CN1074474C - Synthetic plant protein filaments - Google Patents
Synthetic plant protein filaments Download PDFInfo
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- CN1074474C CN1074474C CN99116636A CN99116636A CN1074474C CN 1074474 C CN1074474 C CN 1074474C CN 99116636 A CN99116636 A CN 99116636A CN 99116636 A CN99116636 A CN 99116636A CN 1074474 C CN1074474 C CN 1074474C
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Abstract
The present invention relates to synthetic plant protein filaments which are composed of plant proteins and polyvinyl alcohol heavy polymers respectively having the contents of 23 to 55 portions and 77 to 45 portions. The solutions of the plant proteins and the polyvinyl alcohol heavy polymers are mixed to prepare original spinning liquid, and spun filament bundles can become finished products through a series of procedures, such as wet bath elongation, baking, dry heat elongation, heat setting, etc. by deaeration and wet spinning. The physical property of the synthetic filaments is similar to that of silk, and has the advantages of favorable moisture absorption and ventilation property. The present invention develops a new direction for the further processing of agronomic crops, and has high social benefit and economic benefit.
Description
The invention belongs to textile material, relate in particular to and include the synthetic silk of phytoprotein, relate to the manufacture method of this synthetic silk simultaneously for component wherein.
The known fiber that contains protein is animal protein, and as natural silk, it is copied by silk cocoon and makes, and the obtaining of this silk will be paid a lot of work and the time of extremely growing and be yielded poorly.And Japan once disclosed in the fibre chemistry magazine and a kind ofly isolates protein and acrylonitrile with milk and mix jointly and make the milk protein silk, this synthetic silk shortens a time if pay can play in suitability for industrialized production, increase the effect of output, but because its adopts is animal protein, so product cost is high.
The purpose of this invention is to provide that a kind of cost is low, the synthetic silk that contains phytoprotein of hygroscopicity, good permeability, the manufacture method of this synthetic silk is provided simultaneously.
The technical scheme that achieves the above object is:
This synthetic plant protein filaments, its component are phytoprotein and high-molecular polyvinyl alcohol polymer, and phytoprotein accounts for 23～55 parts of gross weight, and the high-molecular polyvinyl alcohol polymer accounts for 77～45 parts of gross weight.
Described phytoprotein is the protein that separation and Extraction goes out from the dregs of rice of soybean or peanut or cottonseed or rapeseed.
The manufacture method of this synthetic plant protein filaments comprises cooling, acetalation after the program that is processed in the semi-finished product and the semi-finished product, washes, oils, dries, curls, typing and cut-out program, and it is processed into half-finished program and is followed successively by: the pure isolated protein of extraction from the dregs of rice that contain natural plant protein matter plant; Isolated protein after purifying is dissolved into solution again, and to be concentrated to concentration be 15～20%; The high-molecular polyvinyl alcohol polymer dissolution, become concentration and be 15～20% the aqueous solution; Be concentration that the high-molecular polyvinyl alcohol polymer solution of 15～20% isolated protein solution and 15～20% mixes and stirs by proportioning and makes spinning solution; Spinning solution is carried out entering wet-spinning frame employing wet spinning after the deaeration; Enter coagulation bath by the silk that comes out in the spinning spray cap, through wet drawing-off, oven dry, dry heat drafting and the HEAT SETTING program of bathing.
Isolated protein after purifying is dissolved into solution again, and should adopt pH value is 8.5～12.5 alkaline solution, dissolution time 3～8 hours, and 40 ℃～100 ℃ of solution temperatures, the solution after the dissolving should be concentrated into the solution of 15～20% concentration; The solution temperature of high-molecular polyvinyl alcohol polymer is 98 ℃～130 ℃, dissolution time 2～4 hours, and solution concentration transfers to 15%～20%; By mixed protein solution of proportioning and high-molecular polyvinyl alcohol polymer solution, should under 95 ℃～100 ℃ temperature, stir 1 hour, making viscosity is 34～180 millimeters
2The spinning solution of/second; Spinning solution is 80 ℃～95 ℃ in temperature, leaves standstill to carry out deaeration in 4～10 hours under normal pressure; During at wet spinning, spray silk speed is 8～17 meters/minute through the spinning solution after the deaeration, and the coagulation bath that enters is salt and aqueous acid, and its salt content is 420～438 grams per liters, and acid content is 0.26～0.5 grams per liter, and bath temperature is 38 ℃～43 ℃; Tow is 4～9 times at wet total draft multiple of bathing in drawing-off and the dry heat drafting; In the acetalation program in later stage: the hydroformylation liquid temp is 65 ℃～70 ℃, and acetalation solution is the solution that contains aldehyde, acid and anhydrous sodium sulfate; Aldehydes content is 32～80 grams per liters, and acid content is 240～300 grams per liters; The content of anhydrous sodium sulfate is 120～200 grams per liters.
Initial temperature was 40 ℃～45 ℃ when the isolated protein after purifying was dissolved into solution again, pH value is 8.5～9, and temperature is risen 8 ℃～12 ℃, and pH value is every 1～1.5 value of rising in 2 hours, dissolution time is 6～8 hours, and the protein solution of dissolving adopts negative pressure to concentrate again.
In vegetable protein that is adopted in the technical solution of the present invention and the used ratio of high-molecular polyvinyl alcohol polymer, and the synthetic silk that goes out by the fabrication process among the present invention, its performance is close with the silk physical property.Therefore has the advantage of hygroscopicity and good permeability, because this kind protein is a kind of vegetable protein, and extracts from dregs of rice material, so product cost is reduced greatly, it is again to adopt suitability for industrialized production, copies the throwing method of silk with sericulture and compares a time to shorten greatly.Therefore the raw material of product is the dregs of rice material that contains vegetable protein based on soybean, peanut etc. in addition, has changed the idea that vegetable protein is in the past cooked food only, and the present invention has opened up new direction to the deep processing of crops, so it has great social benefit.
Be described further below in conjunction with accompanying drawing and embodiment.
Fig. 1 is a process chart.
Embodiment 1: getting dregs of beans, to add pH value be 9～10 sodium hydrate aqueous solution, and dregs of rice material is 1: 15 with the ratio of above-mentioned solution, is to soak 4 hours in 30 ℃～35 ℃ in temperature, with centrifugal separator dregs of rice slag is separated with leaching liquor then; Hydrogen chloride is added in the leaching liquor, transfer isoelectric points of proteins to make the isolated protein precipitation, the isolated protein that is settled out is added entry wash, shift out upper clear supernate, washing once more, three times repeatedly, sediment is sent into the seperator dehydration again separate, make the true protein collection store stand-by.
It is that 9 sodium hydroxide solution makes its dissolving that the true protein that makes is added pH value again, concentration reaches 5%～7%, the dissolving initial temperature is 40 ℃, behind the dissolution time to 1 hour, its temperature is risen 10 ℃, and the like rose 10 ℃ every 1 hour, course of dissolution will be adjusted the pH value of solution, the pH value that every two hours rises, whole dissolution time be with 6 hours, then protein solution is played cooling in another container, leave standstill after with the concentration of solution concentration to 16%～19%.
(PVA) adds entry with the high-molecular polyvinyl alcohol polymer, makes its dissolving under 110 ℃ temperature, dissolution time 3 hours, and transferring to concentration after the dissolving is 18%～20%.
Above-mentioned two kinds of solution are mixed in proportion, and its additional proportion is: protein solution is 40 weight portions, and PVA is 60 weight portions, stirs 1 hour under 100 ℃ of temperature, and making range of viscosities is 80～120 millimeters
2The spinning solution of/second, be that normal pressure carried out deaeration in static 7 hours under 80 ℃～85 ℃ the temperature in temperature then: through the weaving stoste after the deaeration after refiltering, enter wet-spinning frame, the weaving of employing wet method, the speed of nozzle spray silk is 10 meters/minute, it is sodium sulphate that the spray silk enters the interior coagulation bath of coagulating tank, the solution of sulfuric acid and water, the contains sodium sulfate amount is 429 grams per liters in this body lotion, sulfuric acid is 0.35 grams per liter, bath temperature is 40 ℃, through the drawing-off of in air, wetting of the tow behind the supersolidification, degree of draft is 2.2 times, tow after wet leading enters again does wet drawing-off in the fluid groove, body lotion is for containing aqueous sodium persulfate solution in the groove, sodium sulphate content is 400 grams per liters in this solution, solution temperature is 88 ℃, the wet degree of draft of tow is 1.7 times in the groove, to enter heating, drying program tow surface temperature be 100 ℃ in a hot case to tow after the wet drawing-off, it is 195 ℃ in the two hot casees, it is 225 ℃ in the three hot casees, it is 227 ℃ in the four hot casees, it is 220 ℃ in the five hot casees, tow carries out dry heat drafting between three hot casees and four hot casees, its traction rate is 1.6 times, and three times total draft reaches 5.5 times, and the procedure of tow is identical with the procedure of other fibers behind dry heat drafting, clean acetalation, but acetalation temperature in the present embodiment should be 65 ℃～67 ℃, and in the solution of this acetalation, its content of formaldehyde is 32～50 grams per liters, sulfuric acid content is 240～260 grams per liters, and the anhydrous slufuric acid sodium content is 150～180 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 2: when producing phytoprotein, select for use peanut meal to do raw material, add the alkaline solution pH value in the dregs of rice material and be 10～11.5 potassium hydroxide aqueous solution, temperature is 50 ℃～60 ℃, soaked 2.5 hours, and should add soft water when the isolated protein that precipitates is cleaned.
The true protein of making is dissolved once more, its concentration is 7%～10%, add pH value during dissolving and be 10 the potassium hydroxide alkalescence aqueous solution, the concentration of ordinary dissolution of true protein is 8%～10%, and the initial temperature of dissolving is 50 ℃, rose 6 ℃ every 0.5 hour, the pH value of solution is every 0.3 pH value of rising in 0.5 hour, and dissolution time is 4 hours, takes out solution, solution is concentrated under the situation of negative pressure, and its simmer down to concentration reaches 17%～19%.
By 25 and 75 weight portion proportioning, making viscosity is 125～180 millimeters the protein solution after concentrating and PVA solution
2The spinning solution of/second, this stoste under 85 ℃～90 ℃ normal pressures static 4～6 hours, wet spinning is then adopted in deaeration, and spray silk speed is 16 meters/minute, enter first bath, coagulation bath is the solution of sodium chloride, hydrochloric acid and water in the groove, and sodium chloride content is 430 grams per liters in the body lotion, and content of hydrochloric acid is 0.26 grams per liter, bath temperature is 38 ℃, and temperature is 92 ℃ in second bath.
It is 130 ℃ in a hot case that tow enters heating, drying program tow surface temperature, is 220 ℃ in the two hot casees, is 227 ℃ in the three hot casees, is 235 ℃ in the four hot casees, is 220 ℃ in the five hot casees, carries out dry heat drafting between two hot casees and three hot casees.
Tow total draft multiple is 8.5 times, divides three drawing-offs.
In the acetalation program, adopt benzaldehyde, the mixed liquor of hydrochloric acid and anhydrous sodium sulfate, its benzaldehyde content is 70 grams per liters, and hydrochloric acid is 250～260 grams per liters, and anhydrous sodium sulfate is 180～200 grams per liters.
Other technological parameters are identical with embodiment 1 with procedure.
Embodiment 3: when producing phytoprotein, select for use cottonseed meal to do raw material, in the dregs of rice material to add alkaline solution be that pH value is 8～9.5 sodium hydrate aqueous solution, in temperature be to soak 4 hours under 35 ℃～55 ℃ the temperature.
When the true protein of making was dissolved once more, concentration of ordinary dissolution was 10%～12%, and solution is concentrated into concentration under the situation of negative pressure be 18%～20%.
Protein solution and PVA solution are pressed 23 and 77 weight portion proportioning after concentrating, making viscosity is the spinning solution of 34～85 milli m2/Ss, this stoste leaves standstill deaeration in 6～8 hours under 90 ℃～95 ℃ normal pressure, then adopt wet spinning, and spray silk speed is 17 meters/minute; Coagulation bath is the solution of sodium chloride and sulfuric acid in the bath that enters for the first time, and sodium chloride content is 438 grams per liters in the coagulation bath, and sulfuric acid is 0.5 grams per liter, and bath temperature is 43 ℃, enters in the bath for the second time, and bath temperature is 90 ℃.
Tow total draft multiple is 6 times.
Tow surface temperature temperature in a hot case is 120 ℃, and two hot casees are 210 ℃, and three hot casees are 226 ℃, four hot casees are 230 ℃, and five hot casees are 220 ℃, dry heat drafting once between two hot casees and three hot casees, its drafting multiple is 2 times, and the wet each drawing-off of drawing-off is 2 times.
In the acetalation program in later stage, acetalation liquid is the solution that contains glutaraldehyde, sulfuric acid and anhydrous sodium sulfate, their content is respectively 70～grams per liter, 280～300 grams per liters and 160～180 grams per liters in the solution, and other technological parameters are identical with embodiment 1 with procedure.
Embodiment 4: select the rapeseed dregs of rice for use when producing phytoprotein, produce pure isolated protein with conventional method.
Initial temperature was 40 ℃ when true protein was dissolved once more, and the pH value of solution is 8.5, rose 7.5 ℃ every 1 hour temperature, and the pH value of solution is every 1 value of rising in 2 hours, and dissolution time is 8 hours; Solution concentration is 7%～8%, is concentrated into 15%～17%.
Protein solution after concentrating and PVA solution are with 55 and 45 weight portion proportionings, and making viscosity is 120～160 millimeters
2The spinning solution of/second; This stoste is to leave standstill deaeration in 8～10 hours under 80 ℃～85 ℃ normal pressures in temperature, then adopts wet spinning, and spray silk speed is 8 meters/minute; Enter first bath, coagulation bath is the solution of sulfur-bearing acid amide and sulfuric acid in the groove, and the sulfur-bearing acid amide is 425 grams per liters in the coagulation bath, and the content of sulfuric acid is 0.4 grams per liter, and bath temperature is 42 ℃, then enters second bath, and bath temperature is 89 ℃.
Three drawing-off general times of tow are 9 times, 3 times of each drawing-offs.
In the acetalation program, acetalation liquid is benzaldehyde, and the solution of sulfuric acid and anhydrous sodium sulfate, its content are respectively 35～49 grams per liters, 260～270 grams per liters, 120～150 grams per liters.
Other processes, technical parameter and adding raw material are with embodiment 2.
Embodiment 5: with conventional method respectively from the dregs of rice of soybean, peanut, cottonseed, rapeseed separation and Extraction go out protein.
Above four kinds of protein are mixed, by among the embodiment 1 again dissolving method dissolve once more.
Protein and PVA are with 31 and 69 weight portion proportionings, and spray silk speed is 14 meters/minute.
Coagulation bath is the solution of contains sodium sulfate, sodium chloride and sulfuric acid amine and sulfuric acid, and wherein the summation of three kinds of salt contents is 460 grams per liters, and sulfuric acid content is 0.48 grams per liter.
Tow total draft multiple is 4 times, wherein does 1 times of drawing-off, 1.5 times of other twice each drawing-offs, and other processes, technical parameter number and adding raw material etc. are all identical with embodiment 4.
In the present invention, do raw material after the phytoprotein that also can adopt any two or three dregs of rice material to propose mixes and produce synthetic silk, these are all at the row of protection.
Claims (9)
1. synthetic plant protein filaments, it is characterized in that: its component is phytoprotein and high-molecular polyvinyl alcohol polymer, and phytoprotein accounts for 23～55 parts of gross weight, and the high-molecular polyvinyl alcohol polymer accounts for 77～45 parts of gross weight.
2. synthetic plant protein filaments according to claim 1 is characterized in that: described phytoprotein is the protein that separation and Extraction goes out from the dregs of rice of soybean or peanut or cottonseed or rapeseed.
The manufacture method of claim 1 or 2 described synthetic plant protein filaments comprise cooling, acetalation after the program that is processed in the semi-finished product and the semi-finished product, wash, oil, dry, curl, typing and cut-out program, it is characterized in that: be processed into half-finished program and be followed successively by:
A, from the dregs of rice that contain natural plant protein matter plant, extract pure isolated protein:
B, the isolated protein after purifying is dissolved into solution again, and to be concentrated to concentration be 15～20%;
C, the high-molecular polyvinyl alcohol polymer dissolution, become concentration and be 15～20% the aqueous solution;
D, be concentration that the high-molecular polyvinyl alcohol polymer solution of 15～20% isolated protein solution and 15～20% mixes and stirs by proportioning and makes spinning solution;
E, spinning solution carried out entering after the deaeration wet-spinning frame adopt wet spinning:
F, enter coagulation bath by the silk that comes out in the spinning spray cap, through wet drawing-off, oven dry, dry heat drafting and the HEAT SETTING program of bathing.
4. manufacture method according to claim 3 is characterized in that:
A, the isolated protein after purifying is dissolved into solution again, should adopt pH value is 8.5～12.5 alkaline solution, dissolution time 3～8 hours, and 40 ℃～100 ℃ of solution temperatures, the solution after the dissolving should be concentrated into the solution of 15～20% concentration;
The solution temperature of b, high-molecular polyvinyl alcohol polymer is 98 ℃～130 ℃, dissolution time 24 hours, and solution concentration transfers to 15%～20%;
C, by mixed protein solution of proportioning and high-molecular polyvinyl alcohol polymer solution, should under 95 ℃～100 ℃ temperature, stir 1 hour, making viscosity is 34～180 millimeters
2The spinning solution of/second;
D, spinning solution are 80 ℃～95 ℃ in temperature, leave standstill to carry out deaeration in 4～10 hours under normal pressure;
E, through the spinning solution after the deaeration during at wet spinning, spray silk speed is 8～17 meters/minute, the coagulation bath that enters is salt and aqueous acid, its salt content is 420～438 grams per liters, acid content is 0.26～0.5 grams per liter, bath temperature is 38 ℃～43 ℃;
F, tow are 4～9 times at wet total draft multiple of bathing in drawing-off and the dry heat drafting;
G, in the acetalation program in later stage: the hydroformylation liquid temp is 65 ℃～70 ℃, and acetalation solution is the solution that contains aldehyde, acid and anhydrous sodium sulfate; Aldehydes content is 32～80 grams per liters, and acid content is 240～300 grams per liters; The content of anhydrous sodium sulfate is 120～200 grams per liters.
5. the manufacture method of synthetic plant protein filaments according to claim 4, it is characterized in that: initial temperature was 40 ℃～45 ℃ when the isolated protein after purifying was dissolved into solution again, pH value is 8.5～9, temperature is risen 8 ℃～12 ℃, pH value is every 1～1.5 value of rising in 2 hours, dissolution time is 6～8 hours, and the protein solution of dissolving adopts negative pressure to concentrate again.
6. the manufacture method of synthetic plant protein filaments according to claim 5 is characterized in that:
It is the solution that contains NaOH that isolated protein after a, described handle are purified dissolves used alkaline solution again;
Salt in b, the described coagulation bath is sodium sulphate, and acid is sulfuric acid;
Aldehyde is that formaldehyde, acid are the solution of sulfuric acid in c, the used solution of acetalation.
7. the manufacture method of synthetic plant protein filaments according to claim 5 is characterized in that:
It is the solution that contains potassium hydroxide that isolated protein after a, described handle are purified dissolves used alkaline solution again;
Salt in b, the coagulation bath is sodium chloride, and acid is hydrochloric acid;
Aldehyde is benzaldehyde in c, the used solution of acetalation, and acid is hydrochloric acid.
8. the manufacture method of synthetic plant protein filaments according to claim 5 is characterized in that:
It is the solution that contains NaOH that isolated protein after a, described handle are purified dissolves used alkaline solution again;
Salt in b, the described coagulation bath is sulfuric acid amine, and acid is hydrochloric acid;
Used aldehydes is a glutaraldehyde in c, the acetalation, and acid is sulfuric acid.
9. the manufacture method of synthetic plant protein filaments according to claim 5 is characterized in that:
It is the solution that contains potassium hydroxide that isolated protein after a, described handle are purified dissolves used alkaline solution again;
B, described salt of doubting in the solid body lotion are sodium sulphate, sodium chloride and sulfuric acid amine three's mixing, and acid is sulfuric acid;
Used aldehydes is a benzaldehyde in c, the acetalation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN99116636A CN1074474C (en) | 1999-09-01 | 1999-09-01 | Synthetic plant protein filaments |
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| CN99116636A CN1074474C (en) | 1999-09-01 | 1999-09-01 | Synthetic plant protein filaments |
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| CN1074474C true CN1074474C (en) | 2001-11-07 |
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| CN99116636A Expired - Lifetime CN1074474C (en) | 1999-09-01 | 1999-09-01 | Synthetic plant protein filaments |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1168858C (en) * | 2002-01-04 | 2004-09-29 | 李官奇 | Plant protein synthetic fiber and its manufacturing method |
| CN101649504B (en) * | 2009-09-10 | 2011-09-14 | 山东省花生研究所 | Preparation method of blend fiber of peanut protein and chitosin |
| CN102154731A (en) * | 2011-01-26 | 2011-08-17 | 尹兆明 | Animal blood protein fiber and preparation method thereof |
| CN102808237A (en) * | 2011-06-02 | 2012-12-05 | 陈福库 | Protein composite fiber for wig and manufacturing method thereof |
| CN102534859B (en) * | 2011-12-23 | 2014-01-01 | 上海全宇生物科技遂平有限公司 | Manufacturing method of soybean protein and polyvinyl alcohol polymerized fiber |
| CN102851774A (en) * | 2012-06-06 | 2013-01-02 | 武汉纺织大学 | Method for improving viscose fiber strength |
| CN103628165B (en) * | 2012-12-27 | 2016-03-30 | 青岛海芬海洋生物科技有限公司 | The preparation method of enteromorpha protein fiber |
| CN103334177B (en) * | 2013-07-31 | 2015-06-24 | 韩晓根 | Flame-retardant corn protein fiber production method and product thereof |
| CN103343395B (en) * | 2013-07-31 | 2015-06-24 | 韩晓根 | Production method and product of antibacterial corn protein fibers |
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|---|---|---|---|---|
| US552393A (en) * | 1895-12-31 | Combined driving and check rein | ||
| CN1062934A (en) * | 1990-12-24 | 1992-07-22 | 成都科技大学 | Silk-fibroin and polyvinyl alcohol blending fiber |
| CN2154866Y (en) * | 1993-02-12 | 1994-02-02 | 乐山市自动化仪表三厂 | Natural protein long silk spinning machine |
| US5750064A (en) * | 1996-01-19 | 1998-05-12 | E. I. Du Pont De Nemours And Company | Dry spinning process for producing zein fibers |
-
1999
- 1999-09-01 CN CN99116636A patent/CN1074474C/en not_active Expired - Lifetime
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US552393A (en) * | 1895-12-31 | Combined driving and check rein | ||
| CN1062934A (en) * | 1990-12-24 | 1992-07-22 | 成都科技大学 | Silk-fibroin and polyvinyl alcohol blending fiber |
| CN2154866Y (en) * | 1993-02-12 | 1994-02-02 | 乐山市自动化仪表三厂 | Natural protein long silk spinning machine |
| US5750064A (en) * | 1996-01-19 | 1998-05-12 | E. I. Du Pont De Nemours And Company | Dry spinning process for producing zein fibers |
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