CN103060939B - Preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking - Google Patents
Preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking Download PDFInfo
- Publication number
- CN103060939B CN103060939B CN201210567331.4A CN201210567331A CN103060939B CN 103060939 B CN103060939 B CN 103060939B CN 201210567331 A CN201210567331 A CN 201210567331A CN 103060939 B CN103060939 B CN 103060939B
- Authority
- CN
- China
- Prior art keywords
- cellulose acetate
- temperature
- fibre
- spinning
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking. The polybasic carboxylic acid crosslinking preparation method of the cellulose acetate fiber is characterized by, by weight, adding 21-44.5 parts of cellulose acetate tablets of which degree of substitution is 2-2.7 and degree of polymerization is 200-600, 0.5-2 parts of polybasic carboxylic acid, 0-2 parts of additives and 55-75 parts of acetone to a dissolving autoclave which is provided with a mixer and a thermometer, mixing for dissolving for 6-12h at the temperature of 40-70 DEG C to form even and stable spinning solution, deaerating and cooling the spinning solution to the constant temperature of 25-50 DEG C; metering the spinning solution by a metering pump, extruding the spinning solution from a spinneret orifice of which the diameter is 0.08-0.3 mm and the temperature is 25-40 DEG C, a spinning thread entering into a hot channel, after solvent is removed at the temperature of 25-80 DEG C, winding the spinning thread at the winding speed of 200-400 m/min to obtain cellulose acetate nascent fiber; then heat-treating the cellulose acetate nascent fiber for 1-10 min at the temperature of 170-230 DEG C to form the crosslinked cellulose acetate fiber through reaction. The fiber is obviously improved in mechanical performance and used for cigarette filtering materials, top grade textile materials and medical materials.
Description
Technical field
The present invention relates to a kind of preparation method with polycarboxylic acid crosslinked cellulose acetate fibre, belong to the preparation field of high-tech fiber.
Background context
Cellulose acetate (cellulose acetate; CA) be by cellulose after acetylation and partial hydrolysis; the substitution value obtaining is the product between 2～2.5; dissolve in concentrated hydrochloric acid, acetone, N; dinethylformamide and N; in the organic solvents such as N-dimethylacetylamide, be widely used a kind of in cellulose derivative.
Cellulose acetate fibre has the features such as moisture absorption, excellent adsorption, is a kind of filtering material of precision, is mainly used in making cigarette filter.And cellulose acetate long filament is to exactly like silk in chemical fibre most, gloss is graceful, it is bright-coloured to dye, dyefastness is strong, soft smooth, quality is light, has good natural quality sense comfortable and easy to wear; Regain is low, good springiness, do not crease easily, and has good drapability, DIMENSIONAL STABILITY, without washing setting; Its fabric has appropriate hygroscopicity, rapid-drying properties, stable anti-pilling, antistatic behaviour, easily washing, can high temperature resistant flatiron and low temperature pleating, as the substitute of silk, be mainly used in the lining of high-grade dress ornament.Cellulose acetate fibre is good textile raw material, can with the fabric of all kinds of fashionable dresses of composite spinning such as terylene, polyamide fibre, polyvinyl and silk, full dress, high-grade sportswear, good market prospects.
The production method of cellulose acetate fibre has dry method, two step wet methods and three kinds of spining technologies of a step wet method, but more because of wet spinning shortcoming, both at home and abroad main cellulose acetate fibre manufacturing enterprise all produces by take the dry spinning technology that acetone is solvent.The acetone of take is prepared cellulose acetate fibre as solvent carries out dry spinning, in order to improve dissolubility in acetone and the mobility of stoste in spinning process, the degree of polymerization of cellulose acetate is conventionally lower, general control is at 200-400, therefore the cellulose acetate fibre mechanical property obtaining is relatively poor, dry is only 1.06-1.23 cN/dtex by force, has greatly limited its Application Areas.
Chinese patent CN102251302A discloses a kind of preparation method of cellulose acetate fibre, it by dissolving cellulose acetate in ionic liquid, form the spinning solution of stable homogeneous, again stoste is carried out to dry-jet wet-spinning, obtain cellulose acetate fibre, its tensile break strength >=1.5cN/dtex.
Chinese patent 102453970A discloses a kind of low vinegar esterify cellobiose cellulose fiber and preparation method thereof, the cellulosic hydroxyl that this patent relates to is replaced by part acetate groups, substitution value is 0.01 ~ 0.5, fibrous fracture intensity >=2.0cN/dtex, elongation at break is 6% ~ 30%, line density≤3.5dtex, this fiber has the advantages that intensity is good, feel is smooth, gloss is soft and dyeability is good, and application surface is wider.This invention be take imidazole type ion liquid as solvent, take OOS as cosolvent, carry out wet method or dry-wet spinning and prepare low vinegar esterified cellulose as-spun fibre, by bathing interior drawing-off, bathe outer drawing-off, lax, washing and the operation such as be dried, the low esterify cellobiose cellulose fiber obtaining.Cellulose acetate fibre mechanical property has obtained raising to a certain degree.
The methylimidazole type ion solvent more than adopting, expensive, not large-scale production; The relative dry spinning of dry-jet wet-spinning, long flow path, production efficiency are low, and environmental pollution is comparatively serious.
Summary of the invention
The object of the invention is provides a kind of preparation method with polycarboxylic acid crosslinked cellulose acetate fibre for the deficiencies in the prior art, is characterized in solving the problem of cellulose acetate fibre poor mechanical property in prior art.Adopt polybasic carboxylic acid compound as crosslinking agent, by acetone, cellulose acetate and additive, be mixed to form uniform and stable spinning solution, through dry spinning, make as-spun fibre, again through heat treatment, make polybasic carboxylic acid become ester cross-linking reaction with cellulose acetate, preparation mechanical property is crosslinked cellulose acetate fibre preferably.The method is simple to operate, polybasic carboxylic acid compound avirulence, and by chemical crosslinking effect, under harsh service condition, crosslinking points is reliable and stable.
Object of the present invention is realized by following technical measures, and wherein said raw material mark is mass fraction except specified otherwise.
Preparation method with polycarboxylic acid crosslinked cellulose acetate fibre comprises following steps:
(1) preparation of cellulose acetate spinning solution
By substitution value, be 2 ~ 2.7, the degree of polymerization is 21 ~ 44.5 parts of 200 ~ 600 cellulose acetate sheets, 0.5 ~ 2 part of polybasic carboxylic acid, 55 ~ 75 parts, 0 ~ 2 part of additive and acetone, add in the dissolution kettle with agitator, thermometer and reflux condenser, in temperature, be 40 ~ 70 ℃, stirring and dissolving 6 ~ 12h, forms uniform and stable spinning solution;
(2) dry spinning of spinning solution
Spinning solution in step (1) is injected to spinning barrel, constant temperature to 25 ~ 50 ℃ after employing heating deaeration, vacuum defoamation or heating in vacuum deaeration; Then after measuring, filter by measuring pump, by orifice diameter, be 0.08～0.3mm, the spinnerets that is 25～40 ℃ in temperature is extruded, dynamic analysis of spinning enters the hot path that length is 4～8m, wherein path upper temp is 25～40 ℃, middle part, path temperature is 40～60 ℃, and path temperature of lower is 60～80 ℃; After desolvation, through oiling, the operation such as boundling, coiling obtains cellulose acetate as-spun fibre, winding speed is 200～400m/min, and spinneret draft multiplying power is 4～10 times; The recovery of acetone solvent adopts absorption method or liquid absorption method, and the rate of recovery is between 90 ~ 95%;
(3) post processing of as-spun fibre
As-spun fibre in step (2) is heat-treated, and heat treatment temperature is 170～230 ℃, and heat treatment time is 1～10min.In heat treatment process, organic polycarboxylic acid reacts with cellulose acetate and forms cross-linked structure; Meanwhile, eliminate the internal stress of fiber and the hole of generation.Fiber after heat treatment is polycarboxylic acid crosslinked cellulose acetate long filament, or through oiling, curling, cut-out, packing process obtain polycarboxylic acid crosslinked cellulose acetate staple fibre.
Described polycarboxylic acid crosslinked dose is 1,2,3,4-BTCA, 2-hydroxy propane-1,2,3-tricarboxylic acids, 1,2, at least one in 3-tricarballylic acid and poly-maleic acid.
Described additive is titanium dioxide, 1, 3, 5-trimethyl-2, 4, 6-(3, 5-di-t-butyl-4-hydroxy benzenes methyl) benzene, four (3, 5-di-t-butyl-4-hydroxyl) benzenpropanoic acid pentaerythritol ester, distearyl pentaerythritol diphosphite, 3-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester, the two dodecane esters of thio-2 acid, two 18 alcohol esters of thio-2 acid, three (2, 4-di-t-butyl) phenyl-phosphite, two (2, 4-di-tert-butyl-phenyl) pentaerythritol diphosphites, N, N'-pair-(3-(3, 5-di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, 2'-(the 2'-hydroxyl-3'-tert-butyl group-5'-aminomethyl phenyl)-5-chlorobenzotriazole and 2-(2'-hydroxyl-3', 5'-di-tert-butyl-phenyl) at least one in-5-chlorinated benzotriazole.
The crosslinked cellulose acetate fibre that described polybasic carboxylic acid prepares as the method for the crosslinked cellulose acetate fibre of crosslinking agent preparation.
Described crosslinked cellulose acetate fibre is as cigarette filter material, high-grade textile material and medical material.
The line density of long filament of the present invention and short fiber is measured according to GB GB/T 14343-2008 < < filament linear density test method > >, GB/T 14335-2008 < < staple line density test method > > respectively; Mechanical property is measured according to GB GB/T 14344-2008 < < filament draw method for testing performance > >, GB/T14337-2008 < < staple fibre Erichsen test method > > respectively.
Result shows: the monofilament linear density of crosslinked cellulose acetate long filament is 2～10dtex, and fracture strength is 2.0～3.0 cN/dtex, and elongation at break is 10% ~ 30%; The monofilament linear density of crosslinked cellulose acetate staple fibre is 2.5～15dtex, and fracture strength is 1.5～2.5 cN/dtex, and elongation at break is 15% ~ 50%.
Tool of the present invention has the following advantages:
1, adopt polycarboxylic acid crosslinked cellulose acetate, fibrous mechanical property is improved significantly;
2, cross-linking reaction occurs in fiber last handling process, therefore in stoste, adds after crosslinking agent, can not affect the spinnability of stoste;
3, crosslinking agent is polybasic carboxylic acid, inanimate object toxicity, and the cellulose acetate fibre making is for underclothes or medical material;
4, crosslinked cellulose acetate fibre has that intensity is good, feel is smooth, gloss is soft and the feature such as dyeability is good, for lining and the fabric of high-grade dress ornament, has good market prospects;
5, adopt existing dry spinning technology and equipment, simple to operate, technical maturity, cost is lower.
The specific embodiment
By the following examples the present invention is specifically described; be necessary to be pointed out that at this present embodiment is only used to further illustrate the present invention; but can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make according to the content of the invention described above improvement and the adjustment of some non-intrinsically safes to the present invention.
Embodiment 1
By 28 parts of the cellulose acetate sheets that substitution value is 2.5, the degree of polymerization is 400,1,2,2 parts of 3,4-BTCA, and in 70 parts of dissolution kettle that add with agitator, thermometer and reflux condenser of acetone, stirring and dissolving 8h at 30 ℃ of temperature, the transparent spinning solution that to form solid content be 30%.By in this spinning solution input spinning barrel, constant temperature to 30 ℃ after heating deaeration, then in the spinneret orifice that is 0.1mm by diameter after measuring, filter by measuring pump, extrude, dynamic analysis of spinning enters desolvation in hot path, spinning plate surface temperature is 40 ℃, path upper temp is 40 ℃, and middle part, path temperature is 60 ℃, and path temperature of lower is 80 ℃; Curing strand through oiling, boundling, coiling operation obtain cellulose acetate as-spun fibre, winding speed is 300m/min, spinneret draft ratio is 6 times.As-spun fibre enters in hot case and heat-treats, and heat treatment temperature is 230 ℃, and heat treatment time is 1min.The monofilament linear density of the crosslinked cellulose acetate long filament of gained is 4.22dtex, and fracture strength is 2.51cN/dtex, and elongation at break is 18.0%.
Embodiment 2
By 33 parts of the cellulose acetate sheets that substitution value is 2.5, the degree of polymerization is 400,2-hydroxy propane-1,2,2 parts of 3-tricarboxylic acids, and in 65 parts of dissolution kettle that add with agitator, thermometer and reflux condenser of acetone, stirring and dissolving 6h at 40 ℃ of temperature, the transparent spinning solution that to form solid content be 35%.By in this spinning solution input spinning barrel, constant temperature to 40 ℃ after heating deaeration, then in the spinneret orifice that is 0.1mm by diameter after measuring, filter by measuring pump, extrude, dynamic analysis of spinning enters desolvation in hot path, spinning plate surface temperature is 40 ℃, path upper temp is 40 ℃, and middle part, path temperature is 60 ℃, and path temperature of lower is 80 ℃; Curing strand through oiling, boundling, coiling operation obtain cellulose acetate as-spun fibre, winding speed is 250m/min, spinneret draft ratio is 5 times.As-spun fibre enters in hot case and heat-treats, and heat treatment temperature is 220 ℃, and heat treatment time is 3min.The monofilament linear density of the crosslinked cellulose acetate long filament of gained is 5.10dtex, and fracture strength is 2.23cN/dtex, and elongation at break is 26.4%.
Embodiment 3
By 44.5 parts of the cellulose acetate sheets that substitution value is 2.3, the degree of polymerization is 300,0.5 part of poly-maleic acid, and in 55 parts of dissolution kettle that add with agitator, thermometer and reflux condenser of acetone, stirring and dissolving 8h under temperature 70 C, the transparent spinning solution that formation solid content is 45%.By in this spinning solution input spinning barrel, constant temperature to 50 ℃ after heating deaeration, then in the spinneret orifice that is 0.1mm by diameter after measuring, filter by measuring pump, extrude, dynamic analysis of spinning enters desolvation in hot path, spinning plate surface temperature is 40 ℃, path upper temp is 40 ℃, and middle part, path temperature is 60 ℃, and path temperature of lower is 80 ℃; Curing strand through oiling, boundling, coiling operation obtain cellulose acetate as-spun fibre, winding speed is 300m/min, spinneret draft ratio is 6 times.As-spun fibre enters in hot case and heat-treats, and heat treatment temperature is 230 ℃, and heat treatment time is 4min.The monofilament linear density of the crosslinked cellulose acetate long filament of gained is 4.01dtex, and fracture strength is 2.14cN/dtex, and elongation at break is 33.2%.
Embodiment 4
By 27.5 parts of the cellulose acetate sheets that substitution value is 2.3, the degree of polymerization is 600,1,2,3,1.5 parts of 4-BTCA, in 70 parts of dissolution kettle that add with agitator, thermometer and reflux condenser of 1 part of distearyl pentaerythritol diphosphite and acetone, at 40 ℃ of temperature, stirring and dissolving is 8 hours, the transparent spinning solution that to form solid content be 30%.By in this spinning solution input spinning barrel, constant temperature to 40 ℃ after heating deaeration, then in the spinneret orifice that is 0.1mm by diameter after measuring, filter by measuring pump, extrude, dynamic analysis of spinning enters desolvation in hot path, spinning plate surface temperature is 40 ℃, path upper temp is 40 ℃, and middle part, path temperature is 60 ℃, and path temperature of lower is 80 ℃; Curing strand through oiling, boundling, coiling operation obtain cellulose acetate as-spun fibre, winding speed is 300m/min, spinneret draft ratio is 6 times.As-spun fibre enters in hot case and heat-treats, and heat treatment temperature is 230 ℃, and heat treatment time is 4min.The monofilament linear density of the crosslinked cellulose acetate long filament of gained is 4.38dtex, and fracture strength is 2.65cN/dtex, and elongation at break is 15.3%.
Embodiment 5
By 21 parts of the cellulose acetate sheets that substitution value is 2.0, the degree of polymerization is 400,1,2,3,2 parts of 4-BTCA, in four (3,5-di-t-butyl-4-hydroxyl) 2 parts of benzenpropanoic acid pentaerythritol esters and 75 parts of dissolution kettle that add with agitator, thermometer and reflux condenser of acetone, stirring and dissolving 8h at 30 ℃ of temperature, the transparent spinning solution that to form solid content be 25%.By in this spinning solution input spinning barrel, constant temperature to 30 ℃ after heating deaeration, then in the spinneret orifice that is 0.08mm by diameter after measuring, filter by measuring pump, extrude, dynamic analysis of spinning enters desolvation in hot path, spinning plate surface temperature is 40 ℃, path upper temp is 40 ℃, and middle part, path temperature is 60 ℃, and path temperature of lower is 80 ℃; Curing strand through oiling, boundling, coiling operation obtain cellulose acetate as-spun fibre, winding speed is 300m/min, spinneret draft ratio is 6 times.As-spun fibre enters in hot case and heat-treats, and heat treatment temperature is 230 ℃, and heat treatment time is 2min.Heat treated fiber through oiling, the operation such as curling, cut-out obtains crosslinked cellulose acetate staple fibre, its monofilament linear density is 4.53dtex, fracture strength is 2.38cN/dtex, elongation at break is 23.6%.
Embodiment 6
By 27.5 parts of the cellulose acetate sheets that substitution value is 2.7, the degree of polymerization is 200,1,2,3,1.5 parts of 4-BTCA, 1 part of additive titanium dioxide, and in 70 parts of dissolution kettle that add with agitator, thermometer and reflux condenser of acetone, stirring and dissolving 8h at 30 ℃ of temperature, the spinning solution that to form solid content be 30%.By in this spinning solution input spinning barrel, constant temperature to 25 ℃ after heating deaeration, then in the spinneret orifice that is 0.3mm by diameter after measuring, filter by measuring pump, extrude, dynamic analysis of spinning enters desolvation in hot path, spinning plate surface temperature is 25 ℃, path upper temp is 25 ℃, and middle part, path temperature is 60 ℃, and path temperature of lower is 80 ℃; Curing strand through oiling, boundling, coiling operation obtain cellulose acetate as-spun fibre, winding speed is 400m/min, spinneret draft ratio is 10 times.As-spun fibre enters in hot case and heat-treats, and heat treatment temperature is 170 ℃, and heat treatment time is 10min.The monofilament linear density of the crosslinked cellulose acetate long filament of gained is 4.28dtex, and fracture strength is 2.46cN/dtex, and elongation at break is 17.5%.
Claims (5)
1. with a preparation method for polycarboxylic acid crosslinked cellulose acetate fibre, it is characterized in that the method includes the steps of:
(1) preparation of cellulose acetate spinning solution
Count by weight, by substitution value, be 2～2.7, the degree of polymerization is 21～44.5 parts of 200～600 cellulose acetate sheets, 0.5～2 part of polybasic carboxylic acid, 55～75 parts, 0～2 part of additive and acetone, add in the dissolution kettle with agitator, thermometer and reflux condenser, in temperature, is 40～70 ℃, stirring and dissolving 6～12h, forms uniform and stable spinning solution;
(2) dry spinning of spinning solution
Spinning solution in step (1) is injected to spinning barrel, constant temperature to 25～50 ℃ after employing heating deaeration, vacuum defoamation or heating in vacuum deaeration; Then after measuring, filter by measuring pump, by orifice diameter, be 0.08～0.3mm, the spinnerets that is 25～40 ℃ in temperature is extruded, dynamic analysis of spinning enters the hot path that length is 4～8m, wherein path upper temp is 25～40 ℃, middle part, path temperature is 40～60 ℃, and path temperature of lower is 60～80 ℃; After desolvation, through oiling, boundling, coiling operation obtain cellulose acetate as-spun fibre; Wherein winding speed is 200～400m/min, and spinneret draft multiplying power is 4～10 times; The recovery of acetone solvent adopts liquid absorption method, and the rate of recovery is between 90～95%;
(3) post processing of as-spun fibre
As-spun fibre in step (2) is heat-treated, and heat treatment temperature is 170～230 ℃, and heat treatment time is 1～10min; In heat treatment process, polybasic carboxylic acid reacts with cellulose acetate and forms cross-linked structure, eliminate the internal stress of fiber and the hole of generation simultaneously, fiber after heat treatment is polycarboxylic acid crosslinked cellulose acetate long filament, or further through oiling, curling, cut-out, packing process obtain polycarboxylic acid crosslinked cellulose acetate staple fibre.
2. as claimed in claim 1 with the preparation method of polycarboxylic acid crosslinked cellulose acetate fibre, it is characterized in that polybasic carboxylic acid is 1,2,3,4-BTCA, 2-hydroxy propane-1,2, at least one in 3-tricarboxylic acids and 1,2,3-tricarballylic acid and poly-maleic acid.
3. the preparation method of polycarboxylic acid crosslinked cellulose acetate fibre as claimed in claim 1, it is characterized in that additive is titanium dioxide, 1, 3, 5-trimethyl-2, 4, 6-(3, 5-di-t-butyl-4-hydroxy benzenes methyl) benzene, four (3, 5-di-t-butyl-4-hydroxyl) benzenpropanoic acid pentaerythritol ester, distearyl pentaerythritol diphosphite, 3-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid n-octadecane alcohol ester, the two dodecane esters of thio-2 acid, two 18 alcohol esters of thio-2 acid, three (2, 4-di-t-butyl) phenyl-phosphite, two (2, 4-di-tert-butyl-phenyl) pentaerythritol diphosphites, N, N'-pair-(3-(3, 5-di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, 2'-(the 2'-hydroxyl-3'-tert-butyl group-5'-aminomethyl phenyl)-5-chlorobenzotriazole and 2-(2'-hydroxyl-3', 5'-di-tert-butyl-phenyl) at least one in-5-chlorinated benzotriazole.
4. the crosslinked cellulose acetate fibre that the preparation method of polycarboxylic acid crosslinked cellulose acetate fibre prepares as described in one of claim 1～3.
5. crosslinked cellulose acetate fibre is used as cigarette filter material, high-grade textile material and medical material as claimed in claim 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210567331.4A CN103060939B (en) | 2012-12-24 | 2012-12-24 | Preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210567331.4A CN103060939B (en) | 2012-12-24 | 2012-12-24 | Preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103060939A CN103060939A (en) | 2013-04-24 |
| CN103060939B true CN103060939B (en) | 2014-09-03 |
Family
ID=48103823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210567331.4A Active CN103060939B (en) | 2012-12-24 | 2012-12-24 | Preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103060939B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108095190B (en) * | 2017-11-09 | 2023-10-24 | 四川大学 | Environment-friendly airflow cooling tar-reducing harm-reducing cigarette holder |
| CN110101151A (en) * | 2019-05-10 | 2019-08-09 | 温州庄吉服饰有限公司 | A kind of western clothes shoulder production method |
| CN113896952B (en) * | 2021-10-14 | 2023-04-18 | 苏州和塑美科技有限公司 | High-transparency cellulose acetate material and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5653278A (en) * | 1979-09-28 | 1981-05-12 | Wakayama Prefecture | Wrinkleproof * shrinkproof and fireproof process of cellulose fiber |
| US5269996A (en) * | 1992-09-14 | 1993-12-14 | Eastman Kodak Company | Process for the production of fine denier cellulose acetate fibers |
| CN101988215A (en) * | 2009-07-30 | 2011-03-23 | 当阳新阳化纤有限公司 | Production process flow of acetate fiber filaments |
| CN102199803B (en) * | 2011-03-22 | 2013-02-27 | 武汉纺织大学 | High elastic non-ironing cellulose fiber and preparation method thereof |
-
2012
- 2012-12-24 CN CN201210567331.4A patent/CN103060939B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN103060939A (en) | 2013-04-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101492837B (en) | Process for producing bacteria cellulose fibre with high degree of polymerization | |
| US20190153625A1 (en) | Process for the production of shaped cellulose articles | |
| CN101942705B (en) | Preparation method of regenerated bacterial cellulose fiber | |
| CN102031572B (en) | A kind of preparation technology of water-soluble polyvinyl alcohol fibers and application thereof | |
| CN102493016B (en) | Porous superfine polyamide 6 fully-drawn yarn, preparation method thereof, and equipment thereof | |
| MX2013013208A (en) | Method for the production of lignin-containing precursor fibres and also carbon fibres. | |
| CN105155033B (en) | A kind of composite fibre of Flameproof polyamide 6 and preparation method thereof | |
| CN103352266B (en) | Preparation method for cellulose and thermoplastic polymer skin-core type composite fiber | |
| CN110172746B (en) | Method for preparing lyocell fibers by dissolving cellulose in solvent | |
| CN102251302A (en) | Preparation method of cellulose diacetate fiber | |
| CN104328511A (en) | Preparation method for high-strength high-modulus polyvinyl alcohol fibers | |
| CN102197080B (en) | Thermoplastic cellulose ester composition and fibers made therefrom | |
| CN106012076B (en) | A kind of wet spinning preparation method of acetate fiber | |
| CN103060939B (en) | Preparation method of cellulose acetate fiber through polybasic carboxylic acid crosslinking | |
| CN109468688A (en) | The spinning process of cellulose fibre | |
| CN101240466A (en) | Solvent method cellulose cotton and bamboo composite fiber and preparation method thereof | |
| US20210388536A1 (en) | Elastic composite fiber and fabrication method therefor | |
| CN102345180A (en) | M-phthalic acid modified terylene low elastic network fiber | |
| CN109161973A (en) | The production technology of acid fiber by polylactic | |
| CN104032399A (en) | Preparation method for acetate fiber through dry-wet process | |
| CN103014893B (en) | Method for preparing crosslinked cellulose acetate fiber with high-boiling amide as solvent | |
| KR101954239B1 (en) | Spinning apparatus for preparing lyocell fiber, and method for preparing lyocell filament fiber and lyocell staple fiber using the same | |
| CN103122499B (en) | A kind of Splittable conjugate fiber and Superfine Fibre Fabric | |
| JP4010568B2 (en) | Cellulose fiber of liquid crystal source having high elongation at break and method for producing the same | |
| CN102888690B (en) | Preparation method and device of composite polyester fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |