CN109881279A - A kind of ionic liquid method regeneration animal ceratin fiber and preparation method thereof - Google Patents
A kind of ionic liquid method regeneration animal ceratin fiber and preparation method thereof Download PDFInfo
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Abstract
A kind of ionic liquid method regeneration animal ceratin fiber, with ionic liquid, by the animal ceratin of crushing, swelling, dissolution, crosslinking, deaeration, filling under crosslinking agent and self-crosslinking agent synergistic effect are mixed, and are obtained through dry-jet wet-spinning, drying, self-crosslinking.The present invention selects ionic liquid as the solvent of regeneration animal ceratin, under crosslinking agent and self-crosslinking agent synergistic effect, animal ceratin fiber is made by physics-chemical method dry-jet wet-spinning, solvent is environmentally protective, is easily recycled.
Description
Technical field
The invention belongs to textile technology field, it is related to a kind of ionic liquid method regeneration animal ceratin fiber and its production side
Method.
Background technique
Currently, regenerated protein be divided into aftergrowth azelon and regeneration animal ceratin fiber, fiber mostly be by
Natural animal and plant albumen depends on that other macromolecule carriers are composite regenerated, and CN99116636, CN03111737 patent disclose
Vegetable protein and polyvinyl alcohol have produced the composite fibre of vegetable protein, and CN03111915, CN02115722 patent
Then disclose protein composite fibre made from animal hair albumen and polyvinyl alcohol blending.Use ionic liquid as novel molten
In terms of agent prepares albumen spinning glue, CN201210070496 patent, which is disclosed, dissolves peanut protein using glyoxaline ion liquid
With the mixture of polyvinyl alcohol, peanut protein/polyvinyl alcohol composite fiber has been produced；CN201310700758,
CN201610362616 patent is individually disclosed to be spun with phosphoric acid ester, miscellaneous bicyclic class ion liquid dissolving animal hair keratin preparation
The method of silk liquid.Native protein forms spherical high polymer after crushing, dissolving, and at silk difficulty, therefore, above-mentioned patent will
Native protein is directly mixed with other high molecular polymers, is fabricated to fiber by other high molecular polymer chain stress,
The strength of terminal fiber will receive certain influence, and the protein in regenerated protein composite fibre obtained is blended in its textile
It is easy to be lost during final finishing (especially alkali process).
Summary of the invention
The purpose of the present invention is to provide a kind of ionic liquid methods to regenerate animal ceratin fiber, while providing its production method
It is another goal of the invention of the invention.
In order to achieve the above objectives, the present invention takes following technical scheme:
A kind of ionic liquid method regeneration animal ceratin fiber, with ionic liquid by the animal ceratin of crushing in crosslinking agent and selfing
Join the lower swelling of agent synergistic effect, dissolution, crosslinking, deaeration, is obtained through filling mixing, dry-jet wet-spinning, drying, self-crosslinking.
The ionic liquid is glyoxaline ion liquid.
The ionic liquid is made of A, part B；Part A is -3 methylimidazole of 1- ethyl (EMIM), -3 first of 1- allyl
One of base imidazoles (AMIM), N- methylimidazole (HMIM), -3 methylimidazole of 1- butyl (BMIM) cationoid；
Part B is AlCl- 3、BrCl- 3、BrI- 2、AlBr- 4、FHF-、BF- 4、PF- 6、CF3SO- 3、SbF- 6 、Ac-Or phosphate ester salt
(DEP) one of anionoid.
The crosslinking agent is 3- (2- pyridine dimercapto) propionic acid N-hydroxy-succinamide ester (SPDP), glyoxal, penta
One of dialdehyde, aromatic aldehyde, salicylide.
The self-crosslinking agent is acrylamide analog derivative.
The self-crosslinking agent is N hydroxymethyl acrylamide (NMA) or N, N'- methylene-bisacrylamide (MBA).
It is 25%-99% that ionic liquid, which accounts for ionic liquid and the percentage of animal ceratin gross mass,；Dosage of crosslinking agent accounts for
The percentage 0.5%-5% of object angle protein by weight；Self-crosslinking agent dosage accounts for the percentage 1%-10% of animal ceratin weight.
The production method of the ionic liquid method regeneration animal ceratin fiber, comprising the following steps:
1) it is swollen: mixed be incorporated under room temperature of smashed animal ceratin and ionic liquid is swollen 0.5h-for 24 hours；
2) it dissolves: the mixed material being swollen being warming up to 60 DEG C -120 DEG C in 1h-2h in mechanical stirring and is dissolved, when dissolution
Between control within 12 hours, form sticky glue；
3) be crosslinked: the glue dissolved is made under mechanical stirring in 1-2h in step 2 by -120 DEG C of control system temperature 50 C
Interior dropwise addition crosslinking agent, crosslinking time 20min-8h；
4) deaeration: by glue obtained by removing the bubble in glue within vacuum defoamation for 24 hours；
5) filling mixing: self-crosslinking agent is filled in spinning glue by injection method before spinning, by mechanical mixture at spinning glue
Liquid；
6) dry-jet wet spinning process forms: uniformly mixed spinning glue is pulled out initial state regeneration by dry-jet wet-spinning moulding process
Keratin protein fiber；Wherein, coagulation bath temperature control is between 0 DEG C -75 DEG C；
7) dry self-crosslinking: will regeneration animal ceratin fiber by baking process, the control of drying self-crosslinking temperature 80 DEG C-
Between 130 DEG C, animal keratin and self-crosslinking agent are copolymerized in fiber, self-crosslinking time 3min-20min.
The coagulating bath that dry-jet wet spinning process molding uses is water or the water solution system being made of water/alcohols.Wherein water
Amount ratio with alcohols is (4-6): 1, when coagulating bath uses water/alcohols, coagulation bath temperature is 0-40 DEG C, when coagulating bath is water
When, coagulation bath temperature is 0 DEG C -75 DEG C, preferably 30 DEG C -75 DEG C.
Alcohols in the water/alcohols coagulating bath is one of methanol, ethyl alcohol, propyl alcohol and butanol, uses water with simple
System is compared, and can accelerate the diffusion velocity of ionic liquid in aqueous solution using water/alcohols coagulating bath, and promotes to regenerate animal horn
Azelon coagulation forming rate helps to improve the strength and spinning speed of fiber.But the additional amount of alcohols should not be too large, if
Additional amount is excessive, then it is too fast to regenerate animal ceratin fibre solidification molding rate, drops low-fiber strength instead.
Compared with prior art, the present invention has following technical effect that the present invention is that natural animal keratolysis exists
In ionic liquid, then make the carbonyl on amino and crosslinking agent on protein that nucleophilic Schiff occur under crosslinking action
Alkali reaction, forms chain macromolecule between protein, then by the acrylamide analog derivative self-crosslinking agent that the later period adds,
Fiber baking zone forms alternate interpenetrating networks shape condensate between self-crosslinking agent and the chain protein molecule of crosslinking early period, mentions
The high tensile stress of final fiber, strength >=1.4CN/dtex, and this method rational technology, the fibre prepared
The style of natural protein fiber is maintained, fibre property is stablized, suitable for scale production and popularization.
Specific embodiment
Using specific embodiment, the present invention will be further described below.
Embodiment 1
A kind of ionic liquid method regeneration animal ceratin fiber, the regeneration animal ceratin fiber moving crushing by ionic liquid
Object angle albumen crosslinking agent and self-crosslinking agent synergistic effect under swelling, dissolution, crosslinking, deaeration, fill mix, through dry-jet wet-spinning,
Drying, self-crosslinking obtain.
In the present embodiment, the ionic liquid is made of A, part B, and the part A is -3 methylimidazole of 1- ethyl
(EMIM) cationic.Part B is phosphate ester salt (DEP) anionoid.The crosslinking agent is 3- (2- pyridine dimercapto) propionic acid
N-hydroxy-succinamide ester (SPDP).The self-crosslinking agent is N hydroxymethyl acrylamide (NMA).
It is 50% that ionic liquid, which accounts for ionic liquid and the percentage of animal ceratin gross mass,；Dosage of crosslinking agent accounts for animal horn
The percentage of protein by weight is 5%；The percentage that self-crosslinking agent dosage accounts for animal ceratin weight is 1%.
The production method of the ionic liquid method regeneration animal ceratin fiber, comprising the following steps:
1) it is swollen: mixed be incorporated under room temperature of smashed animal ceratin and ionic liquid is swollen 0.5h；
2) it dissolves: being warming up to 60 DEG C of dissolutions by the mixed material being swollen in mechanical stirring and in 1h, dissolution time is controlled 10
Hour, form sticky glue；
3) it is crosslinked: 120 DEG C of control system temperature, step 2 being made to the glue dissolved and is handed under mechanical stirring in dropwise addition in 1h
Join agent, crosslinking time 20min；
4) deaeration: by glue obtained by vacuum defoamation 20h, the bubble in glue is removed；
5) filling mixing: self-crosslinking agent is filled in spinning glue by injection method before spinning, by mechanical mixture at spinning glue
Liquid；
6) dry-jet wet spinning process forms: uniformly mixed spinning glue is pulled out initial state regeneration by dry-jet wet-spinning moulding process
Keratin protein fiber；Wherein, coagulation bath temperature control is at 25 DEG C；The coagulating bath that dry-jet wet spinning process molding uses is water/ethyl alcohol
The water solution system of composition.The mass ratio of water and ethyl alcohol is 4:1；Washed arrangement later: washing by 1-3 road washing procedures,
The ionic liquid carried on fiber is washed away, washing is washed using 20-60 DEG C of deionized water；7) it dries self-crosslinking: will regenerate
Animal ceratin fiber is by baking process, and drying self-crosslinking temperature control is at 100 DEG C, animal keratin and selfing in fiber
Join agent copolymerization, self-crosslinking time 3min；
8) finished product: the fiber dried after self-crosslinking is wound into cylinder or cutting is packaged.
Embodiment 2
The present embodiment intermediate ion liquid method regenerates animal ceratin fiber, and difference from Example 1 is:
The ionic liquid is made of A, part B, and part A is -3 methylimidazole of 1- allyl (AMIM) cationoid.The portion B
It is divided into AlCl- 3Anionoid.The crosslinking agent is glyoxal.The self-crosslinking agent is N, N'- methylene-bisacrylamide
(MBA).It is 25% that ionic liquid, which accounts for ionic liquid and the percentage of animal ceratin gross mass,；Dosage of crosslinking agent accounts for animal horn egg
The percentage of Bai Chongliang is 0.5%；The percentage that self-crosslinking agent dosage accounts for animal ceratin weight is 10%.
Its production method, comprising the following steps:
1) it is swollen: mixed be incorporated under room temperature of smashed animal ceratin and ionic liquid is swollen for 24 hours；
2) it dissolves: being warming up to 120 DEG C of dissolutions by the mixed material being swollen in mechanical stirring and in 1h, dissolution time is controlled 12
Hour, form sticky glue；
3) be crosslinked: step 2 is made the glue dissolved and handed under mechanical stirring in dropwise addition in 2h by control system temperature 50 C
Connection agent, crosslinking time 8 hours；
4) deaeration: for 24 hours by vacuum defoamation by glue obtained, the bubble in glue is removed；
5) filling mixing: self-crosslinking agent is filled in spinning glue by injection method before spinning, by mechanical mixture at spinning glue
Liquid；
6) dry-jet wet spinning process forms: uniformly mixed spinning glue is pulled out initial state regeneration by dry-jet wet-spinning moulding process
Keratin protein fiber；Wherein, coagulation bath temperature control is at 75 DEG C；The coagulating bath that dry-jet wet spinning process molding uses is water；Later
Washed arrangement: washing by 1-3 road washing procedures, washes away the ionic liquid carried on fiber, and washing uses 20-60 DEG C
Deionized water washing；
7) dry self-crosslinking: by regeneration animal ceratin fiber by baking process, drying self-crosslinking temperature is controlled at 130 DEG C,
Animal keratin and self-crosslinking agent are copolymerized in fiber, and the self-crosslinking time 3 minutes；
8) finished product: the fiber dried after self-crosslinking is wound into cylinder or cutting is packaged.
Embodiment 3
The present embodiment intermediate ion liquid method regenerates animal ceratin fiber, and difference from Example 1 is:
The ionic liquid is made of A, part B, and the part A is N- methylimidazole (HMIM), -3 methylimidazole of 1- butyl
(BMIM) cationoid.The part B is CF3SO- 3.The crosslinking agent is salicylide.The self-crosslinking agent is N, N'- methylene
Base bisacrylamide (MBA).
It is 90% that ionic liquid, which accounts for ionic liquid and the percentage of animal ceratin gross mass,；Dosage of crosslinking agent accounts for animal horn
The percentage 5% of protein by weight；Self-crosslinking agent dosage accounts for the percentage 5% of animal ceratin weight.
The production method of the ionic liquid method regeneration animal ceratin fiber, comprising the following steps:
1) it is swollen: mixed be incorporated under room temperature of smashed animal ceratin and ionic liquid is swollen 10h；
2) it dissolves: being warming up to 60 DEG C of dissolutions by the mixed material being swollen in mechanical stirring and in 1h, dissolution time is controlled 10
Hour, form sticky glue；
3) it is crosslinked: 120 DEG C of control system temperature, step 2 being made to the glue dissolved and is handed under mechanical stirring in dropwise addition in 1h
Connection agent, crosslinking time 8 hours；
4) deaeration: by glue obtained by vacuum defoamation 20h, the bubble in glue is removed；
5) filling mixing: self-crosslinking agent is filled in spinning glue by injection method before spinning, by mechanical mixture at spinning glue
Liquid；
6) dry-jet wet spinning process forms: uniformly mixed spinning glue is pulled out initial state regeneration by dry-jet wet-spinning moulding process
Keratin protein fiber；Wherein, coagulation bath temperature control is between 0 DEG C；The dry-jet wet spinning process coagulating bath that uses of molding for by water/
The water solution system of ethyl alcohol composition；The mass ratio of water and ethyl alcohol is 6:1；Washed arrangement later: pass through 1-3 road washing procedures
Washing, washes away the ionic liquid carried on fiber, and washing is washed using 20-60 DEG C of deionized water；
7) dry self-crosslinking: by regeneration animal ceratin fiber by baking process, drying self-crosslinking temperature control is fine at 80 DEG C
Animal keratin and self-crosslinking agent are copolymerized in tieing up, and the self-crosslinking time 20 minutes；
8) finished product: the fiber dried after self-crosslinking is wound into cylinder or cutting is packaged.
Claims (10)
1. a kind of ionic liquid method regenerates animal ceratin fiber, which is characterized in that with ionic liquid by the animal ceratin of crushing
Swelling, dissolution, crosslinking, deaeration, filling mixing under crosslinking agent and self-crosslinking agent synergistic effect, through dry-jet wet-spinning, drying, selfing
Connection obtains.
2. ionic liquid method as described in claim 1 regenerates animal ceratin fiber, which is characterized in that the ionic liquid is miaow
Azole ionic liquid.
3. ionic liquid method as claimed in claim 2 regenerates animal ceratin fiber, which is characterized in that the ionic liquid by A,
Part B is constituted；Part A is -3 methylimidazole of 1- ethyl (EMIM), -3 methylimidazole of 1- allyl (AMIM), N- methylimidazole
(HMIM), one of -3 methylimidazole of 1- butyl (BMIM) cationoid；Part B is AlCl- 3、BrCl- 3、BrI- 2、AlBr- 4、
FHF-、BF- 4、PF- 6、CF3SO- 3、SbF- 6 、Ac-Or one of phosphate ester salt (DEP) anionoid.
4. ionic liquid method as described in claim 1 regenerates animal ceratin fiber, which is characterized in that the crosslinking agent is 3-
(2- pyridine dimercapto) propionic acid N-hydroxy-succinamide ester (SPDP), glyoxal, glutaraldehyde, aromatic aldehyde, in salicylide
It is a kind of.
5. ionic liquid method as described in claim 1 regenerates animal ceratin fiber, which is characterized in that the self-crosslinking agent is third
Acrylamide derivative.
6. ionic liquid method as claimed in claim 5 regenerates animal ceratin fiber, which is characterized in that the self-crosslinking agent is N-
Hydroxymethyl acrylamide (NMA) or N, N'- methylene-bisacrylamide (MBA).
7. ionic liquid method as described in claim 1 regenerates animal ceratin fiber, which is characterized in that the ionic liquid account for from
Sub- liquid and the percentage of animal ceratin gross mass are 25%-99%；Dosage of crosslinking agent accounts for the percentage of animal ceratin weight
0.5%-5%；Self-crosslinking agent dosage accounts for the percentage 1%-10% of animal ceratin weight.
8. the production method of ionic liquid method regeneration animal ceratin fiber as claimed in claim 1 to 7, which is characterized in that packet
Include following steps:
1) it is swollen: mixed be incorporated under room temperature of smashed animal ceratin and ionic liquid is swollen 0.5h-for 24 hours；
2) it dissolves: the mixed material being swollen is dissolved in being warming up to 60 DEG C -120 DEG C in 1h-2h under stiring, when dissolution
Between control within 12 hours, form sticky glue；
3) be crosslinked: the glue that has dissolved is made under stiring in dripping in 1h-2h in step 2 by -120 DEG C of control system temperature 50 C
Add crosslinking agent, crosslinking time 20min-8h；
4) deaeration: by glue obtained by removing the bubble in glue within vacuum defoamation for 24 hours；
5) filling mixing: self-crosslinking agent is filled in spinning glue by injection method before spinning, is mixed into spinning glue；
6) dry-jet wet-spinning forms: uniformly mixed spinning glue is pulled out initially by dry-jet wet-spinning moulding process in coagulating bath
State regenerates animal keratin fiber；Wherein, coagulation bath temperature control is between 0-75 DEG C；
7) dry self-crosslinking: by regeneration animal ceratin fiber by drying self-crosslinking process, drying self-crosslinking temperature control exists
Between 80 DEG C -130 DEG C, animal keratin and self-crosslinking agent are copolymerized in fiber, self-crosslinking time 3min-20min.
9. the production method of ionic liquid method regeneration animal ceratin fiber as claimed in claim 8, which is characterized in that dry to squirt
The coagulating bath that spinning process molding uses is water or the water solution system being made of water/alcohols.
10. the production method of ionic liquid method regeneration animal ceratin fiber as claimed in claim 9, which is characterized in that described
Alcohols is one of methanol, ethyl alcohol, propyl alcohol, butanol.
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Cited By (1)
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| US20210363095A1 (en) * | 2020-02-27 | 2021-11-25 | Nankai University | Method capable of realizing preparation and in-situ separation of oligomeric ricinoleate |
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