CN108842451B - A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan - Google Patents
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan Download PDFInfo
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- CN108842451B CN108842451B CN201810386925.2A CN201810386925A CN108842451B CN 108842451 B CN108842451 B CN 108842451B CN 201810386925 A CN201810386925 A CN 201810386925A CN 108842451 B CN108842451 B CN 108842451B
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- carboxymethyl chitosan
- chitin fiber
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- sizing
- crosslinked
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
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- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Materials For Medical Uses (AREA)
Abstract
The present invention relates to a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, after carboxymethyl chitosan is dissolved in water first, it is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, chitin fiber is immersed in crosslinked carboxymethyl chitosan sizing agent again and is dried after uniform starching, finally the chitin fiber after starching is immersed in cross-linking agent solution and is crosslinked, it dries afterwards and carboxymethyl chitosan starching chitin fiber is made, the breaking strength of carboxymethyl chitosan starching chitin fiber improves 71.7~90.2% compared to chitin fiber.It is the method for the present invention simple process, easy to operate, low in cost, the method for sizing of use improves the mechanical strength of chitin fiber, obtained products application is extensive, to being dried after carboxymethyl chitosan starching chitin fiber showering colorant, 30~60min of medicinal alcohol is immersed again, sterilizing is carried out, final vacuum drying is packed up to suture, therefore great application value.
Description
Technical field
The invention belongs to fiber treatment fields, are related to a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan.
Background technique
Chitin fiber belongs to natural material, has many advantages, such as nontoxic, hemostasis, anti-inflammatory, has good phase with biological cell
Capacitive, challeng is small, will not generate rejection with body fluid and cell；Can biodegradable, degradation in vivo
Product is Glucosamine；Glucosamine is harmless, will not generate accumulation in vivo, thus, chitosan is cured in biology
Medicine field application prospect is very extensive.Chitosan and its derivative has as organization bracket, pharmaceutical carrier etc. promotes wound
Heal, prevent tissue adhesion, anticoagulation, lipid-loweringing, norcholesterol, antiulcer, it is antitumor the effects of, in addition can also be with other fibers
It is blended to do garment material.But the main reason for being influenced by raw material, restricting chitin fiber development is that chitin fiber mechanics is strong
Degree is not high, and the breaking strength for the chitin fiber that conventional spinning obtains is only 1.07cN/dtex, and practical application is much not achieved
It is required that.Therefore, chitin fiber is modified to improve its mechanical property and be of great significance.Common enhancing chitin fiber
Method have: enhance during crosslinking enhancing, composite strengthening and spinning technique, but yet there are no the report of crosslinking starching processing so far
Road.
It all needs to carry out starching processing as fiber applications are previous, the effect of starching mainly carries out surface slurry to fiber/yarn
The coating of material and the filling of yarn interfascicular.Performance of the permeability of the thickness of warp yam surface slurry, uniformity and slurry to warp thread
Have a great impact.
Traditional starching mode is mainly soaking paste mode, in recent years, High-pressure Sizing, prewetting sizing, cold starching and is dragged in paddle
The New Sizings methods such as slurry achieve huge progress.Wherein High-pressure Sizing can close yarn texture, reinforcing fiber wearability
Can, fiber filoplume is reduced, while loom efficiency can be improved.Prewetting sizing can improve midge condition, but it can make in stock tank
There is larger fluctuation in concentration of slurry.The slurry of common soaking paste method is intermolecular main by intermolecular force connection, to fiber
Mechanical property enhancing it is limited.
The mechanical property of fiber/yarn can be obviously increased using crosslinking sizing agent starching.Crosslinking cross-linking modified at present
Journey is all before starching, and slurry concentration increases in cross-linking process, is unfavorable for subsequent starching.
Patent CN201510182592.8 discloses a kind of medium temperature textile sizing method, and its step are as follows: preparing first
Agent is starched, required clear water is added in mixing cirtern, stirring is started, obtained sizing agent dry product is added in mixing cirtern, it will be general
Lead to unmodified starch to be added in mixing cirtern, stir, sizing agent dry product is added again, continues to stir, then starts logical steam
Heating after heating, stops logical steam, insulated and stirred 30 minutes, is transported in stock tank with pump, start sizing machine, start sizing.This
Although kind of a method joined crosslinking agent in the slurry, cross-linking reaction occurs before starching, and slurry viscosity increases, be unfavorable on
It starches, product slurry made from such method is unevenly distributed, and product mechanical strength improves limited.As being crosslinked again after starching
The related research result report that then can avoid this problem, but do not there is starching post-crosslinking to handle at present.
Therefore, a kind of starching easy to operate, low in cost and that chitin fiber mechanical property can be significantly improved is developed
The great realistic meaning of method.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of chitin fiber crosslinked carboxymethyl chitosan
Method for sizing.Carboxymethyl chitosan is configured to certain density solution, to chitin fiber starching, immerses crosslinking agent after drying
It is crosslinked in solution.The intensity of starching chitin fiber beam after crosslinking is remarkably reinforced.It is crosslinked again after starching and avoids crosslinking slurry
The problem of concentration increases, and is unfavorable for starching.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, after carboxymethyl chitosan is dissolved in water first,
It is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, then chitin fiber is immersed on crosslinked carboxymethyl chitosan
It is dried after uniform starching in slurry agent, finally the chitin fiber after starching is immersed in cross-linking agent solution and is crosslinked, rear drying is made
Carboxymethyl chitosan starching chitin fiber, the breaking strength of carboxymethyl chitosan starching chitin fiber is compared to chitosan fibre
Dimension improves 71.7~90.2%, and knot strength improves 67.5~88.4%.Chitin fiber of the invention is multifilament fiber,
But protection scope of the present invention is not limited in multifilament fiber, and monfil is equally applicable to the present invention.
As a preferred option:
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan as described above, the carboxymethyl chitosan with
The mass ratio of water is 2~7:100~150.Ratio is too small, and slurry viscosity is low, and the rate of sizing is low；Ratio is excessive, and slurry viscosity is high, slurry
The poor permeability of material, does not utilize starching.
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan as described above, the carboxymethyl chitosan are molten
In water be the stirring and dissolving under the speed of 200~250rpm.Stirring rate is small, and dissolution time is long；Stirring rate is excessive, may
Chitosan macromolecular chain can be cut off, molecular weight is caused to reduce.
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan as described above, the temperature of the drying are 45
~60 DEG C.Drying temperature is excessively high to will lead to chitin fiber decomposition.
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan as described above, the cross-linking agent solution are
Ca2+Aqueous solution, concentration be 3~9wt%.Concentration is low, and crosslinking degree is inadequate, and concentration reaches 9wt%, and the degree of cross linking reaches full
With.Ca2+Aqueous solution not only can be water-soluble for calcium chloride water, calcium dihydrogen phosphate aqueous solution, calcium nitrate aqueous solution, calcium bicarbonate
Liquid, calcium bisulfate aqueous solution, calcium bisulfite aqueous solution, calcium hypochlorite aqueous solution, solution of calcium bromide in water, calcium iodide aqueous solution,
Calcium chlorate aqueous solution, Calcium perchlorate aqueous solution, acerdol aqueous solution, other contain Ca2+Aqueous solution be equally applicable to this hair
It is bright.
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan as described above, the time of the crosslinking are 5
~10min, crosslinking temperature are 15~40 DEG C.Crosslinking time is short, and crosslinking is incomplete；It is crosslinked 10min, the degree of cross linking reaches saturation, hands over
Connection degree no longer increases with the increase of crosslinking time.
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan as described above, to carboxymethyl chitosan starching
It is dried after chitin fiber showering colorant, then immerses 30~60min of medicinal alcohol, carry out sterilizing, it is final to be dried in vacuo
It packs up to suture.
Invention mechanism:
The intensity that can obviously increase the combination of slurry and fiber/yarn is crosslinked to sizing agent, in currently available technology
Cross-linking reaction is generally required could occur under liquid environment, i.e., crosslinking agent is crosslinked with slurry before starching reacts, and is crosslinked
Slurry concentration afterwards increases, and is unfavorable for subsequent starching.
The present invention is cross-linked in situ technology from original using chitin fiber starching, first carries out to chitin fiber
Slurry drying, then the chitin fiber after starching is immersed in crosslinking agent and is crosslinked, it ensure that cross-linking reaction occurs after starching, avoid
The problem of slurry viscosity increases.On the one hand the processing technique of starching post-crosslinking is kept away compared with starching mode after existing crosslinking
The problem of having exempted from slurry viscosity increase, on the other hand, the combination of starching post-crosslinking its crosslinking agent, slurry and fiber is even closer,
More preferably, properties of product are more preferable for the degree of cross linking and the rate of sizing for obtaining product, and the breaking strength of fiber is mentioned compared to pristine fibre after starching
High by 71.7~90.2%, knot strength improves 67.5~88.4%.
The utility model has the advantages that
(1) a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan of the invention is avoided in starching post-crosslinking
The problem of crosslinking slurry concentration increases, and is unfavorable for starching, great application prospect；
(2) method for sizing of a kind of chitin fiber crosslinked carboxymethyl chitosan of the invention, simple process, operation side
Just, low in cost, it is easy to accomplish industrialization；
(3) carboxymethyl chitosan sizing agent is first prepared using the present invention, starching is carried out to chitin fiber, it is upper after drying
It starches chitin fiber beam to immerse in cross-linking agent solution, crosslinks reaction, form one layer of fine and close cross-linked network in fiber surface
Structure greatly improves chitin fiber beam mechanical strength, and the chitin fiber after cross-linking reaction is widely used, can be made into doctor
Use suture.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 200rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 3:120, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
55 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 15 DEG C, the calcium chloride that concentration is 3wt%
It is crosslinked 8min in aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl chitosan is made in 55 DEG C of at a temperature of drying
The breaking strength of sugared starching chitin fiber improves 78.2% compared to chitin fiber, and knot strength improves 67.5%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 30min is immersed, finally
Vacuum drying is packed up to suture.
Embodiment 2
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 220rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 5:100, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
45 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 40 DEG C, the di(2-ethylhexyl)phosphate that concentration is 9wt%
It is crosslinked 6min in hydrogen calcium aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl is made in 40 DEG C of at a temperature of drying
The breaking strength of chitosan starching chitin fiber improves 83.1% compared to chitin fiber, and knot strength improves
88.4%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 40min is immersed, finally
Vacuum drying is packed up to suture.
Embodiment 3
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 250rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 4:130, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
50 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 20 DEG C, the calcium nitrate that concentration is 6wt%
It is crosslinked 7min in aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl chitosan is made in 50 DEG C of at a temperature of drying
The breaking strength of sugared starching chitin fiber improves 71.7% compared to chitin fiber, and knot strength improves 77.5%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 50min is immersed, finally
Vacuum drying is packed up to suture.
Embodiment 4
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 210rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 2:150, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
45 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 30 DEG C, the bicarbonate that concentration is 7wt%
It is crosslinked 10min in calcium aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl shell is made in 45 DEG C of at a temperature of drying
The breaking strength of glycan starching chitin fiber improves 77.9% compared to chitin fiber, and knot strength improves
69.8%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 45min is immersed, finally
Vacuum drying is packed up to suture.
Embodiment 5
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 200rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 7:100, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
60 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 25 DEG C, the hydrogen sulfate that concentration is 5wt%
It is crosslinked 9min in calcium aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl shell is made in 60 DEG C of at a temperature of drying
The breaking strength of glycan starching chitin fiber improves 90.2% compared to chitin fiber, and knot strength improves
85.4%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 60min is immersed, finally
Vacuum drying is packed up to suture.
Embodiment 6
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 240rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 3:140, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
55 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 33 DEG C, the calcium chlorate that concentration is 9wt%
It is crosslinked 5min in aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl chitosan is made in 55 DEG C of at a temperature of drying
The breaking strength of sugared starching chitin fiber improves 83.7% compared to chitin fiber, and knot strength improves 81.2%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 50min is immersed, finally
Vacuum drying is packed up to suture.
Embodiment 7
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 250rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 5:130, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
45 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 20 DEG C, the calcium bromide that concentration is 4wt%
It is crosslinked 6min in aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl chitosan is made in 50 DEG C of at a temperature of drying
The breaking strength of sugared starching chitin fiber improves 74.3% compared to chitin fiber, and knot strength improves 71.5%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 40min is immersed, finally
Vacuum drying is packed up to suture.
Embodiment 8
A kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, first by carboxymethyl chitosan 230rpm's
Stirring and dissolving Yu Shuihou under speed is handled through vacuum defoamation and crosslinked carboxymethyl chitosan sizing agent is made, wherein carboxymethyl chitosan
The mass ratio of sugar and water is 6:100, then immerses chitin fiber in crosslinked carboxymethyl chitosan sizing agent after uniform starching
50 DEG C at a temperature of dry, finally by after starching chitin fiber immerse temperature be 38 DEG C, the permanganic acid that concentration is 3wt%
It is crosslinked 8min in calcium aqueous solution, carboxymethyl chitosan starching chitin fiber, carboxymethyl shell is made in 45 DEG C of at a temperature of drying
The breaking strength of glycan starching chitin fiber improves 89.0% compared to chitin fiber, and knot strength improves
85.1%.
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then medicinal alcohol 30min is immersed, finally
Vacuum drying is packed up to suture.
Claims (7)
1. a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan, it is characterized in that: first that carboxymethyl chitosan is molten
Yu Shuihou is handled through vacuum defoamation and carboxymethyl chitosan sizing agent is made, then chitin fiber is immersed on carboxymethyl chitosan
It is dried after uniform starching in slurry agent, finally the chitin fiber after starching is immersed in cross-linking agent solution and is crosslinked, rear drying is made
Carboxymethyl chitosan starching chitin fiber, the breaking strength of carboxymethyl chitosan starching chitin fiber is compared to chitosan fibre
Dimension improves 71.7~90.2%, and knot strength improves 67.5~88.4%.
2. a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan according to claim 1, which is characterized in that
The mass ratio of the carboxymethyl chitosan and water is 2~7:100~150.
3. a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan according to claim 1, which is characterized in that
It is the stirring and dissolving under the speed of 200~250rpm that the carboxymethyl chitosan, which is dissolved in water,.
4. a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan according to claim 1, which is characterized in that
The temperature of the drying is 45~60 DEG C.
5. a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan according to claim 1, which is characterized in that
The cross-linking agent solution is Ca2+Aqueous solution, concentration be 3~9wt%.
6. a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan according to claim 1, which is characterized in that
The time of the crosslinking is 5~10min, and crosslinking temperature is 15~40 DEG C.
7. a kind of method for sizing of chitin fiber crosslinked carboxymethyl chitosan according to claim 1, which is characterized in that
To drying after carboxymethyl chitosan starching chitin fiber showering colorant, then 30~60min of medicinal alcohol is immersed, final vacuum
Dry packing is up to suture.
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