal protein and polyvinyl alcohol, and this solution is transferred to concentration is 30%, and solution includes phytoprotein, the weight ratio that three kinds of compositions of animal protein and polyvinyl alcohol are done solid amount is 50: 25: 25, in solution, add borax and stir, make spinning solution, making its viscosity is 372 seconds, uses the technology identical with embodiment 1 that this spinning solution is made long filament or staple fibre at last.
In embodiment 16, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 2: 96: 2, solution concentration is 27%, and the viscosity of the spinning solution of making is 315 seconds, and other program is identical with embodiment 5 with technological parameter.
In embodiment 17, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 25: 30: 45, solution concentration is 26%, and the viscosity of the spinning solution of making is 200 seconds, and other program is identical with embodiment 5 with technological parameter.
In embodiment 18, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 4.9: 15.1: 80, solution concentration is 29%, and the viscosity of the spinning solution of making is 308 seconds, and other program is identical with embodiment 1 with technological parameter.
In embodiment 19, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 30.1: 9.9: 60, solution concentration is 31%, and the viscosity of the spinning solution of making is 316 seconds, and other program is identical with embodiment 1 with technological parameter.
In embodiment 20, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 7: 23: 70, solution concentration is 27%, and the viscosity of the spinning solution of making is 296 seconds, and other program is identical with embodiment 5 with technological parameter.
In embodiment 21, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 35: 40: 25, solution concentration is 26%, and the viscosity of the spinning solution of making is 266 seconds, and other program is identical with embodiment 5 with technological parameter.
In embodiment 22, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 49: 50: 1, solution concentration is 29%, and the viscosity of the spinning solution of making is 93 seconds, other program and technological parameter and
Embodiment 2 is identical.
In embodiment 23, the present embodiment, contain in the spinning solution of plant animal protein and polyvinyl alcohol, the weight ratio that phytoprotein, animal protein and three kinds of compositions of polyvinyl alcohol are done solid amount is 80: 10: 10, solution concentration is 31%, and the viscosity of the spinning solution of making is 104 seconds, and other program is identical with embodiment 2 with technological parameter.
In various embodiments of the present invention, the content of triethanolamine should account for 0.01%～1% of spinning solution weight in the spinning solution, doing with washing agent and triethanolamine among the embodiment of isolated protein, the content of washing agent is that every kilogram of spinning solution contains 1～10 gram washing agent in the spinning solution of making.
In the present invention, prepared spinning solution can be that disclosed spinning program and technological parameter are made fiber in 02109966.9 the patent application according to ZL99116636.1 or application number also.
Claims (12)
1, a kind of soylon, form by phytoprotein, animal protein and polyvinyl alcohol, it is characterized in that: the ratio that the total amount of two kinds of protein accounts for fibre weight is: from 1% to less than 20% or from 20% to 40% or from greater than 40% to 99%, surplus is a polyvinyl alcohol, the ratio that accounts for fibre weight when the total amount of two kinds of protein is for from 20% to 40% the time, and the ratio that wherein a kind of protein accounts for total protein is from 1% to 25% or from 75% to 99%; Described animal protein is at least a in the isolated protein of glue protein, glycoprotein or slender cell space animal.
2, soylon according to claim 1, it is characterized in that: described phytoprotein also comprises the isolated protein and the various proteinaceous fruit direct isolated protein that extracts after fragmentation that extract in the maize germ cake after oil expression except that adopting the isolated protein that separation and Extraction goes out from the dregs of rice of soybean or peanut or cottonseed or rapeseed.
3, soylon according to claim 1 is characterized in that: described glue protein is glutin, shellac albumen or gelatine albumen.
4, make the method for soylon as claimed in claim 1, it is characterized in that:
A, the raw material of animal protein and phytoprotein is immersed in PH respectively is in 7.4～8.4 or 9.5～14 or 0.1～3.5 the aqueous solution, and stir, in temperature is that 28 ℃～29.5 ℃ or 36 ℃～37 ℃ separate after through 40～360 minutes and remove waste residue, transfer the isoelectric point of leachate, must separate protein;
B, isolated protein is dissolved in 1≤PH≤4 or aqueous solution PH 〉=7.3, that contain triethanolamine, perhaps isolated protein is dissolved in the aqueous solution that contains triethanolamine and washing agent, make the protein solution that concentration is As, 4%≤As＜14% or 15%＜As＜22% then, solution temperature is 30 ℃～95 ℃;
C, the polyvinyl alcohol of having washed is directly added in the protein solution, make their blend copolymerization, its temperature should be controlled at 60 ℃～100 ℃, and modulation becomes, and to contain protein and polyvinyl alcohol concentration be 8%～38% spinning solution;
D, add boric acid or borax in the solution that contains protein and polyvinyl alcohol, make spinning solution through stirring, the viscosity of this stoste adopts the test of gravity flow viscosimeter to should be 70～400 seconds;
E, spinning solution after filtration after the deaeration, enter the spinning program again, in this program, adopt the spinning technique of wet spinning technology or dry-jet wet-spinning to make soylon.
5, manufacture method according to claim 4 is characterized in that: among the described step a, be that animal protein and vegetable protein raw material are immersed in respectively in the alkaline solution, after branch is left away waste residue, transfer the leachate isoelectric point with acid, must separate protein.
6, manufacture method according to claim 4 is characterized in that: among the described step a, be that animal protein and vegetable protein raw material are immersed in respectively in the acid solution, after branch is left away waste residue, transfer the leachate isoelectric point with alkali, must separate protein.
7, manufacture method according to claim 4, it is characterized in that: among the described step c, the concentration of spinning solution is 20%～38%, adopt dry-jet wet spinning process among the described step e, spinning solution enters in the coagulation bath and does the wet method drawing-off through the silk of shower nozzle ejection is advanced 5～250mm in air after.
8, according to claim 4 or 5 or 6 described manufacture methods, it is characterized in that: in the described b step, isolated protein is dissolved in the aqueous solution 1≤PH≤4, that contain triethanolamine, in the spinning program, coagulation bath should be alkalescence.
9, according to claim 4 or 5 or 6 described manufacture methods, it is characterized in that: in the described b step, isolated protein is dissolved in aqueous solution PH 〉=7.3, that contain triethanolamine, in the spinning program, it is acid that coagulation bath should be.
10, according to claim 4 or 5 or 6 described methods, it is characterized in that: in the described b step, isolated protein is dissolved in the aqueous solution that contains triethanolamine and washing agent, in the spinning program, it is acid that coagulation bath should be.
11, manufacture method according to claim 5 is characterized in that: being used to transfer the acid of leachate isoelectric point is hydrochloric acid, sulfuric acid, boric acid or phosphoric acid.
12, manufacture method according to claim 6 is characterized in that: being used to transfer the alkali of leachate isoelectric point is NaOH or potassium hydroxide.
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| CN 03111814 CN1217041C (en) | 2003-01-09 | 2003-01-09 | Protein synthetic fiber and its production method |
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| CN1814869B (en) * | 2005-02-05 | 2010-04-28 | 李官奇 | Protein fiber spinning dope capable of absorbing wave, shielding and absorbing heat, and its preparing method |
| CN100424242C (en) * | 2006-04-28 | 2008-10-08 | 韩晓根 | Zein fiber and its preparing process |
| CN100424239C (en) * | 2006-04-28 | 2008-10-08 | 韩晓根 | Maize protein colored textile fiber and method for producing same |
| CN102174720B (en) * | 2011-03-25 | 2014-02-12 | 上海全宇生物科技遂平有限公司 | Compound protein fiber and preparation method thereof |
| CN103388194A (en) * | 2012-05-10 | 2013-11-13 | 郭洁清 | Protein regeneration composite fiber spinning solution and production method thereof |
| CN107151831A (en) * | 2017-06-20 | 2017-09-12 | 海安县中山合成纤维有限公司 | A kind of PVA, collagen and duck's down fiber composite fibers material |
| CN108754640A (en) * | 2018-06-07 | 2018-11-06 | 江苏广盛源科技发展有限公司 | A kind of automatic intelligent special fibre spinning-drawing machine |
| CN108914234A (en) * | 2018-06-07 | 2018-11-30 | 江苏广盛源科技发展有限公司 | A kind of equipment for producing special fibre |
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