CN1670274A - Soya protein/polyurethane/polyacrylonitrile blended composite fiber and its preparing method - Google Patents
Soya protein/polyurethane/polyacrylonitrile blended composite fiber and its preparing method Download PDFInfo
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Abstract
The invention discloses a manufacturing method for soyabean protein, polyammonia fats and polyacrylonitrile commixture compounding fiber. It takes dimethyl sulfoxide as solution to fully dissolving the three groups and forms the raw liquid for filature. The fiber would be produced by wet method. Using soyabean protein and polyammonia fat improves the moisture absorption, chromaticity, anti-static performace, resilience and comfort of the polyacrylonitrile. The invention could use the original device to manufacture the commixture compounding fiber and is benefit for the application for soyabean protein.
Description
Technical field
The invention belongs to Polymer Synthesizing fibre technology field, be specifically related in the polyacrylonitrile fibre spinning solution, add soybean protein and dyeability, antistatic behaviour, the resilience of polyurethane, improve a kind of preparation method of the wearing comfort of polyacrylonitrile fibre to improve polyacrylonitrile fibre.
Background technology
Be that the azlon of matrix just is subjected to the U.S., Europe and Japan as the cheap substitute of real silk and wool and greatly pays close attention at the 19th-century end with protein, but because the restriction of scientific and technological level, it is former thereby fail to realize suitability for industrialized production that the protein fibre of developing this period is poor because of physical and mechanical properties, the technical difficulty of preparation is big etc.Afterwards, reasons such as development owing to petro chemical industry, the researcher turns to the research direction of new fiber the development of synthetic fiber and regenerated celulose fibre, synthetic fiber have many premium properties, but also exist dyeability, hygroscopicity, gas permeability poor, the easy build up of electrostatic charge of fiber, shortcomings such as the easy pilling of fabric.The modern pursues naturalization, comfortableization, personalization, and natural fabric is subjected to increasing favor.But natural fabrics such as cotton, fiber crops, wool, silk are planted, the restriction of cultured area, can't develop in a large number.The chemical fibre degradation speed is slow simultaneously, cause serious environmental to pollute, and oil is limited in the storage capacity in the whole world, and the alternate resources of seeking oil is the focus that people pay close attention to always.Therefore since the end of the eighties, the research work to azlon both at home and abroad begins again to pay attention to.
With regenerated protein modifying chemical fiber performance, the normal method that adopts has: 1. polymeric modification: with regenerated protein and polymer monomer graft copolymerization, make product have the two excellent properties of natural high polymer and synthetic high polymer concurrently.The beginning sixties, Japanese Japan spins company and has studied soybean, corn protein grafted propylene nitrile, through process for spinning fibre by wet, relevant patent is seen the clear 37-18387 of Japan's special permission publishing bulletin, clear 38-9431, clear 39-90, clear 40-15821, clear 40-15823, clear 40-15979, clear 43-9748, clear 43-27407, clear 44-23137, clear 51-53098.But Japan spins company and has succeeded in developing casein grafted propylene nitrile fiber, and commodity are called " Chinon "; 2. blending and modifying, this method small investment of blending and modifying, instant effect are one of most active fields in current polymer material science and the engineering.Phytoprotein and polyvinyl alcohol or polyacrylonitrile or viscose glue blending fiber are seen relevant patents such as CN 01104271.0 CN99116636.1 CN 02138823.7 CN 03115288.0 respectively.
Polyacrylonitrile fibre is because good, antibiotic, the mildew-resistant of its full and warm property, mothproof, anti-illumination ageing, raw material is easy to get, and very superior radiation resistance and corrosion resistance are arranged and be widely used in dress ornament, decoration and industrial circle, its output is positioned at the 4th in synthetic fiber at present.But because intrinsic hydrophobicity and the insulating properties of polyacrylonitrile fibre, its feel, hygroscopicity, dyeability are relatively poor, easily produce static, have limited the application of polyacrylonitrile in a lot of fields.
In common vegetable seeds, the albumen quality that soybean contains is maximum.Most soya seeds contains the protein of 30-45%, extracts the soybean protein isolate obtain by defatted soybean meal and then contains protein more than 90%.Output is big because soybean protein has, recyclability, biodegradable and compare comparatively cheap price with animal protein, and beans belongs to fixed nitrogen class plant simultaneously, helps the protection of soil.So soybean protein is one of focus of regenerated protein research at present.
Polyurethane fiber is a kind of highly elastic fiber, and its elongation at break is greater than 400%, and the elastic restoration ratio during deformation 300% is more than 95%, and this is that any fiber is incomparable.Polyurethane macromolecular is a kind of line-type block polymer, is made up of soft chain segment and hard segment, wherein is gathered into microcell by stronger intermolecular force such as hydrogen bond between the hard segment.
Summary of the invention
The object of the invention provides a kind of soybean protein/polyurethane/polyacrylonitrile blended composite fiber, to overcome the existing defective of homogenous material;
The object of the invention provides a kind of method for preparing soybean protein/polyurethane/polyacrylonitrile blended composite fiber.
The present invention utilizes soybean protein to improve hygroscopicity, dyeability and the antistatic behaviour of polyacrylonitrile fibre; Utilize the high resilience of polyurethane elastomeric fiber to improve the resilience of polyacrylonitrile fibre, to reach the purpose that improves the polyacrylonitrile fibre wearing comfort.
Soybean protein/polyurethane provided by the present invention/polyacrylonitrile blended composite fiber is by soybean protein, polyurethane and polyacrylonitrile blended being composited, wherein: the parts by weight of soybean protein are 5-30 part, the parts by weight of polyacrylonitrile are 90-60 part, and the parts by weight of polyurethane are 5-10 part.
The preparation method of soybean protein/polyurethane of the present invention/polyacrylonitrile blended composite fiber comprises the steps:
With weight concentration is that 9～15% soybean protein Dimesulfoxid solution, weight concentration are that 15～20% polyacrylonitrile dimethyl sulfoxide solution and weight concentration are that 20～35% polyurethane dimethyl sulfoxide solution mixes, obtain spinning slurry, wherein, soy proteinaceous parts by weight are 5-30 part, the parts by weight of polyacrylonitrile are 90-60 part, the parts by weight of polyurethane are 5-10 part, and the weight solid content in the spinning slurry is 15-25%.
The polyacrylonitrile dimethyl sulfoxide solution is directly synthetic or obtains through concentrating or being dissolved in the methyl-sulfoxide by the fibrous polypropylene nitrile that the solid content of polyacrylonitrile is 12-20% in the solution;
The polyurethane dimethyl sulfoxide solution is directly synthetic or obtains through concentrating or being dissolved in the methyl-sulfoxide by fibre-grade polyurethane that the solid content of polyurethane is 15-35% in the solution;
The soybean protein dimethyl sulfoxide solution is to adopt following method preparation:
Soy proteinaceous solid content is 9-15% in the soybean protein dimethyl sulfoxide solution.
The spinning slurry addressed through the vacuum discontinuous degassing, is filtered, and spinning solution is pressed in the coagulating bath through spinning head, coagulating bath is that weight concentration is the methyl-sulfoxide aqueous solution of 50-60%, bathe warm 20-30 ℃, spinning speed 5-10m/min, coagulating bath can be one or more levels;
Spun fiber carries out low power through pre-heating bath and stretches, and the preheating bath temperature is 30-60 ℃, and the weight content of methyl-sulfoxide is 2.5-3%, and draw ratio is 1.5-2.5 times;
The tow that goes out after the pre-heating bath still contains a certain amount of methyl-sulfoxide, and washing about 40～60 ℃ makes methyl-sulfoxide content in the fiber of washing back less than 0.1%;
Fiber after the washing is 80-140 ℃ of following drawing-off, and draw ratio is 5-10 times;
At 80-180 ℃ of following compacting by drying, under 70-100 ℃ temperature, curl then, at last 80-160 ℃ of following decatize typing.
It is raw material that the present invention adopts the soybean protein isolates and the polyurethane that extract in the oil expression soybean meal afterwards, utilize the acid-dyeable of protein, compatibility with human body, improve dyeability, the antistatic behaviour of polyacrylonitrile fibre, utilize the high elasticity raising soybean protein of polyurethane fiber and the resilience of polyacrylonitrile blended composite fiber.This fiber has promptly kept the original advantage of polyacrylonitrile fibre, has overcome the shortcoming of polyacrylonitrile fibre static electrification and human body compatibility difference again, to reach the purpose that improves the polyacrylonitrile fibre wearing comfort.Aspect fiber preparation method, can utilize the original production equipment of polyacrylonitrile fibre substantially, needn't carry out big change, only needing to add some simple equipment gets final product, accessory substance to crops has carried out deep processing and utilization more simultaneously, adopt the substitute of reproducible, degradable phytoprotein, help producing new economic benefit as the part petroleum resources.
The specific embodiment
To help to understand the present invention by following examples, but not limit content of the present invention.
Embodiment 1
10 kilograms soybean proteins are added in 90 kilograms of methyl-sulfoxide/urea mixed solvents, and stirring also slowly heats up makes it abundant dissolving, obtains transparent soybean protein solution; In the mixed solvent, the weight concentration of cosolvent urea is 10%;
17 kilograms of polyacrylonitrile are dissolved in 83 kilograms of methyl-sulfoxides;
The weight solid content of synthesis of polyurethane is 25% resin liquid.
Above-mentioned three kinds of solution are mixed with spinning solution in proportion, and wherein soy proteinaceous parts by weight are 15 parts, and the parts by weight of polyurethane are 5 parts, and the parts by weight of polyacrylonitrile are 80 parts.
The total solid content of ter-polymers in spinning solution is 18%.
Above-mentioned spinning solution is filtered after spinning head and being pressed in the coagulating bath through the vacuum discontinuous degassing, and coagulating bath is 50% the methyl-sulfoxide aqueous solution, bathes 25 ℃ of temperature, spinning speed 8m/min.As-spun fibre is 60 ℃ bathing temperature, and solvent is to carry out 1.5 times stretching in 3% the pre-heating bath.With 50 ℃ desalted water fiber is washed then, in 98 ℃ steam bath, stretched 8 times.Fiber after the washing carries out compacting by drying under 100 ℃ of conditions, dried fiber curls under 90 ℃ temperature, and the decatize typing is carried out in the back in temperature is 140 ℃ decatize typing pot, obtain soybean protein polyurethane polyacrylonitrile blended composite fiber.Line density, fracture strength and elongation at break with reference to GB/T14335-93 and GB/T14337-93 test calculating soybean protein polyurethane polyacrylonitrile blended composite fiber see Table sample 1 in 1.
Embodiment 2
12 kilograms soybean proteins are added in 88 kilograms of methyl-sulfoxide/urea mixed solvents, and stirring also slowly heats up makes it abundant dissolving, obtains transparent soybean protein solution; In the mixed solvent, the weight concentration of cosolvent urea is 14%;
20 kilograms of polyacrylonitrile are dissolved in 80 kilograms of methyl-sulfoxides;
The synthesis of polyurethane solid content is 28% resin liquid.Above-mentioned three kinds of solution are mixed with spinning solution in proportion, and wherein soy proteinaceous parts by weight are 12 parts, and the parts by weight of polyurethane are 8 parts, and the parts by weight of polyacrylonitrile are 80 parts.
Ter-polymers in spinning solution total solid content be 20%.
Above-mentioned spinning solution is filtered after spinning head and being pressed in the coagulating bath through the vacuum discontinuous degassing, and coagulating bath is 55% the methyl-sulfoxide aqueous solution, bathes 30 ℃ of temperature, spinning speed 10m/min.As-spun fibre is 60 ℃ bathing temperature, and solvent is to carry out 1.4 times stretching in 3% the pre-heating bath.With 50 ℃ desalted water fiber is washed then, in 90 ℃ steam bath, stretched 9 times.Fiber after the washing carries out compacting by drying under 120 ℃ of conditions, dried fiber curls under 85 ℃ temperature, and the decatize typing is carried out in the back in temperature is 130 ℃ decatize typing pot, obtain soybean protein polyurethane polyacrylonitrile blended composite fiber.Line density, fracture strength and elongation at break with reference to GB/T14335-93 and GB/T14337-93 test calculating soybean protein polyurethane polyacrylonitrile blended composite fiber see Table sample 2 in 1.
Embodiment 3
15 kilograms soybean proteins are added in 85 kilograms of methyl-sulfoxide/urea mixed solvents, and stirring also slowly heats up makes it abundant dissolving, obtains transparent soybean protein solution; In the mixed solvent, the weight concentration of cosolvent urea is 14%;
20 kilograms of polyacrylonitrile are dissolved in 80 kilograms of methyl-sulfoxides;
The synthesis of polyurethane solid content is 30% resin liquid.
Above-mentioned three kinds of solution are mixed with spinning solution in proportion, and wherein soy proteinaceous parts by weight are 15 parts, and the weight polyurethane umber is 10 parts, and the polyacrylonitrile parts by weight are 75 parts.
The total solid content of ter-polymers in spinning solution is 20%.
Above-mentioned spinning solution is filtered after spinning head and being pressed in the coagulating bath through the vacuum discontinuous degassing, and coagulating bath is 50% the methyl-sulfoxide aqueous solution, bathes 30 ℃ of temperature, spinning speed 10m/min.As-spun fibre is 55 ℃ bathing temperature, and solvent is to carry out 1.5 times stretching in 3% the pre-heating bath.With about 50 ℃ desalted water fiber is washed then, in 90 ℃ steam bath, stretched 9 times.Fiber after the washing carries out compacting by drying under 110 ℃ of conditions, dried fiber curls under 95 ℃ temperature, and the decatize typing is carried out in the back in temperature is 135 ℃ decatize typing pot, obtain soybean protein polyurethane polyacrylonitrile blended composite fiber.Line density, fracture strength and elongation at break with reference to GB/T14335-93 and GB/T14337-93 test calculating soybean protein polyurethane polyacrylonitrile blended composite fiber see Table sample 3 in 1.
Embodiment 4
15 kilograms soybean proteins are added in 85 kilograms of methyl-sulfoxide/guanidine hydrochloride mixed solvents, and stirring also slowly heats up makes it abundant dissolving, obtains transparent soybean protein solution, and in the mixed solvent, the weight concentration of cosolvent guanidine hydrochloride is 15%;
20 kilograms of polyacrylonitrile are dissolved in 80 kilograms of methyl-sulfoxides;
The synthesis of polyurethane solid content is 30% resin liquid.
Above-mentioned three kinds of solution are mixed with spinning solution in proportion, and wherein soy proteinaceous parts by weight are 15 parts, and the parts by weight of polyurethane are 10 parts, and the parts by weight of polyacrylonitrile are 75 parts.The total solid content of ter-polymers in spinning solution is 20%.
Above-mentioned spinning solution is filtered after spinning head and being pressed in the coagulating bath through the vacuum discontinuous degassing, and coagulating bath is 50% the methyl-sulfoxide aqueous solution, bathes 30 ℃ of temperature, spinning speed 10m/min.As-spun fibre is 55 ℃ bathing temperature, and solvent is to carry out 1.5 times stretching in 3% the pre-heating bath.With about 50 ℃ desalted water fiber is washed then, in 90 ℃ steam bath, stretched 9 times.Fiber after the washing carries out compacting by drying under 110 ℃ of conditions, dried fiber curls under 95 ℃ temperature, and the decatize typing is carried out in the back in temperature is 135 ℃ decatize typing pot, obtain soybean protein polyurethane polyacrylonitrile blended composite fiber.Line density, fracture strength and elongation at break with reference to GB/T14335-93 and GB/T14337-93 test calculating soybean protein polyurethane polyacrylonitrile blended composite fiber see Table sample 4 in 1.
Embodiment 5
Is with weight fraction 15% (to need identical narration with the above embodiments? 15 kilograms) soybean protein isolates add in 85 kilograms of methyl-sulfoxide/guanidine hydrochloride mixed solvents, stir and slowly heat up and make it abundant dissolving, obtain transparent soybean protein solution, in the mixed solvent, the weight concentration of cosolvent guanidine hydrochloride is 15%;
20 kilograms of polyacrylonitrile are dissolved in 80 kilograms of methyl-sulfoxides;
The synthesis of polyurethane solid content is 28% resin liquid.
Above-mentioned three kinds of solution are mixed with spinning solution in proportion, and wherein soybean protein accounts for 15 parts of total solid content, and polyurethane accounts for 10 parts of total solid content, and polyacrylonitrile accounts for 75 parts of total solid content.The total solid content of ter-polymers in spinning solution is 18%.
Above-mentioned spinning solution is filtered after spinning head and being pressed in the coagulating bath through the vacuum discontinuous degassing, and coagulating bath is 55% the methyl-sulfoxide aqueous solution, bathes 35 ℃ of temperature, spinning speed 10m/min.As-spun fibre is 55 ℃ bathing temperature, and solvent is to carry out 1.6 times stretching in 2.5% the pre-heating bath.With about 50 ℃ desalted water fiber is washed then, in 95 ℃ steam bath, stretched 9 times.Fiber after the washing carries out compacting by drying under 120 ℃ of conditions, dried fiber curls under 90 ℃ temperature, and the decatize typing is carried out in the back in temperature is 140 ℃ decatize typing pot, obtain soybean protein polyurethane polyacrylonitrile blended composite fiber.Line density, fracture strength and elongation at break with reference to GB/T14335-93 and GB/T14337-93 test calculating soybean protein polyurethane polyacrylonitrile blended composite fiber see Table sample 5 in 1.
Table 1: the performance summary sheet of the fiber sample among the embodiment
| Sequence number | Line density (dt) | Fracture strength (cN/dt) | Elongation at break (%) |
| Sample 1 | ?1.69 | ?1.90 | ?52.11 |
| Sample 2 | ?1.64 | ?2.22 | ?48.72 |
| Sample 3 | ?3.17 | ?1.98 | ?53.77 |
| Sample 4 | ?3.26 | ?2.14 | ?51.65 |
| Sample 5 | ?6.58 | ?1.76 | ?50.01 |
Claims (9)
1. soybean protein/polyurethane/polyacrylonitrile blended composite fiber is characterized in that, the parts by weight of soybean protein are 5-30 part, and the parts by weight of polyacrylonitrile are 90-60 part, and the parts by weight of polyurethane are 5-10 part.
2. the preparation method of soybean protein/polyurethane according to claim 1/polyacrylonitrile blended composite fiber is characterized in that, comprises the steps:
Soybean protein dimethyl sulfoxide solution, polyacrylonitrile dimethyl sulfoxide solution and polyurethane dimethyl sulfoxide solution are mixed, obtain spinning slurry;
The spinning slurry addressed through the vacuum discontinuous degassing, is filtered, and spinning solution is pressed in the coagulating bath through spinning head;
Spun fiber carries out low power through pre-heating bath and stretches;
Hot wash;
The drawing-off in hot water or steam of fiber after the washing;
Compacting by drying curls then, last decatize typing.
3. method according to claim 2, it is characterized in that, with weight concentration is that 9～15% soybean protein dimethyl sulfoxide solution, weight concentration are that 15～20% polyacrylonitrile dimethyl sulfoxide solution and weight concentration are that 20～35% polyurethane dimethyl sulfoxide solution mixes, and obtains spinning slurry.
4. method according to claim 2 is characterized in that, in the spinning slurry, soy proteinaceous parts by weight are 5-30 part, the parts by weight of polyacrylonitrile are 90-60 part, and the parts by weight of polyurethane are 5-10 part, and the weight solid content in the spinning slurry is 15-25%.
5. method according to claim 4 is characterized in that, the polyacrylonitrile dimethyl sulfoxide solution is directly synthetic or obtains through concentrating or being dissolved in the methyl-sulfoxide by the fibrous polypropylene nitrile that the solid content of polyacrylonitrile is 12-20% in the solution;
The polyurethane dimethyl sulfoxide solution is directly synthetic or obtains through concentrating or being dissolved in the methyl-sulfoxide by fibre-grade polyurethane that the solid content of polyurethane is 15-35% in the solution;
Soy proteinaceous solid content is 15-35% in the soybean protein dimethyl sulfoxide solution.
6. method according to claim 2 is characterized in that, coagulating bath is that weight concentration is the methyl-sulfoxide aqueous solution of 50-60%, bathes warm 20-30 ℃, spinning speed 5-10m/min, and coagulating bath can be one or more levels.
7. method according to claim 2 is characterized in that, the preheating bath temperature is 30-60 ℃, and draw ratio is 1.5-2.5 times.
8. method according to claim 2 is characterized in that, goes out tow after the pre-heating bath 40～60 ℃ of washings.
9. method according to claim 2 is characterized in that, the fiber after the washing is 80-140 ℃ of following drawing-off, and draw ratio is 5-10 times;
At 80-180 ℃ of following compacting by drying, under 70-100 ℃ temperature, curl then, at last 80-160 ℃ of following decatize typing.
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| CN1298902C (en) * | 2005-03-14 | 2007-02-07 | 东华大学 | Plant protein/polyurethane/polyacrylonitrile blended composite fiber and preparing process |
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| CN105088407A (en) * | 2015-09-15 | 2015-11-25 | 苏州顺唐化纤有限公司 | Preparation method for hydrophilic polyacrylonitrile fibers |
| CN105113042A (en) * | 2015-09-15 | 2015-12-02 | 苏州顺唐化纤有限公司 | Moisture-absorption polyacrylonitrile fiber |
| CN108221179A (en) * | 2017-12-29 | 2018-06-29 | 孙祎 | A kind of preparation method of moisture absorption heating Anti-bacteria yarn |
| CN108424632A (en) * | 2018-04-19 | 2018-08-21 | 钱兴 | A kind of waterproof tensile stretches the preparation method of strap |
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| CN109957851A (en) * | 2019-03-25 | 2019-07-02 | 四川大学 | One kind matter containing heavy metal biological-polymer composite fiber and preparation method thereof |
| CN110484991A (en) * | 2019-08-28 | 2019-11-22 | 安徽宜民服饰股份有限公司 | A kind of preparation method of high-performance refractory blend fibre |
| CN110685035A (en) * | 2019-10-23 | 2020-01-14 | 台州市旭泓服饰有限公司 | Special enhanced elastic composite protein fiber for close-fitting textiles and preparation method |
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