CN105369389B - Collagen fiber and its production process - Google Patents

Collagen fiber and its production process Download PDF

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CN105369389B
CN105369389B CN201510431030.2A CN201510431030A CN105369389B CN 105369389 B CN105369389 B CN 105369389B CN 201510431030 A CN201510431030 A CN 201510431030A CN 105369389 B CN105369389 B CN 105369389B
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collagen
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weight
fabric
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CN105369389A (en
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黄森元
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Zeng Yisong
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Abstract

A collagen fiber and its preparation method are provided. The process of the collagen fiber comprises: step A: a fiber raw material solution containing a fiber raw material is prepared. And B: a collagen solution containing collagen is prepared. The collagen is 5-10 parts by weight based on 100 parts by weight of the fiber raw material. And C: mixing the fiber raw material solution and the collagen solution to form a spinning solution, and preparing the spinning solution into collagen fibers by a wet spinning method. The process has the advantage of difficult yarn breakage during spinning into fibers, and the collagen fibers with good deodorization function and skin moisturizing function can be manufactured by using a small amount of collagen.

Description

The processing procedure of collagen fabric and collagen fabric obtained
Technical field
The present invention relates to a kind of fiber, the processing procedure and collagen obtained more particularly to a kind of collagen fabric are fine Dimension.
Background technology
There are many different functional fibers, with the difference of functional kinds of fibers, different functional fibers on the market Can have the function of that such as moisture absorption, warming, antibacterial and deodorizing etc. are different, wherein, collagen fabric has good smelly eliminating work( Energy and moisture-retention function of skin, and collagen is the ingredient originally having in human body, thus skin-friendly is good.Since collagen fabric has There is the advantages of aforementioned, so how to provide a kind of can produce the processing procedure of collagen fabric, and make the collagen produced Fiber have good deodorizing function and moisture-retention function of skin, be one be worth solve the problems, such as.
Invention content
The first object of the present invention is to provide a kind of processing procedure of collagen fabric, can be in spinning smoothly Collagen fabric is produced, and obtained collagen fabric has good deodorizing function and moisture-retention function of skin.
The processing procedure of collagen fabric of the present invention includes step A:It is molten to prepare a fibrous raw material for including fibrous raw material Liquid, step B:Prepare a collagen solution for including collagen, in step B, with the fiber of 100 parts by weight On the basis of raw material, which is 5~10 parts by weight, and the processing procedure of the collagen fabric also includes one after step B Step C, in step C, mixing the fibrous raw material solution and the collagen solution becomes a kind of spinning solution, and with wet type Collagen fabric is made in the spinning solution by spin processes.
The processing procedure of collagen fabric of the present invention, in step B, the weight of the collagen accounts for the collagen egg The 25%~35% of white solution gross weight.
The processing procedure of collagen fabric of the present invention, molecular weight are point of the collagen of 655~1791dalton Son accounts for whole collagen ratio more than 50%.
The processing procedure of collagen fabric of the present invention, the average molecular weight of the collagen is 1000dalton.
The processing procedure of collagen fabric of the present invention, the fibrous raw material of the fibrous raw material solution for regenerated cellulose or Acryl.
The second object of the present invention is to provide a kind of collagen fabric have good deodorizing function and skin moisture-keeping Function.
Collagen fabric of the present invention, the collagen fabric are that manner described above is made.
Fibrous raw material of the present invention can be the regenerated cellulose for rayon (rayon) to be made, and also can be for making Make acryl (acryl) material of staple fibre.Meeting natural, environmentally friendly demand, the fibrous raw material is preferably using regeneration Cellulose.Collagen fabric as that must prepare long fine kenel, which is preferably acryl material.Prepare the fiber The method of material solution is for example first to collect suitable natural cellulose with regenerated cellulose, and the cellulose Can for paper products, timber, linen-cotton or above-mentioned material the natural material from the Nature such as any combination, then by the cellulose It is dissolved in a solvent, stirs at room temperature, the cellulose solution that fibrous raw material is regenerated cellulose can be made.The solvent Can be sodium hydroxide solution, N-methylmorpholine-N- oxides (N-methylmorpholineN-oxide, NMMO), tertiary amine oxygen Compound, cyclic annular amine oxide, ethyl alcohol, carbon disulfide, dimethylformamide, diformazan sulfurous or above-mentioned material any combination. On implementing other than voluntarily preparing the fibrous raw material solution, it can also come in fact in buying ready-made fibrous raw material solution finished product on the market Apply the present invention.
The source of collagen of the present invention need not be particularly limited to, as being made with animal materials such as ox and pigs.Compared with Goodly, in order to avoid the propagation of the common disease of people and animals, which can be made with fish of raw material.More preferably, using fish scale as original The collagen of no fish stink can be more made in material.The method for preparing the collagen solution washes with water collected first Fish scale, to wash away the impurity of such as silt etc..Then clean the fish scale with acid solution again, with remove nonprotein other into Part, and obtain transparent flap.The flap is poured into the water-bath added with ferment, by the fish scale after heating stirring Yellowish lysate is made in piece hydrolysis.After obtaining the lysate, the activity to destroy ferment is heated, and add in active carbon adsorption Impurity and removal agent of raw meat smell deodorization, later filtering can obtain the transparent liquid of limpid and similary micro- Huang.Again on demand with ion exchange resin Filtering absorption heavy metal or concentration, can be made the collagen solution.
When implementing the present invention, the concentration of the collagen solution should limit.When concentration is too high, caking gelation is had The problem of not easy to be processed, and when the concentration is too low, after being mixed with the fibrous raw material solution, it can cause the concentration of the collagen It crosses dilute, the collagen can not be made fully to be combined with the fibrous raw material.It is thus preferable to the weight of the collagen is to account for this The 25%~35% of the gross weight of collagen solution.More preferably, the weight of the collagen is account for the collagen solution total The 35% of weight.In addition, using the gross weight of the fibrous raw material contained by fibrous raw material solution prepared in step A as 100 parts by weight, Collagen contained by the collagen solution is preferably 5~10 parts by weight.When the weight of the collagen exceeds in 10 weights When measuring part, the effect that the collagen that more adds can increase is not obvious, and in step C, can reduce spinnability, also It is to say that higher wire broken rate can be generated in spinning process.When collagen is when weighing less than 5 parts by weight, obtained collagen The functionals such as the smelly eliminating of azelon and moisturizing can be bad, therefore the parts by weight of the collagen are preferably 5~10 parts by weight, more Good ground can be 10 parts by weight.
In step C, when mixing the fibrous raw material solution with the collagen solution, it should be noted that the collagen solution The distribution of the molecular size range and molecular weight of contained collagen.Since collagen is one kind for belonging to high molecular material, And since the molecular weight of high molecular material has no centainly, and the physics of molecular weight effects material and engineering properties are very big, therefore the glue The molecular weight of former albumen should limit.When the average molecular weight of the collagen is too big, then collagen is not easy and fibrous raw material Uniformly mixing can make the poor quality of collagen fabric finished product obtained, if the average molecular weight of the collagen is too small, It represents collagen and is almost cracked into Amino acid, collagen possessed functional in itself can be lost.In addition, if collagen The molecular weight distribution of albumen is excessively wide, as intermolecular otherness is excessive so that and the interregional otherness of finished product is big, and Therefore cause that the finished product easy stress in stress is uneven and damages.Therefore preferably, molecular weight is 655~1791dalton's The molecule of collagen accounts for the ratio of whole collagen more than 50%, and the average molecular weight of the collagen is 1000dalton。
It is to pour into the spinning solution in spinning tank in step C, and passes through spinning-drawing machine and spun with wet-spinning, then put Enter one containing sulfuric acid, sodium sulphate and zinc sulfate solidification liquid in, solidified forming collagen fabric and obtain finished product.
The beneficial effects of the present invention are:By controlling the ratio of the fibrous raw material and the collagen, can take into account In the case of spinnability, the collagen fabric with good deodorizing function and moisture-retention function of skin is made.
Description of the drawings
Nothing.
Specific embodiment
The embodiment 1 of the processing procedure of collagen fabric of the present invention and collagen fabric obtained, comprising:
Step A:Prepare the fibrous raw material solution for including fibrous raw material.It is first collected for example during making:Paper products, linen-cotton etc. Fiber base material containing cellulose, and the base material and sodium hydrate aqueous solution are acted on forming alkalinized celluloses.The hydrogen The concentration of aqueous solution of sodium oxide, preferably 5~20 weight %.More preferably, the present embodiment is with the sodium hydroxide of 18 weight % Solution is handled.Obtain it is experienced after after (matured) and weight percent account for about 30~40% alkalinized celluloses, add Carbon disulfide reacts, and is dissolved with the sodium hydrate aqueous solution of 5 weight %, after filtering and deaeration, and fibrous raw material, which can be made, is The fibrous raw material solution of regenerated cellulose.On the implementation, the fibrous raw material solution also can be purchased from existing products on the market, The step of equally also completing to prepare the fibrous raw material solution.
Step B:Prepare the collagen solution of an including collagen.Anoplura fish scale, and high pressure washing institute are collected first Anoplura fish scale is stated to wash away impurity.The Anoplura fish scale of 5000g is taken, and adds in 0.6 centinormal 1 15 liters of stirrings of aqueous hydrochloric acid solution After one day, 0.3 centinormal 1 15 liters of aqueous hydrochloric acid solution is put into coarse net filtering Anoplura squama again, stirs 10 minutes and filters.Then It pickling 1 time and washes 6 times again, the Anoplura fish scale of the common 3800g of weight in wet base can be obtained.The Anoplura fish scale is put into 10 liters of reaction In pot, then add after the water of 5000g when being heated up to 50 DEG C, add in the ferment of 4g, the pH value of solution is about 3.2 at this time.Continuous heating After three hours, fish scale meeting almost all is dissolved, and the pH value of solution increases to 4.0 or so.Removal agent of raw meat smell, the 20g of 40g is added in later Activated carbon, and increase temperature up to 90 DEG C maintain 40 minutes after be filtered to get limpid yellowish transparent liquid.It will be transparent Liquid is cooled to 40 DEG C hereinafter, the transparent liquid is made to flow through anion-cation exchange resin, after removing heavy metal, can obtain about 8000 milliliters Unconcentrated collagen solution.Using vacuum decker, the content which is concentrated into collagen accounts for always The 35% of weight, that is to say, that collagen nearly weighs 1155g, and water nearly weighs 2145g, which always weighs about 3300g.
Collagen solution made from method described above, the average molecular weight of collagen is 1000, and molecular weight is The molecule of the collagen of 655~1791dalton accounts for whole collagen ratio more than 50%, the molecule of the collagen Distribution record is measured in table 1.
Table 1
When taking collagen solution made from this step, it should be noted that with the weight of the fibrous raw material of the fibrous raw material solution It measures as 100 parts by weight, which is 5 parts by weight.For example, as the usage amount of the fibrous raw material solution be 100g when, According to the fibrous raw material that should contain about 21g for the ratio of step A.Therefore, the collagen content of the collagen solution should be 1.05g, that is to say, that the usage amount of the collagen solution is 3g.
Step C:Mixing the fibrous raw material solution and the collagen solution becomes a spinning solution, and the spinning solution is wet by one Formula spinning-drawing machine is spun with the speed of 60m/min, and the solidified forming in a solidification liquid, after forming again after washing oils etc. Processing can obtain collagen fabric.Every liter of the solidification liquid contains 120 grams of 98% concentrated sulfuric acid, 280 grams of sodium sulphate And 15 grams of zinc sulfate, and pH value is between 2~3.The fiber bodies of obtained collagen fabric can contain regenerated cellulose The fibrous raw material and the collagen.The smelly eliminating ability of collagen fabric obtained by last re-test the present embodiment and Skin moisture-keeping sexuality, and result is reported in Table 2 below.
The embodiment 2 of the processing procedure of collagen fabric of the present invention and collagen fabric obtained is similar with the embodiment 1, Different places are:The usage amount of the collagen is increased into 10 parts by weight.Glue obtained by similary test the present embodiment The smelly eliminating ability of former azelon and skin moisture-keeping sexuality, and result is reported in Table 2 below.
The comparative example 1 of the processing procedure of collagen fabric of the present invention and collagen fabric obtained is similar with the embodiment 1, Different places is in step B, using the weight of the fibrous raw material of the fibrous raw material solution as 100 parts by weight, the collagen The weight of albumen is 1 parts by weight.The smelly eliminating ability and skin moisture-keeping of collagen fabric obtained by similary test the present embodiment Sexuality, and result is reported in Table 2 below.
The comparative example 2 of the processing procedure of collagen fabric of the present invention and collagen fabric obtained is similar with the embodiment 1, Different places is in step B, using the weight of the fibrous raw material of the fibrous raw material solution as 100 parts by weight, the collagen The weight of albumen is 11 parts by weight.Though due to this comparative example still can spinned fiber because wire broken rate is high, do not meet economic effect Rate, therefore omit the test of smelly eliminating ability and skin moisture-keeping sexuality.
The comparative example 3 of the processing procedure of collagen fabric of the present invention and collagen fabric obtained is similar with the embodiment 1, Different places is in step B, using the weight of the fibrous raw material of the fibrous raw material solution as 100 parts by weight, the collagen The parts by weight of albumen are 15 parts by weight.Since this comparative example is not easy spinned fiber, therefore smelly eliminating ability and skin guarantor can not be carried out The test of moist ability.
Table 2
(1) smelly eliminating is tested:It is tested using equipment analysis detection tube method and equipment analysis GC methods.
(2) skin moisture-keeping test condition is as follows:Environment temperature is 20 ± 1 DEG C, and ambient humidity is 65 ± 4%, test pair It is 30 minutes during covering the test of sample as being 10 minutes during for 30 years old women, not covering the adaptation of sample, measurement sites For forearm, posture is sitting posture during measurement, and measuring instrument is Evaporimeter EP2, and moisturizing benchmark is pure cotton material.
(3) above-mentioned test is that collagen fabric is made knitted fabric to test, and the composition of knitted fabric is 50% Collagen fabric, 48% cotton and 2% spandex.
(4) the spinnability evaluation criterion described in is as follows:" excellent " represents in spinning process in 3 hours not fracture of wire, " good " generation Fracture of wire 1~2 time in 3 hours in table spinning process, "available" represents in spinning process fracture of wire in 3 hours, and, more than 5 times, " poor " represent is spun It is not easy to form silk during silk, that is to say, that silk intensity difference.
Before embodiment described in comparison and the comparative example is started, first to illustrate, due to most in industrial implementation Using 5 parts by weight as exploiting entity, therefore 2 parts by weight are omitted to the comparative example between 4 parts by weight and 6 parts by weight between 9 parts by weight Comparative example.The difference of implementation result of the present invention is not only involved additionally, due to spinnability, more involves whether the present invention is able to reality The emphasis applied, therefore in this specification between 10 to 15 parts by weight, also in addition test the comparative example 2 of 11 parts by weight.
It is learnt by the embodiment 1 and the experimental result of the comparative example 1, which removes for acetic acid and valeric acid (lucky grass Acid) smelly eliminating ability be substantially better than outside the comparative example 1, skin moisture-keeping is also significantly promoted to 16% by 2%.By the implementation Example 2 and the experimental result of the comparative example 2 and the comparative example 3 are learnt, although the embodiment 2 meeting fracture of wire, wire broken rate Shang Neng hold Perhaps range, but the wire broken rate of the comparative example 2 is excessive, and which is then almost difficult to that fiber is made.In addition, observe the embodiment 1st, the embodiment 2 and the comparative example 3, we can have found, when collagen is increased to 5 parts by weight by 1 parts by weight, skin is protected Moist effect rises to 8 times, and when the collagen is increased to 10 parts by weight by 5 parts by weight, skin moisture-keeping effect is to carry A height of 1.25 times, therefore we can know that, when the weight of collagen is more than 10 parts by weight, the production cost of input with into The increased functional of product will be disproportionate, does not have economic benefit.
On the implementation, which can also replace with the fibrous raw material solution using acryl as fibrous raw material, and The collagen fabric of the present invention is mixed and is made with the collagen solution.Due to the fibrous raw material solution of acryl fiber It is all conventional art to prepare and how to be spun into fiber, therefore is no longer illustrated.As long as control the weight of the collagen solution Part and concentration are in the range of as previously described.
In conclusion the processing procedure of collagen fabric of the present invention, by the parts by weight and the fiber that control the collagen The ratio of the parts by weight of raw material so that while this processing procedure takes into account preferable spinning rate, can produce with good deodorizing function And the collagen fabric of moisture-retention function of skin, therefore the purpose of the present invention can be reached really.

Claims (5)

1. a kind of processing procedure of collagen fabric, includes step A:Prepare the fibrous raw material solution for including fibrous raw material, Step B:Prepare a collagen solution for including collagen;It is characterized in that:The collagen be using flap as Raw material, and fish scale is poured into the water added with ferment, the flap is dissolved into a lysate after heating stirring, then lead to After crossing heating destruction yeast activity, after adding in activated carbon adsorption dye matter and removal agent of raw meat smell deodorization, the saturating of limpid and micro- Huang is obtained by filtration Bright liquid, then the object with ion exchange resin absorption heavy metal gained, while the collagen that molecular weight is 655~1791dalton Molecule accounts for whole collagen ratio more than 50%,
In step B, on the basis of the fibrous raw material of 100 parts by weight, which is 5~10 parts by weight, should Comprising the step C after step B one, in step C, it is molten also to mix the fibrous raw material for the processing procedure of collagen fabric Liquid and the collagen solution become a kind of spinning solution, and the spinning solution is made collagen fabric with wet-spinning.
2. the processing procedure of the collagen fabric as described in claim 1, it is characterised in that:In step B, the collagen Weight account for the 25%~35% of the collagen solution gross weight.
3. the processing procedure of the collagen fabric as described in claim 2, it is characterised in that:The average molecular weight of the collagen For 1000dalton.
4. the processing procedure of the collagen fabric as described in claim 1, it is characterised in that:The fiber of the fibrous raw material solution is former Expect for regenerated cellulose or acryl.
5. a kind of collagen fabric, it is characterised in that:The collagen fabric is with right any in claim 1 to 4 It is required that the processing procedure is made.
CN201510431030.2A 2014-08-07 2015-07-22 Collagen fiber and its production process Active CN105369389B (en)

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TW103127053A TWI565483B (en) 2014-08-07 2014-08-07 The preparation of collagen fibers and the collagen fibers obtained

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108096054A (en) * 2017-12-08 2018-06-01 厦门医学院 The purposes of milkfish fish scale collagen
CN110878439A (en) * 2018-09-05 2020-03-13 东莞盛翔新材料技术有限公司 Fulispun silk collagen peptide titanium amino acid fiber cloth
CN115323517A (en) * 2022-09-01 2022-11-11 广州迈菲科技有限公司 Preparation method of collagen fiber, collagen fiber and application
CN115748249B (en) * 2022-11-23 2024-06-25 浙江诸暨聚源生物技术有限公司 Recombinant collagen hydrogel fiber and preparation method thereof

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CN101215733A (en) * 2008-01-14 2008-07-09 四川大学 Collagen-base PEG composite fibre and spinning technique thereof
CN101597817A (en) * 2008-07-01 2009-12-09 河南瑞贝卡发制品股份有限公司 A kind of preparation method of collagen fiber for artificial hair
CN101660215A (en) * 2009-09-23 2010-03-03 陈福库 Protein and cellulose composite fiber and manufacturing method thereof
CN102181959A (en) * 2011-04-07 2011-09-14 北京服装学院 Fish collagen composite fibers and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101008110A (en) * 2007-01-12 2007-08-01 四川大学 Method for preparing collagen/ polyvinyl alcohol composite fiber using dialdehyde as cross-linking agent
CN101215733A (en) * 2008-01-14 2008-07-09 四川大学 Collagen-base PEG composite fibre and spinning technique thereof
CN101597817A (en) * 2008-07-01 2009-12-09 河南瑞贝卡发制品股份有限公司 A kind of preparation method of collagen fiber for artificial hair
CN101660215A (en) * 2009-09-23 2010-03-03 陈福库 Protein and cellulose composite fiber and manufacturing method thereof
CN102181959A (en) * 2011-04-07 2011-09-14 北京服装学院 Fish collagen composite fibers and preparation method thereof

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