CN103789857A - Preparation method of collagen regenerated cellulose fiber - Google Patents
Preparation method of collagen regenerated cellulose fiber Download PDFInfo
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- CN103789857A CN103789857A CN201410013961.6A CN201410013961A CN103789857A CN 103789857 A CN103789857 A CN 103789857A CN 201410013961 A CN201410013961 A CN 201410013961A CN 103789857 A CN103789857 A CN 103789857A
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Abstract
The invention provides a preparation method of collagen regenerated cellulose fiber. The preparation method comprises the following steps: preparing viscose spinning dope; adding collagen solution into the viscose spinning dope, wherein the adding quantity of the collagen accounts for 4-15% of the mass of the methylcellulose of the viscose spinning dope; evenly mixing to obtain protein viscose mixed liquid; adding an initiator into the mixed liquid, wherein the adding quantity of the initiator accounts for 2.3-5% of the mass of the collagen; after that, stirring at the temperature of 19-25 DEG C for 2-8h to obtain spinning solution; filtering and defoaming the spinning solution, and then carrying out wet spinning. After the preparation method is adopted, the collagen is successfully grafted into the regenerated cellulose fiber, and the collagen regenerated cellulose fiber can be spun; the grafting efficiency and the grafting rate of the method are high; the obtained collagen fiber has silk-like gloss and is fluffy and soft in hand feeling.
Description
Technical field
The invention belongs to textile fabric processing technique field, be specifically related to a kind of preparation method of collagen regenerated celulose fibre.
Background technology
Collagen is a kind of natural fibrin, is mainly present in the tissue such as skin, bone, tendon of animal, and be structural proteins important in connective tissue, play the function that supports organ, protection body.Collagen claims again collagen, and its molecular weight is 300,000 dalton, and it is formed by 2 I chains, 1 II chain combination, and then forms triple helix structure.These 3 peptide chains are mutually wound around and form right hand composite screw collagen with distinctive left-handed α chain, it is characterized in that amino acid presents chain Gly-x-y periodic structure.
There is the active forces such as the hydrophobic bond of ionic bond, hydrogen bond, Van der Waals force and non-polar group generation in collagen peptide interchain.Meanwhile, in tropocollagen molecule and intermolecularly also have 3 kinds of crosslinked actions, 3 peptide chains of collagen are coupled together securely, make collagen there is very high tensile strength.Between tropocollagen molecule, assemble and form the fibrillation very stable, toughness is very strong by " 1/4th stagger arrangement " mode supermolecule, fibrillation is further assembled formation collagenous fibres.In addition, molecule is interior and intermolecular covalent cross-linking is given collagen height physical and chemical stability and biological nature, as high-tensile strength, biodegradability, biocompatibility, low antigenicity, low irritant and low cytotoxicity, and the performance such as Promote cell's growth.
Diversity and the complexity of this 26S Proteasome Structure and Function feature of collagen, determined that it is in the good application prospect of field of textiles.In field of textiles, see the modification of collagen to silk fiber at present, to the modification of cotton fiber, blending and modifying with synthetic fiber, at present the excellent wearability of cellulose fibre has obtained the approval of textile industry and has had large-scale commercial application, therefore itself and collagen be combined with important Research Significance.But collagen combines with regenerated cellulose and to spin out collagen regenerated celulose fibre actually rare, trace it to its cause and be that collagen and the percent grafting of cellulose macromolecule chain and the influence factor of grafting efficiency are more, and more difficult control, the concentration of initator also has considerable influence to the content of celloglobulin.
Publication number is that the patent documentation that 102286803A, name are called " a kind of collagen/cellulose composite fiber and preparation method thereof " discloses a kind of collagen/cellulose composite fiber and preparation method thereof, first collagen solution is joined in cellulose viscose solution, mix with viscose solution; Obtain collagen/cellulose composite fiber through spinning.This invention is just by collagen solution and cellulose viscose solution co-blended spinning, and collagen cannot form bonding with covalent bond with cellulose fibre, spinning, weave with dyeing and finishing and add the loss that is easily subject to external influence man-hour and cause collagen.It is more that collagen and acrylonitrile carry out the conduct oneself patent of fraud originating party face of graft modification, but also rarely have report take regenerated celulose fibre as basic collagen graft modification patent.
Summary of the invention
The preparation method who the object of the invention is to overcome the deficiencies in the prior art and provide a kind of collagen regenerated celulose fibre.
A preparation method for collagen regenerated celulose fibre, comprises the steps:
Step 1, produces rayon spinning stoste;
Step 2, collagen solution is added in the rayon spinning stoste of step 1, collagen addition accounts for 4%～15% of the fine quality of rayon spinning liquid first, after mixing, obtain albumen viscose glue blending liquid, add again initator, initator addition accounts for 2.3%～5% of collagen quality, after then stirring 2～8 hours at 19 ℃～25 ℃ spinning solution;
Step 3, will carry out wet spinning after step 2 gained spinning solution filtration deaeration.
The mass ratio of collagen solution and rayon spinning liquid has directly affected percent grafting and grafting efficiency.Consider from the angle of chemical balance, increase the concentration of reactant, balance always moves right.The increase of collagenic protein solution proportion, the free radical of generation increases, and increases with the probability of cellulosic molecule collision contact, has promoted protein and cellulosic grafting, and therefore percent grafting and grafting efficiency all increase to some extent.But, excessive when the consumption of protein, cause that mixture system viscosity is less is unfavorable for spinning, thus can not fibroblast.
Temperature is comparatively complicated on the impact of percent grafting and grafting efficiency, and percent grafting and grafting efficiency are all that first the rising along with temperature is risen, and then decline again.This is because the rising of temperature increases the collision frequency between little molecule, has promoted graft reaction, percent grafting and grafting efficiency are all raise, but in the time of excess Temperature, depolymerization reaction is accelerated thereupon, and percent grafting and grafting efficiency decline on the contrary.In the time that temperature exceedes 48 ℃, there is gelatin phenomenon, do not possess spinning condition.
Free radical grafting reaction is along with the increase of time, and grafting efficiency improves very fast, but after reaction certain hour, increases not obviously, and this is to tend to balance gradually owing to reacting.And rayon spinning liquid at a certain temperature, place after certain hour, the performance of rayon spinning liquid can change, so when adding after initator, take into account the variation of viscose ripening degree, guarantee the synchronism of degree of ripeness and reaction speed, make spinning solution there is good spinnability, otherwise be easy to occur too " always " of spinning solution, and be unfavorable for spinning.
Under lower initiator ions concentration, most of initiator ions are adsorbed in initial reaction stage, and the free radical producing on cellulose molecular chain is less, add part initator free radical generation coupling termination, therefore percent grafting and grafting efficiency are all lower; Along with the increase of initiator ions concentration, after being reacted by cellulose absorption, leaving the free radical producing on the cellulose initiated strand of initiator ions of q.s increases, and percent grafting and grafting efficiency also increase thereupon; After initiator ions concentration exceedes finite concentration, because grafted chain increases, the diffusion velocity of protein declines, and adds that the stopped reaction of free radical on initiator ions and cellulose molecular chain increases, and percent grafting and grafting efficiency decline gradually.If it is very large just to have started initator addition, cause initial concentration higher, now spinning solution there will be gelation, be unfavorable for spinning, if addition is lower, cause insufficient, can cause the reduction of percent grafting and grafting efficiency, the increasing of the prolongation in reaction time and protein loss rate.
As foregoing invention further preferably, described collagenic protein concentration of polymer solution is 5%～25%.
As foregoing invention further preferably, described initator is persulfate-slaine or non-peroxide.
Redox initiation system mainly divides five classes: redox system and the non-peroxide systems of hydrogen peroxide system, persulfate system-slaine system, organic peroxide systems, multielectron transfer.Organic peroxide evocating agent is water-soluble poor, and rayon spinning liquid is water solution system, and compatibility is between the two poor; The redox system initiation temperature of multielectron transfer is higher, reaches 50 ℃ of left and right, and the temperature of rayon spinning liquid is generally 20 ℃ of left and right, and the too high meeting of temperature causes the gelation of spinning solution, cannot spinning; The efficiency of initiation of peroxisome series initiators and result reappearance are poor, therefore also inadvisable.
As foregoing invention further preferably, the persulfate in described persulfate-slaine is ammonium persulfate or potassium peroxydisulfate, slaine is the one in sulfurous acid iron, sodium hydrogensulfite or sodium sulfite; Described non-peroxide is ammonium ceric nitrate.
Compared with prior art, its remarkable advantage is in the present invention: the first, successfully collagen is grafted on regenerated celulose fibre, and spin out collagen regenerated celulose fibre, grafting efficiency and percent grafting are higher; The second, collagen fabric prepared by the method has the gloss as silk, and the fluffy softness of feel; The 3rd, the build-in attribute of reservation collagen, skin-friendly excellence, and human body skin is had to maintenance effect.In a most preferred embodiment of the present invention, percent grafting can reach 23.1%, and grafting efficiency can reach 50.8%.
The specific embodiment
Embodiment 1
A preparation method for collagen regenerated celulose fibre, comprises the steps:
The preparation of viscose solution: adopt the Cotton Pulp of the fine mass content 93.5% of the degree of polymerization 520, first, prepare spinning viscose solution through operations such as dipping, squeezing, pulverizing, experienced, yellow, dissolvings successively.Make the fine mass content 8.9% of viscose solution first, NaOH mass content 5.5%, viscosity (falling ball method) 50s, degree of ripeness (10%NH
4cl) 8.5mL.
Falling ball method: 2mm steel ball falls the required time of 20cm from described viscose solution.
The preparation of the graft copolymerization liquid of collagen liquid and rayon spinning liquid:
(1) preparation of the blended liquid of collagen liquid and rayon spinning liquid: the collagenic protein solution that is 20% by distilled water preparation mass concentration, this solution is added in above-mentioned rayon spinning liquid, wherein collagenic protein addition accounts for 8% of the fine quality of rayon spinning liquid first, mix, obtain albumen viscose glue blending liquid.
(2) blended liquid graft copolymerization: with distilled water compound concentration be 0.017mol/L ceric ammonium nitrate solution; This ceric ammonium nitrate solution is joined in the prepared blended liquid of step (1), fully stir, in ceric ammonium nitrate solution, ammonium ceric nitrate quality accounts for 3.5% of collagen quality, fully stirs graft copolymerization 8 hours at 19 ℃, the spinning solution after grafting is filtered to deaeration and send into spinning.
Wet spinning: the mixed solution of precrosslink protein and viscose glue is sent into wet spinning operation and carry out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 ℃, and plasticizing-bath temperature is 95 ℃.Coagulation bath composition is: sulfuric acid 90g/L, sodium sulphate 300 g/L, zinc sulfate 15 g/L.Post processing desulfurization adopts the sodium sulfite doctor solution of 70 ℃ of 30 g/L to carry out desulfurization.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.69dtex; Dry strong 2.24cN/ dtex; Wet strong 1.32cN/ dtex; Dryly stretch 17.6%.
Embodiment 2
The preparation of viscose solution: adopt the Cotton Pulp of the fine mass content 93.5% of the degree of polymerization 520, first, prepare spinning viscose solution through operations such as dipping, squeezing, pulverizing, experienced, yellow, dissolvings successively.Make the fine mass content 8.9% of first, NaOH mass content 5.4%, viscosity (falling ball method) 48s, degree of ripeness (10%NH4Cl) 8.3ml, is stand-by viscose solution.
Falling ball method: 2mm steel ball falls the required time of 20cm from described viscose solution.
The preparation of the graft copolymerization liquid of collagen liquid and rayon spinning liquid:
(1) preparation of the blended liquid of collagen liquid and rayon spinning liquid: the collagenic protein solution that is 25% by 5%NaOH solution preparation mass concentration, this solution is added in above-mentioned rayon spinning liquid, wherein collagenic protein addition accounts for 15% of the fine quality of rayon spinning liquid first, mix, obtain albumen viscose glue blending liquid.
(2) blended liquid graft copolymerization: with distilled water compound concentration be 0.025mol/L ammonium persulfate and solution of sodium bisulfite; This solution is joined in the prepared blended liquid of step (1), fully stir, in ammonium persulfate solution, ammonium persulfate quality accounts for 5% of collagen quality, fully stirs graft copolymerization 2 hours at 25 ℃, the spinning solution after grafting is filtered to deaeration and send into spinning.
Wet spinning: the mixed solution of precrosslink protein and viscose glue is sent into wet spinning operation and carry out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 ℃, and plasticizing-bath temperature is 95 ℃.Coagulation bath composition is: sulfuric acid 92g/L, sodium sulphate 305g/L, zinc sulfate 14g/L.Post processing desulfurization adopts the sodium sulfite doctor solution of 70 ℃ of 25 g/L to carry out desulfurization.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.58dtex; Dry strong 2.07cN/dtex; Wet strong 1.26cN/dtex; Dryly stretch 18.5%.
Embodiment 3
The preparation of viscose solution: adopt the Cotton Pulp of the fine mass content 93.5% of the degree of polymerization 520, first, prepare spinning viscose solution through operations such as dipping, squeezing, pulverizing, experienced, yellow, dissolvings successively.Make the fine mass content 8.9% of first, NaOH mass content 5.4%, viscosity (falling ball method) 48s, degree of ripeness (10%NH4Cl) 8.3ml, is stand-by viscose solution.
Falling ball method: 2mm steel ball falls the required time of 20cm from described viscose solution.
The preparation of the graft copolymerization liquid of collagen liquid and rayon spinning liquid:
(1) preparation of the blended liquid of collagen liquid and rayon spinning liquid: the collagenic protein solution that is 5% by 1%NaOH solution preparation mass concentration, this solution is added in above-mentioned rayon spinning liquid, wherein collagenic protein addition accounts for 4% of the fine quality of rayon spinning liquid first, mix, obtain albumen viscose glue blending liquid.
(2) blended liquid graft copolymerization: with distilled water compound concentration be 0.012mol/L ceric ammonium nitrate solution; This ceric ammonium nitrate solution is joined in the prepared blended liquid of step (1), fully stir, in ceric ammonium nitrate solution, ammonium ceric nitrate quality accounts for 2.3% of collagen quality, fully stirs graft copolymerization 6 hours at 20 ℃, the spinning solution after grafting is filtered to deaeration and send into spinning.
Wet spinning: the mixed solution of precrosslink protein and viscose glue is sent into wet spinning operation and carry out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 55 ℃, and plasticizing-bath temperature is 95 ℃.Coagulation bath composition is: sulfuric acid 88g/L, sodium sulphate 295g/L, zinc sulfate 12g/L.Post processing desulfurization adopts the sodium sulfite doctor solution of 70 ℃ of 25 g/L to carry out desulfurization.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.52dtex; Dry strong 2.32cN/dtex; Wet strong 1.28cN/dtex; Dryly stretch 16.8%.
Embodiment 4
The preparation of viscose solution: adopt the Cotton Pulp of the fine mass content 93.5% of the degree of polymerization 520, first, prepare spinning viscose solution through operations such as dipping, squeezing, pulverizing, experienced, yellow, dissolvings successively.Make the fine mass content 8.9% of first, NaOH mass content 5.4%, viscosity (falling ball method) 48s, degree of ripeness (10%NH4Cl) 8.3ml, is stand-by viscose solution.
Falling ball method: 2mm steel ball falls the required time of 20cm from described viscose solution.
The preparation of the graft copolymerization liquid of collagen liquid and rayon spinning liquid:
(1) preparation of the blended liquid of collagen liquid and rayon spinning liquid: the collagenic protein solution that is 5% by 1%NaOH solution preparation mass concentration, this solution is added in above-mentioned rayon spinning liquid, wherein collagenic protein addition accounts for 4% of the fine quality of rayon spinning liquid first, mix, obtain albumen viscose glue blending liquid.
(2) blended liquid graft copolymerization: with distilled water compound concentration be 0.012mol/L potassium peroxydisulfate and solution of sodium bisulfite; This solution is joined in the prepared blended liquid of step (1), fully stir, in potassium persulfate solution, potassium peroxydisulfate quality accounts for 5% of collagen quality, fully stirs graft copolymerization 2 hours at 25 ℃, the spinning solution after grafting is filtered to deaeration and send into spinning.
Wet spinning: the mixed solution of precrosslink protein and viscose glue is sent into wet spinning operation and carry out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 55 ℃, and plasticizing-bath temperature is 95 ℃.Coagulation bath composition is: sulfuric acid 88g/L, sodium sulphate 302g/L, zinc sulfate 15g/L.Post processing desulfurization adopts the sodium sulfite doctor solution of 70 ℃ of 28g/L to carry out desulfurization.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.63dtex; Dry strong 2.18cN/dtex; Wet strong 1.22cN/dtex; Dryly stretch 17.6%.
The method of testing of percent grafting and grafting efficiency:
In measuring cup or small beaker, take the graft copolymerization liquid of about 1-1.5g collagen liquid and rayon spinning liquid, be placed in 10 × 10 centimetres of clean glass sheet, the sheet glass measure-alike with another piece weighs wounded, makes viscose glue be pressed into a film, evenly low being distributed on sheet glass.Then make two blocks of sheet glass pull open in the opposite direction, be immersed in 45-47 ℃ of solidification liquid and (as muddiness, after clarification, use), make viscose glue be frozen into a film.This film is fully washed with hot water, and desulfurization 5-10 min in the sodium sulfite doctor solution (25-30 g/L) that is placed on 70 ℃, makes film transparent.Finally use distilled water washes clean, at 105 ℃, dry, and cooling in drier, weigh.Whether to reach constant weight in order checking, then to dry half an hour in baking oven, as front cooling, weigh, weigh for twice and be more or less the same in 0.5 ㎎.
The percent grafting of protein is the mass percent that is grafted to protein on cellulose and accounts for cellulose matrix, is calculated as follows:
Percent grafting %=(m
1-m
c)/m
c× 100%
M
1for the quality of cellulose sample after grafting, m
cfor the quality of cellulose sample before grafting.
The grafting efficiency of protein is the mass percent that the protein of participation graft reaction consumption accounts for the protein in the front system of grafting, is calculated as follows: grafting efficiency %=(m
1-m
c)/m
p× 100%, m
pfor the amount of the protein that adds.
The percent grafting of collagenic protein and grafting efficiency under table 1 different condition
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Percent grafting % | 23.1 | 19.8 | 25.3 | 16.1 |
| Grafting efficiency % | 50.8 | 25.5 | 46.2 | 29.2 |
Claims (4)
1. a preparation method for collagen regenerated celulose fibre, is characterized in that, comprises the steps:
Step 1, produces rayon spinning stoste;
Step 2, collagen solution is added in the rayon spinning stoste of step 1, collagen addition accounts for 4%～15% of the fine quality of rayon spinning liquid first, after mixing, obtain albumen viscose glue blending liquid, add again initator, initator addition accounts for 2.3%～5% of collagen quality, after then stirring 2～8 hours at 19 ℃～25 ℃ spinning solution;
Step 3, will carry out wet spinning after step 2 gained spinning solution filtration deaeration.
2. the preparation method of collagen regenerated celulose fibre according to claim 1, is characterized in that: described collagenic protein concentration of polymer solution is 5%～25%.
3. the preparation method of collagen regenerated celulose fibre according to claim 1, is characterized in that: described initator is persulfate-slaine or non-peroxide.
4. the preparation method of collagen regenerated celulose fibre according to claim 3, it is characterized in that: the persulfate in described persulfate-slaine is ammonium persulfate or potassium peroxydisulfate, slaine is the one in sulfurous acid iron, sodium hydrogensulfite or sodium sulfite; Described non-peroxide is ammonium ceric nitrate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106139232A (en) * | 2016-07-29 | 2016-11-23 | 江苏蓝湾生物科技有限公司 | A kind of preparation method of collagen protein regenerated cellulose combine dressing |
| TWI683043B (en) * | 2018-11-16 | 2020-01-21 | 達紡企業股份有限公司 | Silk collagen fiber, fabric and producing method thereof |
| CN111485420A (en) * | 2020-04-23 | 2020-08-04 | 罗莱生活科技股份有限公司 | Skin care fiber with semi-interpenetrating network structure and preparation method and application thereof |
| CN112877880A (en) * | 2021-01-11 | 2021-06-01 | 浙江大能纺织印染有限公司 | Preparation method of fragrant antibacterial collagen fiber cotton blended dyed knitted fabric |
| CN116005361A (en) * | 2022-12-29 | 2023-04-25 | 东莞盛翔新材料技术有限公司 | Preparation method of cellulose-collagen composite nanofiber membrane |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN111485420A (en) * | 2020-04-23 | 2020-08-04 | 罗莱生活科技股份有限公司 | Skin care fiber with semi-interpenetrating network structure and preparation method and application thereof |
| CN112877880A (en) * | 2021-01-11 | 2021-06-01 | 浙江大能纺织印染有限公司 | Preparation method of fragrant antibacterial collagen fiber cotton blended dyed knitted fabric |
| CN116005361A (en) * | 2022-12-29 | 2023-04-25 | 东莞盛翔新材料技术有限公司 | Preparation method of cellulose-collagen composite nanofiber membrane |
| CN116005361B (en) * | 2022-12-29 | 2023-07-21 | 东莞盛翔新材料技术有限公司 | Preparation method of cellulose-collagen composite nanofiber membrane |
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