CN102251302A - Preparation method of cellulose diacetate fiber - Google Patents
Preparation method of cellulose diacetate fiber Download PDFInfo
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- CN102251302A CN102251302A CN 201110142220 CN201110142220A CN102251302A CN 102251302 A CN102251302 A CN 102251302A CN 201110142220 CN201110142220 CN 201110142220 CN 201110142220 A CN201110142220 A CN 201110142220A CN 102251302 A CN102251302 A CN 102251302A
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- cellulose diacetate
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- methylimidazole
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Abstract
The invention relates to a preparation method of cellulose diacetate fiber, in particular to a preparation method of cellulose diacetate fiber for carrying out dry-jet wet spinning with ionic liquid serving as a solvent. The preparation method comprises the following steps of: 1, dissolving the cellulose diacetate in the ionic liquid to form a uniform and stable spinning stock solution, and 2, carrying out dry-jet wet spinning on the spinning stock solution to obtain the cellulose diacetate fiber. According to the preparation method of the cellulose diacetate fiber, provided by the invention, the problems of low tensile strength of fiber and poor mechanical performance existed in the cellulose diacetate dry spinning process, and low degree of substitution of the cellulose acetate fiber prepared by using the ionic liquid as the solvent, lower strength of the prepared fiber, and the like in the prior art are solved.
Description
Technical field
The present invention relates to a kind of preparation method of cellulose diacetate fibers, particularly relating to a kind of is the preparation method that solvent carries out the cellulose diacetate fibers of dry-jet wet-spinning with the ionic liquid.
Background technology
Cellulose diacetate (CDA) is meant: carry out the Triafol T that obtains (CTA) after the acetylation by cellulose, pass through partly-hydrolysed hydrolysis again after, the substitution value that obtains is generally the product between 2～2.5.It is to use in the cellulose derivative early, and is widely used a kind of.
Cellulose diacetate fibers is the fiber that is obtained by the dissolving of cellulose diacetate process, spinning, has characteristics such as moisture absorption, excellent adsorption, is a kind of secondary filter material, is mainly used in the making cigaratte filter.The cellulose diacetate long filament of weaving usefulness is the most approaching with real silk in chemical fibre, the gloss gracefulness, and it is bright-coloured to dye, the dyeing COLOR FASTNESS is strong, soft, quality is light, and regain is low, good springiness, do not crease easily, have good drapability, DIMENSIONAL STABILITY, its fabric has appropriate hygroscopicity, rapid-drying properties.And have stable anti-pilling, antistatic behaviour, spot easily comes off, easily washing, can be used for high-grade dress ornament in material, be subjected to consumer's favor.The cellulose diacetate long filament can with the compound compound silks of making such as polyvinyl, terylene, statecraft and real silk, be applied to all kinds of men and women's fashionable dresses, full dress, high-grade sportswear and suiting.The cellulose diacetate long filament is good textile raw material, and market prospects are fine.
Cellulose diacetate fibers is mainly produced by the dry spinning technology, and solvent is an acetone.At present, the fine company of domestic Nantong vinegar, the fine company of Zhuhai vinegar, the fine company of Kunming vinegar and Xi'an favour major company produce cellulose diacetate fibers, are used for cigaratte filter.Abroad except cigarette filter with the Celluloseacetate cigarette filter tow, there is the cellulose diacetate long filament of plurality of specifications to put on market, as the Italian Novaceta 84dtex/23f of company, the mould proof vinegar ester of 167dtex/38f " Silfresh ", preceding painted acetate filament series is spun by U.S. Eastman company " Chromspun ", product specification 84dtex/19f, 330dtex/76f, wherein " ChromspunTFAJ " is used for air-jet loom, and other also come into the market as thin dawn acetate filament yarn, the acetate filament at thin dawn of monofilament and cross dyeing effect acetate filament.The cellulose diacetate long filament that the report dry spinning is produced in " the fine continuous yarn product performance of vinegar, production technology and market prospects " (" international weaving Leader " S1 phase in 2002) is done and is about 1.06～1.23cN/dtex by force.
The solvent acetone of preparation cellulose diacetate use has very strong volatility at present, and flash-point low (subzero 20 ℃) promptly arrives boiling point under 56 ℃, have certain risk during use, and the sealing and the resistance to pressure of equipment are had relatively high expectations.And contact acetone for a long time human body is had very major injury, production environment is relatively poor.
People (Preparation and Subsequent Shaping of Cellulose Acetates Using Ionic Liquids.Macromolecular Materials and Engineering such as Birgit Kosan and Thomas Heinze; 2010 (295): 676-681)) announced a kind of in ionic liquid ([BMIM] Cl) dissolving cellulos and to its acetylation, and then spinning moulding obtains the method for fiber.In its reported method, control degree of acetylation by the mole proportioning that changes acetic anhydride and unit anhydroglucose, obtain the different cellulose acetate of substitution value.Obtain tensile strength of fiber and reduce along with the increase of degree of acetylation, report in the document that substitution value was 1.4 when degree of acetylation was the highest, the TENSILE STRENGTH of respective fiber is 1.68cN/dtex.
The weak point that above-mentioned technology prepares the cellulose diacetate fibers existence mainly is that fibre strength is on the low side, and market is used and is restricted.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of cellulose diacetate fibers, particularly providing a kind of is that solvent carries out the method that dry-jet wet-spinning prepares cellulose diacetate with the ionic liquid, to solve prior art existing tensile strength of fiber is low in cellulose diacetate dry spinning process, mechanical property is bad and to be that solvent prepares problems such as substitution value is not high in the cellulose acetate fibre, the gained fibre strength is lower with the ionic liquid.
In order to solve the problems of the technologies described above, the technical scheme that the present invention uses is: a kind of preparation method of cellulose diacetate fibers is to be the method that solvent prepares cellulose diacetate fibers with the ionic liquid, may further comprise the steps:
(1) cellulose diacetate is dissolved in ionic liquid, form the spinning solution of stable homogeneous;
Described cellulose diacetate and described ion liquid mass ratio are 1: 2～20;
The temperature of described dissolving is 70～130 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 1.5～5.0dtex,
TENSILE STRENGTH 〉=1.5cN/dtex;
70～130 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 0～70 ℃; Described dry-jet wet-spinning has the twice washing, and the temperature of first road washing is 20～100 ℃, and the temperature of second road washing is 30～100 ℃;
To solidify the aerial distance of water-bath be 10～80mm to spinning solution up to entering from going out spinnerets; Spinning speed 10～150m/min, 2～15 times of drawing-off multiplying powers.Orifice diameter is 0.08～0.2mm;
Wherein,
Described cellulose diacetate molecular formula is [C
6H
7O
2(COOCH
3)
x(OH)
3-x]
n, n=200～600 wherein, x is a substitution value, x=2～2.5;
Described ionic liquid is a methylimidazole type ionic liquid, is 1-butyl-3-methylimidazole villaumite, 1-butyl-3-methylimidazole bromine salt, 1-allyl-3-methylimidazole bromine salt, 1-ethyl-3 methylimidazole acetate, 1-ethyl-3 methylimidazole formates or 1-ethyl-3 methylimidazole methyl phosphite salt.
As optimized technical scheme:
The TENSILE STRENGTH of described cellulose diacetate fibers is 1.5～3.5cN/dtex.
Beneficial effect
(1) the diacetate fibre element need not process as harmful organic solvent dissolutions such as acetone, DMAc, DMF, and ionic liquid is nontoxic, and is non-volatile, avoided the pollution to environment, helps improving production environment.
(2) compare with the method that people such as Birgit Kosan and Thomas Heinze announce; this method adopts ionic liquid directly to dissolve the cellulose diacetate sheet; the two can finely be dissolved in together; solute effect is more abundant than adding acetic anhydride or chloroacetic chloride acetylation in the cellulose/ion liquid system, and the concentration of ordinary dissolution upper limit significantly improves.This method preparation technology is simple in addition, and technological parameter is selected comparatively flexible, and the TENSILE STRENGTH of gained fiber is significantly improved.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) be 2.5 with substitution value, the degree of polymerization is 600 cellulose diacetate, dissolves in 1-butyl-3-methylimidazole villaumite, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 2;
The temperature of described dissolving is 130 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 1.5dtex, fracture strength is 2.5cN/dtex; 105 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 10 ℃; Described dry-jet wet-spinning has the twice washing, and the temperature of first road washing is 65 ℃, and the temperature of second road washing is 100 ℃; To solidify the aerial distance of water-bath be 80mm to spinning solution up to entering from going out spinnerets; Spinning speed 150m/min, 15 times of drawing-off multiplying powers.
Embodiment 2
(1) be 2 with substitution value, the degree of polymerization is 200 cellulose diacetate, dissolves in 1-butyl-3-methylimidazole bromine salt, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 20;
The temperature of described dissolving is 70 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 3.0dtex, fracture strength is 1.5cN/dtex; 70 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 0 ℃; Described dry-jet wet-spinning has the twice washing stretching, and the temperature of the first road washing stretching is 50 ℃, and the temperature of second road washing is 90 ℃; To solidify the aerial distance of water-bath be 10mm to spinning solution up to entering from going out spinnerets; Spinning speed 10m/min, 2 times of drawing-off multiplying powers.
Embodiment 3
(1) be 2.35 with substitution value, the degree of polymerization is 300 cellulose diacetate, dissolves in ionic liquid 1-ethyl-3 methylimidazole acetate, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 9; The temperature of described dissolving is 90 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 5.0dtex, TENSILE STRENGTH is 2.0cN/dtex; 90 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulating bath of described dry-jet wet-spinning is a deionized water, and temperature is 5 ℃; Described dry-jet wet-spinning has the twice washing stretching, and the temperature of the first road washing stretching is 80 ℃, and the temperature of the second road washing stretching is 95 ℃; To solidify the aerial distance of water-bath be 50mm to spinning solution up to entering from going out spinnerets; Spinning speed 50m/min, 10 times of drawing-off multiplying powers.
Embodiment 4
(1) be 2.4 with substitution value, the degree of polymerization is 300 cellulose diacetate, dissolves in 1-ethyl-3 methylimidazole formates, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 8; The temperature of described dissolving is 100 ℃;
(2) with spinning solution standing and defoaming under uniform temperature and vacuum condition; Temperature is 100 ℃; Vacuum condition is meant that vacuum is 0.08MPa; The time of deaeration is 4 hours;
(3) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 3.8dtex, TENSILE STRENGTH is 2.1cN/dtex; 100 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 9 ℃; Described dry-jet wet-spinning has the twice washing stretching, and the temperature of the first road washing stretching is 70 ℃, and the temperature of the second road washing stretching is 98 ℃; To solidify the aerial distance of water-bath be 50mm to spinning solution up to entering from going out spinnerets; Spinning speed 100m/min, 10 times of drawing-off multiplying powers.
Embodiment 5
(1) be 2.3 with substitution value, the degree of polymerization is 400 cellulose diacetate, dissolves in 1-allyl-3-methylimidazole bromine salt, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 7; The temperature of described dissolving is 80 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 4.0dtex, TENSILE STRENGTH is 3.5cN/dtex; 90 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 10 ℃; Described dry-jet wet-spinning has the twice washing stretching, and the temperature of the first road washing stretching is 80 ℃, and the temperature of the second road washing stretching is 100 ℃; To solidify the aerial distance of water-bath be 20mm to spinning solution up to entering from going out spinnerets; Spinning speed 80m/min, 8 times of drawing-off multiplying powers.
Embodiment 6
(1) be 2.36 with substitution value, the degree of polymerization is 300 cellulose diacetate, dissolves in 1-allyl-3-methylimidazole bromine salt, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 6; The temperature of described dissolving is 110 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 3.5dtex, TENSILE STRENGTH is 4.0cN/dtex; 110 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 15 ℃; Described dry-jet wet-spinning has the twice washing stretching, and the temperature of first road washing is 60 ℃, and the temperature of second road washing is 90 ℃; To solidify the aerial distance of water-bath be 30mm to Polymer Solution up to entering from going out spinnerets; Spinning speed 40m/min, 4 times of drawing-off multiplying powers.。
Embodiment 7
(1) be 2.3 with substitution value, the degree of polymerization is 600 cellulose diacetate, dissolves in 1-ethyl-3 methylimidazole methyl phosphite salt, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 5; The temperature of described dissolving is 115 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 2.0dtex, TENSILE STRENGTH is 1.8cN/dtex; 115 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 5 ℃; Described dry-jet wet-spinning has the twice washing stretching, and the temperature of first road washing is 50 ℃, and the temperature of second road washing is 96 ℃; To solidify the aerial distance of water-bath be 40mm to Polymer Solution up to entering from going out spinnerets; Spinning speed 60m/min, 12 times of drawing-off multiplying powers.
Embodiment 8
(1) be 2.47 with substitution value, the degree of polymerization is 500 cellulose diacetate, dissolves in 1-ethyl-3 methylimidazole methyl phosphite salt, forms the spinning solution of stable homogeneous; Described cellulose diacetate and described ion liquid mass ratio are 1: 4; The temperature of described dissolving is 95 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 3.0dtex, TENSILE STRENGTH is 3.0cN/dtex; 95 ℃ of the spinning temperatures of described dry-jet wet-spinning; The coagulation bath temperature of described dry-jet wet-spinning is 7 ℃; Described dry-jet wet-spinning has the twice washing stretching, and the temperature of the first road washing stretching is 60 ℃, and the temperature of the second road washing stretching is 97 ℃; To solidify the aerial distance of water-bath be 20mm to spinning solution up to entering from going out spinnerets; Spinning speed 120m/min, 12 times of drawing-off multiplying powers.
Claims (2)
1. the preparation method of a cellulose diacetate fibers is characterized in that may further comprise the steps:
(1) cellulose diacetate is dissolved in ionic liquid, form the spinning solution of stable homogeneous;
Described cellulose diacetate and described ion liquid mass ratio are 1: 2～20;
The temperature of described dissolving is 70～130 ℃;
(2) spinning solution is carried out dry-jet wet-spinning, obtain described cellulose diacetate fibers, filament number 1.5～5.0dtex, tensile break strength 〉=1.5cN/dtex;
70～130 ℃ of the spinning temperatures of described dry-jet wet-spinning; To solidify the aerial distance of water-bath be 10～80mm to spinning solution up to entering from going out spinnerets; Spinning speed 10～150m/min, 2～15 times of drawing-off multiplying powers.
Wherein,
Described cellulose diacetate molecular formula is [C
6H
70
2(COOCH
3)
x(OH)
3-x]
n, n=200～600 wherein, x is a substitution value, x=2～2.5;
Described ionic liquid is a methylimidazole type ionic liquid, is 1-butyl-3-methylimidazole villaumite, 1-butyl-3-methylimidazole bromine salt, 1-allyl-3-methylimidazole bromine salt, 1-ethyl-3 methylimidazole acetate, 1-ethyl-3 methylimidazole formates or 1-ethyl-3 methylimidazole methyl phosphite salt.
2. the preparation method of a kind of cellulose diacetate fibers according to claim 1 is characterized in that, the tensile break strength of described cellulose diacetate fibers is 1.5～3.5cN/dtex.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014892A (en) * | 2012-12-26 | 2013-04-03 | 东华大学 | Preparation method of cellulose acetate fiber |
| CN103173878A (en) * | 2013-03-22 | 2013-06-26 | 南通醋酸纤维有限公司 | Cellulose acetate fiber high speed spinning integral process |
| CN104032399A (en) * | 2014-05-09 | 2014-09-10 | 南通醋酸纤维有限公司 | Preparation method for acetate fiber through dry-wet process |
| CN105088371A (en) * | 2015-07-21 | 2015-11-25 | 河南工程学院 | Preparation method of high-draft aliphatic polyamide fibers by adoption of melt spinning |
| CN106012076A (en) * | 2016-07-15 | 2016-10-12 | 吉林富博纤维研究院有限公司 | Wet spinning method for preparing cellulose acetate fiber |
| CN106381564A (en) * | 2016-09-21 | 2017-02-08 | 东华大学 | Preparation method of functional regeneration cellulose fiber |
| CN107475782A (en) * | 2017-07-31 | 2017-12-15 | 东华大学 | A kind of acetate fiber and preparation method thereof |
| CN109793269A (en) * | 2019-01-30 | 2019-05-24 | 湖北中烟工业有限责任公司 | Preparation method and application for the floral type tow in Novel heating not burning tobacco |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1851063A (en) * | 2006-05-19 | 2006-10-25 | 东华大学 | Method for preparing cellulose fiber using ion liquid as solvent |
| CN101089249A (en) * | 2007-07-06 | 2007-12-19 | 东华大学 | Preparation and application of cellulose mixed fibre using ion liquid as solvent |
| CN101230494A (en) * | 2008-02-22 | 2008-07-30 | 东华大学 | Solvent preparation cellulose blending fibre and use thereof |
| JP2009256830A (en) * | 2008-04-16 | 2009-11-05 | Mitsubishi Rayon Co Ltd | Method for producing cellulose acetate combined filament yarn |
-
2011
- 2011-05-28 CN CN 201110142220 patent/CN102251302A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1851063A (en) * | 2006-05-19 | 2006-10-25 | 东华大学 | Method for preparing cellulose fiber using ion liquid as solvent |
| CN101089249A (en) * | 2007-07-06 | 2007-12-19 | 东华大学 | Preparation and application of cellulose mixed fibre using ion liquid as solvent |
| CN101230494A (en) * | 2008-02-22 | 2008-07-30 | 东华大学 | Solvent preparation cellulose blending fibre and use thereof |
| JP2009256830A (en) * | 2008-04-16 | 2009-11-05 | Mitsubishi Rayon Co Ltd | Method for producing cellulose acetate combined filament yarn |
Non-Patent Citations (1)
| Title |
|---|
| 《上海化工》 20050228 李宙雷等 离子液体在溶解方面的研究进展 第22-24页 1-2 第30卷, 第2期 * |
Cited By (14)
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| CN103014892B (en) * | 2012-12-26 | 2014-10-22 | 东华大学 | Preparation method of cellulose acetate fiber |
| CN103014892A (en) * | 2012-12-26 | 2013-04-03 | 东华大学 | Preparation method of cellulose acetate fiber |
| CN103173878A (en) * | 2013-03-22 | 2013-06-26 | 南通醋酸纤维有限公司 | Cellulose acetate fiber high speed spinning integral process |
| CN103173878B (en) * | 2013-03-22 | 2015-09-23 | 南通醋酸纤维有限公司 | Acetate fiber high speed spinning integrated technique |
| CN104032399A (en) * | 2014-05-09 | 2014-09-10 | 南通醋酸纤维有限公司 | Preparation method for acetate fiber through dry-wet process |
| CN105088371B (en) * | 2015-07-21 | 2017-11-03 | 河南工程学院 | It is a kind of can high drafting melt-spun aliphatic polyamide fiber preparation method |
| CN105088371A (en) * | 2015-07-21 | 2015-11-25 | 河南工程学院 | Preparation method of high-draft aliphatic polyamide fibers by adoption of melt spinning |
| CN106012076A (en) * | 2016-07-15 | 2016-10-12 | 吉林富博纤维研究院有限公司 | Wet spinning method for preparing cellulose acetate fiber |
| CN106012076B (en) * | 2016-07-15 | 2018-06-19 | 吉林富博纤维研究院有限公司 | A kind of wet spinning preparation method of acetate fiber |
| CN106381564A (en) * | 2016-09-21 | 2017-02-08 | 东华大学 | Preparation method of functional regeneration cellulose fiber |
| CN106381564B (en) * | 2016-09-21 | 2018-11-23 | 东华大学 | A kind of preparation method of functional regeneration cellulose fibre |
| CN107475782A (en) * | 2017-07-31 | 2017-12-15 | 东华大学 | A kind of acetate fiber and preparation method thereof |
| CN107475782B (en) * | 2017-07-31 | 2019-10-29 | 东华大学 | A kind of acetate fiber and preparation method thereof |
| CN109793269A (en) * | 2019-01-30 | 2019-05-24 | 湖北中烟工业有限责任公司 | Preparation method and application for the floral type tow in Novel heating not burning tobacco |
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Application publication date: 20111123 |