CN107287697A - A kind of preparation method of chitin fiber - Google Patents
A kind of preparation method of chitin fiber Download PDFInfo
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- CN107287697A CN107287697A CN201710510660.8A CN201710510660A CN107287697A CN 107287697 A CN107287697 A CN 107287697A CN 201710510660 A CN201710510660 A CN 201710510660A CN 107287697 A CN107287697 A CN 107287697A
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- chitin fiber
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- spinning
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/06—Feeding liquid to the spinning head
- D01D1/09—Control of pressure, temperature or feeding rate
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
Abstract
The invention discloses a kind of preparation method of chitin fiber, belong to functional fiber preparing technical field.The present invention, which first mixes middle deacetylation chitosan with oxalic acid solution, is swelled rear heating stirring dissolving, again through sieving, vacuum defoamation, spinning solution is made, spinning solution is then delivered to spinning cap with measuring pump and extruded, after being solidified through coagulating bath, obtain as-spun fibre, again by after gained as-spun fibre drawn, then it is scrubbed, obtain shaping fiber, baked, dry again, cut-out, produces chitin fiber.Gained chitin fiber of the invention, with moisture evaporation after the decomposition of additive impurity, will not be impacted, the raising of product purity in preparation process to product purity, and when product is used for curable product, the performance such as bacteriostasis rate is effectively lifted.
Description
Technical field
The invention discloses a kind of preparation method of chitin fiber, belong to functional fiber preparing technical field.
Background technology
Chitosan, also known as chitosan, are a kind of linear polymerics, with fibre forming property, can spinnability.Chitin fiber is exactly
It is made using the good ropiness energy of crust solution, is a kind of functional fiber.Chitin fiber has broad-spectrum antiseptic, resisted
Bacterium efficiency high and it is nontoxic the advantages of；There is the ability of biodegradability, bioactivity and adsorbing metal ions again simultaneously.Therefore
It can be applied to the fields such as medical textile, health clothing and industry.
Chitin fiber is generally prepared using wet spinning at present.The process route of spinning is generally：Chitosan-dissolving-
Spinning solution-filtering-deaeration-metering-filtering-spinning-coagulating bath-stretch bath-washing-drying-fiber.By years of researches
And development, the production of chitin fiber has been made significant headway, but still there are problems that, there is to be solved.
1. the purity of chitin fiber is low.Spinning solution is formd in coagulating bath to be existed in as-spun fibre, as-spun fibre
Solvent and coagulator, most of solvent can be removed in the stretch bath and washing bath below, but still have a little dissolvent residual
In the fibre, and in order to improve in the dissolubility and fibre forming property of chitosan, spinning process usually using some chemical assistants, this
A little auxiliary agents are difficult to be completely removed in the later process of spinning.The presence of solvent, coagulator and auxiliary agent in fiber not only makes
The cost of chitin fiber is improved, and reduces the purity of chitin fiber, limits chitin fiber absorbable in human body
The medical field such as suture and artificial kidney film is widely used；
2. the spinning property of chitin fiber is poor.Current scientific research institution both domestic and external, institution of higher learning and some enterprises are raising shell
The spinnability of glycan fiber has done substantial amounts of research.Research shows, by the spinning technique of the well chitin fiber, to chitosan
Fiber, which is modified the methods such as processing, can improve the spinning properties such as the intensity of chitin fiber, but chitin fiber spinnability still
It is so very poor.Chitin fiber is partially thick there are still low strength, line density, and easy adhesion, is also easy to produce short in spinning between fiber
The defects such as suede.To overcome these defects, chitin fiber can be with viscose rayon, terylene, polypropylene filament yarn, viscose filament yarn and spun silk etc.
Fiber blend, can also make non-woven fabrics, but pure spinning chitin fiber still has certain difficulty.
Therefore, on the premise of auxiliary agent or unreal used additives are reduced, the purity of chitin fiber how is further improved
And performance, strengthen the spinnability of chitin fiber, will be researcher and the producer's urgent problem to be solved of chitin fiber.
The content of the invention
The present invention solves the technical problem of：For conventional wet spinning technique prepare chitin fiber use compared with
Many auxiliary agents, it is adjuvant used to remain in chitin fiber, cause product purity not high, there is provided one for the problem of influenceing its performance
Plant the preparation method of chitin fiber.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）It is 1 in mass ratio：20~1：30, chitosan and oxalic acid solution are poured into after mixer, 20~40min of stirring mixing,
Standing is swelled 6~8h, is stirred under heating after dissolving, sieving, vacuum defoamation, obtains spinning solution；
（2）Above-mentioned gained spinning solution is delivered into spinning cap with measuring pump to be extruded, after solidifying through coagulating bath, must come into being fibre
Dimension；
（3）After above-mentioned gained as-spun fibre drawn, then it is scrubbed, shaping fiber, then baked, dry, cut-out are obtained, is produced
Chitin fiber.
Step（1）Described chitosan is deacetylation chitosan in 70~85%.
Step（1）Described oxalic acid solution is the oxalic acid solution that mass fraction is 4~6%.
Step（1）Described heating stirring dissolution conditions are：It it is 45~55 DEG C in temperature, rotating speed is 300~500r/min
Under the conditions of, 3~5h of constant temperature stirring and dissolving.
Step（2）Described measuring pump transfer rate is 10~15kg/min.
Step（2）Described filature cap hole footpath is 0.06~0.08mm, and hole density is 800~1000 holes/cm2, hole count is
15~200,000 holes.
Step（2）Described coagulating bath is that to be preheated to 35~40 DEG C of mass fraction be 4~8% ammoniacal liquor.
Step（3）The draw ratio is 2~3 times.
Step（3）Described drying is the pneumatic conveying drying under the conditions of 25~35 DEG C or vacuum is cold under the conditions of -65~-60 DEG C
It is lyophilized it is dry in one kind.
Step（3）Described baking conditions are：90~92 DEG C of stoving temperature, bakee to shaping fiber moisture content be 20~
30%。
The beneficial effects of the invention are as follows：
（1）Deacetylation chitosan during technical solution of the present invention considered critical first uses 70~85%, because chitosan is
Efficient chelating media, the adsorption capacity size of chitosan depends on its deacetylation, and deacetylation is bigger, then adsorption capacity is got over
By force, using relatively low deacetylation chitosan, the chitosan adsorbing contaminant in preparation process can be avoided, so as to influence product
Purity, but not deacetylation is more low better, if using lower low deacetylation chitosan, dissolution of raw material degree is further
Decline, chitosan will be caused not to be dissolved in oxalic acid solution, be unfavorable for the preparation of spinning solution, and deacetylation shell gathers in using
Sugar is effectively reduced the absorption to impurity again under conditions of solubility is ensured, improves product purity；
（2）Technical solution of the present invention uses ammoniacal liquor for coagulating bath, because chitosan under alkaline environment solubility reduce, and ammoniacal liquor with
Oxalic acid solution system can slow down solidification rate, be conducive to chitin fiber curing molding, form the as-spun fibre of circular cross-section, and
Ammonia molecule has stronger permeability in ammoniacal liquor, is conducive to making Rotating fields inside and outside fiber to reach unanimity, in addition, being bakeed in the later stage
During, oxalic acid is produced carbon dioxide and water by thermal decomposition, and ammonia and moisture evaporation, will not make to product purity after ammoniacal liquor is heated
Into influence.
Embodiment
It is 1 in mass ratio first：20~1：30, it is that 4~6% oxalic acid solutions pour into mixer by chitosan and mass fraction,
In under room temperature condition, after 200~400r/min rotating speeds stirring mixing, 20~40min, standing is swelled 6~8h, is subsequently heated liter
Temperature is to 45~55 DEG C, and regulation speed of agitator is to 300~500r/min, and constant temperature 3~5h of stirring and dissolving is stainless after 325~500 mesh
Steel is sieved, and obtains chitosan solution, and by gained chitosan solution under the conditions of vacuum is 92~96%, dynamic 2~4h of deaeration is obtained
Spinning solution；Using wet spinning, gained spinning solution is delivered to spinning-drawing machine spinning by measuring pump with 10~15kg/min speed
Cap is extruded, and is solidified after extrusion through being preheated to 35~40 DEG C of mass fraction for 4~8% ammoniacal liquor, is stretched in solidification,
Drawing multiple is 2~3 times, after end to be tensioned, under the conditions of supersonic frequency is 40~45kHz, is successively 40~55 with temperature
DEG C warm water washs 3~5min, and absolute ethyl alcohol washs 2~4min, and deionized water washs 2~5min, obtains shaping fiber；Again by gained
Shaping fiber is evenly laid out in stainless steel pallet, and tiling thickness is 1~3mm, under the conditions of temperature is 90~92 DEG C, bakees extremely
Shaping fiber moisture content is 20~30%, obtains baking and forming fiber, then by after gained baking and forming fiber drying, cut-out produces shell
Glycan fiber.Described chitosan is deacetylation chitosan in 70~85%.Described filature cap hole footpath be 0.06~
0.08mm, hole density is 800~1000 holes/cm2, hole count is 15~200,000 holes.Described drying is under the conditions of 25~35 DEG C
Pneumatic conveying drying or one kind in vacuum freeze drying under the conditions of -65~-60 DEG C.
Example 1
It is 1 in mass ratio first：30, it is that 6% oxalic acid solution pours into mixer by chitosan and mass fraction, under room temperature condition,
After 400r/min rotating speeds stirring mixing 40min, standing is swelled 8h, is subsequently heated and is warming up to 55 DEG C, regulation speed of agitator to
500r/min, constant temperature stirring and dissolving 5h, after 500 mesh stainless steels sieve, obtain chitosan solution, and by gained chitosan solution in true
Reciprocal of duty cycle be 96% under the conditions of, dynamic deaeration 4h obtains spinning solution；Using wet spinning, by gained spinning solution by measuring pump with
15kg/min speed is delivered to spinning-drawing machine spinning cap and extruded, solidifying for 8% ammoniacal liquor through being preheated to 40 DEG C of mass fraction after extrusion
Gu, stretched, drawing multiple is 3 times, after end to be tensioned, under the conditions of supersonic frequency is 45kHz, used successively in solidification
Temperature is 55 DEG C of warm water washing 5min, absolute ethyl alcohol washing 4min, deionized water washing 5min, obtains shaping fiber；Again by gained
Shaping fiber is evenly laid out in stainless steel pallet, and tiling thickness is 3mm, under the conditions of temperature is 92 DEG C, bakees fine to being molded
It is 30% to tie up moisture content, obtains baking and forming fiber, then by after gained baking and forming fiber drying, cut-out produces chitin fiber.
Described chitosan is deacetylation chitosan in 80%.Described filature cap hole footpath be 0.08mm, hole density be 1000 holes/
cm2, hole count is 200,000 holes.Described drying is pneumatic conveying drying or the vacuum freeze drying under the conditions of -60 DEG C under the conditions of 35 DEG C
In one kind.
Example 2
It is 1 in mass ratio first：30, it is that 6% oxalic acid solution pours into mixer by chitosan and mass fraction, under room temperature condition,
After 400r/min rotating speeds stirring mixing 40min, standing is swelled 8h, is subsequently heated and is warming up to 55 DEG C, regulation speed of agitator to
500r/min, constant temperature stirring and dissolving 5h, after 500 mesh stainless steels sieve, obtain chitosan solution, and by gained chitosan solution in true
Reciprocal of duty cycle be 96% under the conditions of, dynamic deaeration 4h obtains spinning solution；Using wet spinning, by gained spinning solution by measuring pump with
15kg/min speed is delivered to spinning-drawing machine spinning cap and extruded, solidifying for 8% ammoniacal liquor through being preheated to 40 DEG C of mass fraction after extrusion
Gu, stretched, drawing multiple is 3 times, after end to be tensioned, under the conditions of supersonic frequency is 45kHz, used successively in solidification
Temperature is 55 DEG C of warm water washing 5min, absolute ethyl alcohol washing 4min, deionized water washing 5min, obtains shaping fiber；Again by gained
Shaping fiber is evenly laid out in stainless steel pallet, and tiling thickness is 3mm, under the conditions of temperature is 92 DEG C, bakees fine to being molded
It is 30% to tie up moisture content, obtains baking and forming fiber, then by after gained baking and forming fiber drying, cut-out produces chitin fiber.
Described chitosan is 90% chitosan with high deacetylation degree.Described filature cap hole footpath be 0.08mm, hole density be 1000 holes/
cm2, hole count is 200,000 holes.Described drying is pneumatic conveying drying or the vacuum freeze drying under the conditions of -60 DEG C under the conditions of 35 DEG C
In one kind.
Example 3
It is 1 in mass ratio first：30, it is that 6% oxalic acid solution pours into mixer by chitosan and mass fraction, under room temperature condition,
After 400r/min rotating speeds stirring mixing 40min, standing is swelled 8h, is subsequently heated and is warming up to 55 DEG C, regulation speed of agitator to
500r/min, constant temperature stirring and dissolving 5h, after 500 mesh stainless steels sieve, obtain chitosan solution, and by gained chitosan solution in true
Reciprocal of duty cycle be 96% under the conditions of, dynamic deaeration 4h obtains spinning solution；Using wet spinning, by gained spinning solution by measuring pump with
15kg/min speed is delivered to spinning-drawing machine spinning cap and extruded, and the mass fraction through being preheated to 40 DEG C is 8% hydroxide after extrusion
Sodium solution solidify, while solidification while stretched, drawing multiple be 3 times, after end to be tensioned, in supersonic frequency be 45kHz conditions
Under, it is successively that 55 DEG C of warm water wash 5min, absolute ethyl alcohol washing 4min, deionized water washing 5min with temperature, obtains shaping fiber；
Again that gained shaping fiber is evenly laid out in stainless steel pallet, tiling thickness is 3mm, under the conditions of temperature is 92 DEG C, is bakeed
It is 30% to shaping fiber moisture content, obtains baking and forming fiber, then by after gained baking and forming fiber drying, cut-out produces shell and gathered
Sugared fiber.Described chitosan is deacetylation chitosan in 80%.Described filature cap hole footpath is 0.08mm, and hole density is
1000 holes/cm2, hole count is 200,000 holes.Described drying is the pneumatic conveying drying under the conditions of 35 DEG C or vacuum is cold under the conditions of -60 DEG C
It is lyophilized it is dry in one kind.
The gained of example 1 to 3 chitin fiber is subjected to performance detection, and spunlace non-woven is made using spun lacing reinforcement process
Material, protects covering material applied to Medical wounded surface, resulting materials bacteriostasis rate is tested, the specific following institute of method of testing
State：
1. the vertical and horizontal section morphology of chitin fiber is observed using light microscope and SEM；
2. fracture strength, elongation at break and the initial modulus of chitin fiber are measured using XQ-2 fiber strength and elongations instrument, test
Condition is：Rate of extension 20m/min, stretching distance 20cm, pre-tension 0.98mN；
3. carry out bacteriostasis rate test using staphylococcus aureus and Escherichia coli.
Specific testing result is as shown in table 1：
Table 1
| Example 1 | Example 2 | Example 3 | |
| Longitudinal cross-section form | Surface is smooth | Rough surface, there is a small amount of groove | Rough surface, there is a small amount of groove |
| Lateral cross section form | It is approximate circle, without obvious skin-core structure | It is approximate circle, without obvious skin-core structure | Ellipse, there is a little skin-core structure |
| Dry break strength（cN/dtex） | 2.85 | 2.79 | 2.68 |
| Wet break strength | 2.33 | 2.31 | 2.28 |
| Water free breaking elongation rate（%） | 8.66 | 8.59 | 8.23 |
| Wet break elongation（%） | 8.87 | 8.75 | 8.56 |
| Initial modulus（cN/dtex） | 83.21 | 82.92 | 82.11 |
| Purity（%） | 99.6 | 96.2 | 94.8 |
| Bacteriostasis rate（%） | 99.8 | 92.4 | 85 |
From the testing result of table 1, the chitin fiber purity prepared using technical solution of the present invention is high, makes as medical material
With bacteriostasis rate is high.
Claims (10)
1. a kind of preparation method of chitin fiber, it is characterised in that specifically preparation process is：
（1）It is 1 in mass ratio：20~1：30, chitosan and oxalic acid solution are poured into after mixer, 20~40min of stirring mixing,
Standing is swelled 6~8h, is stirred under heating after dissolving, sieving, vacuum defoamation, obtains spinning solution；
（2）Above-mentioned gained spinning solution is delivered into spinning cap with measuring pump to be extruded, after solidifying through coagulating bath, must come into being fibre
Dimension；
（3）After above-mentioned gained as-spun fibre drawn, then it is scrubbed, shaping fiber, then baked, dry, cut-out are obtained, is produced
Chitin fiber.
2. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（1）Described shell
Glycan is deacetylation chitosan in 70~85%.
3. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（1）Described grass
Acid solution is the oxalic acid solution that mass fraction is 4~6%.
4. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（1）Described adds
Thermal agitation dissolution conditions are：In temperature be 45~55 DEG C, rotating speed be 300~500r/min under the conditions of, constant temperature stirring and dissolving 3~
5h。
5. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（2）Described meter
It is 10~15kg/min to measure pump transfer rate.
6. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（2）Described spinning
Silk cap aperture footpath is 0.06~0.08mm, and hole density is 800~1000 holes/cm2, hole count is 15~200,000 holes.
7. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（2）Described is solidifying
Gu bath is 4~8% ammoniacal liquor for the mass fraction for being preheated to 35~40 DEG C.
8. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（3）The stretching
Multiple is 2~3 times.
9. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（3）Described is dry
Dry is pneumatic conveying drying or one kind in vacuum freeze drying under the conditions of -65~-60 DEG C under the conditions of 25~35 DEG C.
10. a kind of preparation method of chitin fiber according to claim 1, it is characterised in that：Step（3）Described baking
Roasting condition is：90~92 DEG C of stoving temperature, it is 20~30% to bakee to shaping fiber moisture content.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108589040A (en) * | 2018-04-26 | 2018-09-28 | 海斯摩尔生物科技有限公司 | A kind of preparation method of high-hydroscopicity chitosan mask substrate |
| CN108625172A (en) * | 2018-04-26 | 2018-10-09 | 东华大学 | A kind of processing method of chitin fiber |
| CN109235105A (en) * | 2018-07-23 | 2019-01-18 | 华南理工大学 | A method of chitin fiber paper base material is prepared based on wet papermaking technology |
| CN109576803A (en) * | 2018-10-18 | 2019-04-05 | 青岛即发集团股份有限公司 | A kind of production method of chitin fiber |
| CN111254506A (en) * | 2020-01-19 | 2020-06-09 | 武汉纺织大学 | High-strength chitosan filament and interfacial photopolymerization preparation method and device thereof |
| CN111748870A (en) * | 2019-03-29 | 2020-10-09 | 武汉大学 | Fiber material prepared from chitosan solution with pH value of 6-8 and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108589040A (en) * | 2018-04-26 | 2018-09-28 | 海斯摩尔生物科技有限公司 | A kind of preparation method of high-hydroscopicity chitosan mask substrate |
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| CN109235105A (en) * | 2018-07-23 | 2019-01-18 | 华南理工大学 | A method of chitin fiber paper base material is prepared based on wet papermaking technology |
| CN109576803A (en) * | 2018-10-18 | 2019-04-05 | 青岛即发集团股份有限公司 | A kind of production method of chitin fiber |
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| CN111748870A (en) * | 2019-03-29 | 2020-10-09 | 武汉大学 | Fiber material prepared from chitosan solution with pH value of 6-8 and preparation method thereof |
| CN111254506A (en) * | 2020-01-19 | 2020-06-09 | 武汉纺织大学 | High-strength chitosan filament and interfacial photopolymerization preparation method and device thereof |
| CN111254506B (en) * | 2020-01-19 | 2020-11-20 | 武汉纺织大学 | High-strength chitosan filament and interfacial photopolymerization preparation method and device thereof |
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