CN101838861A - Method for preparing cellulose fiber - Google Patents
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- CN101838861A CN101838861A CN 201010164773 CN201010164773A CN101838861A CN 101838861 A CN101838861 A CN 101838861A CN 201010164773 CN201010164773 CN 201010164773 CN 201010164773 A CN201010164773 A CN 201010164773A CN 101838861 A CN101838861 A CN 101838861A
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Abstract
The invention discloses a method for preparing cellulose fiber. By using melting spinning technology, the method comprises the following steps of: 1, mixing cellulose and ionic liquid in a mass ratio of 5-8:5-2 to obtain an uniform mixture, wherein the cellulose is wood pulp, cotton pulp or bamboo pulp with degree of polymerization of 400 to 1,000; the ionic liquid consists of cations and anions; the cations are substituent-containing alkyl imidazole ions, wherein the substituent is more than one of hydrogen, C1 to C6 alkyl group, ethyl, propenyl, butenyl, ethoxyl, hydroxypropyl and alkoxy groups; the anions are halogen ions, BF4-, PF4-, SCN-, CN-, OCN-, CNO-, CF3SO3-, CFCOO-, CH3COO-, and (CF3SO2)2N- or (CF3SO2)2Cl-; 2, feeding the mixture into a double-screw extruder for melting spinning and stretching the extruded yarn by 0.5 to 6 times; and 3, washing, performing thermal forming and winding to obtain the cellulose fiber.
Description
Technical field
The present invention relates to the preparation method of cellulose fibre, particularly a kind of is plasticizer with the ionic liquid, and adopts melt-spinning technology to prepare the method for cellulose fibre.
Background technology
Cellulose is that nature is vouchsafed the abundantest human natural high molecular substance, and it not only originates abundant, and is reproducible resource.Processing and utilize cellulosic material that world's recycling economy and sustainable development are had positive meaning.Because unmodified cellulose can not fusion, so the solution processing method is the main means of preparation material of regenerated cellulose always.The production of cellulose fibre mainly is viscose process at present, yet this method energy consumption height can produce a large amount of waste gas and waste water aborning, and environment is caused substantial pollution.
In recent years, a kind of cellulosic novel solvent ionic liquid has been subjected to paying close attention to widely.Ionic liquid is meant the ionic compound that is liquid near the temperature range very big room temperature.Because it has interval big, the characteristics such as soluble end is wide, vapour pressure is extremely low, Heat stability is good of fluid temperature, is a kind of ideal solvent of various organic matters, organo-metallic compound, inorganic matter.Ionic liquid still is a kind of solvent that designs, in catalytic reaction, can ionic liquid be designed to acid or alkalescence, hydrophilic or oleophylic according to concrete demand, in addition can be designed to high-dissolvability at some concrete compounds or low solubility; And ion liquid another characteristics can reuse exactly.Therefore, be that solvent prepares the novel environment-friendly preparation method that cellulose fibre is considered to a kind of alternative viscose process with the ionic liquid.Reported by preparation method's patent documentation of the cellulose fibre of solvent is existing about ionic liquid: for example, the CN101240467A document discloses a kind of blended fiber of cellulose/polyacrylonitrile, it promptly is the cosolvent of cellulose and polyacrylonitrile with the ionic liquid, the preparation core-skin fibre, wet spinning has been adopted in this method spinning; The CN101089249A document discloses a kind of preparation method of cellulose blending fibre, and this method also is with cellulose, chitin/chitosan and ionic liquid blend dissolving and spinning, also belongs to wet spinning; The CN101240454A document discloses a kind of preparation method of blended fiber cellulose fiber, and it carries out wet spinning after the cellulose of different proportion/polyethylene base class high polymer and ion liquid dissolving are mixed again; It is the method that solvent prepares cellulose fibre with the ionic liquid that the CN1851063A document has then been reported a kind of, and this method is wet spinning equally.The cellulose solution concentration that method for preparing goes out is all lower, solution concentration the highest also less than 40%.In the scope of applicant's retrieval, be plasticizer with the ionic liquid, and the technology that adopts melt spinning method to prepare cellulose fibre is not then appeared in the newspapers.
Summary of the invention
At the deficiencies in the prior art, the technical problem that quasi-solution of the present invention is determined is, a kind of preparation method of cellulose fibre is provided, and this method is plasticizer with the ionic liquid, adopts the melt-spinning technology preparation, has the efficient height, technology is simple, and cost savings are low in the pollution of the environment, be suitable for industrializing implementation, meet characteristics such as low-carbon economy demand for development.
The technical scheme that the present invention solve the technical problem is, designs a kind of preparation method of cellulose fibre, and this preparation method adopts melt-spinning technology, comprises the following steps:
(1) in blender, with cellulose and ionic liquid solution by 5～8: 5～2 mass ratio is made homogeneous mixture,
Described cellulose is that the degree of polymerization is 400～1000 wood pulp, cotton pulp or bamboo pulp;
Described ionic liquid is made up of CATION and anion, and CATION is for containing substituent alkyl imidazole ion, and wherein substituting group is hydrogen, C
1～C
6Alkyl, vinyl, propenyl, cyclobutenyl, ethoxy, hydroxypropyl, alkoxyl in more than one; Anion is halide ion, BF
4 -, PF
4 -, SCN
-, CN
-, OCN
-, CNO
-, CF
3SO
3 -, CFCOO
-, CH
3COO
-, (CF
3SO
2)
2N
-Or (CF
3SO
2)
2Cl
-
(2) with the mixture feeding twin-screw spinning machine melt spinning that obtains in (1) step, spinning temperature is 100～170 ℃, wherein, the temperature of feeding section, melt zone, metering section and head section is respectively 100～110 ℃, 110～140 ℃, 110～160 ℃ and 120～170 ℃, screw speed is 10～100 rev/mins; Directly hot-stretch in hot dry wind of the fiber filaments of extruding, 80～140 ℃ of hot blast temperatures, draw ratio are 0.5～6 times;
(3) fiber after will stretching is washed, 50～90 ℃ of washing temperature, and HEAT SETTING, coiling promptly obtain cellulose fibre then.
Compared with prior art, the beneficial effect of the inventive method is: 1. adopt suitable ionic liquid to carry out melt spinning for the cellulose plasticizer, improved the production efficiency of cellulose fibre, significantly reduced ion liquid use amount (can with the ionic liquid mass content by 70～80% drop to melt spinning 20%), production process obviously shortens, process energy consumption and operating cost are low, and help environmental protection, meet the requirement of green production; 2. the prepared cellulose fibre of the inventive method has excellent mechanical intensity, and it is the cellulose fibre of the wet method spinning of solvent with the ionic liquid that its mechanical performance is higher than corresponding.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Preparation method's (abbreviation method) of the cellulose fibre of the present invention's design, this method adopts melt-spinning technology, comprises the following steps:
(1) in blender, with cellulose and ionic liquid solution by 5～8: 5～2 mass ratio is made homogeneous mixture,
Described cellulose is that the degree of polymerization is 400～1000 wood pulp, cotton pulp or bamboo pulp; For improving mixed effect and efficient, before mixing cellulose powder is broken into the following size of 1mm * 1mm, and then by described mixed;
Described ionic liquid is made up of CATION and anion, and CATION is for containing substituent alkyl imidazole ion, and wherein substituting group is hydrogen, C
1～C
6Alkyl, vinyl, propenyl, cyclobutenyl, ethoxy, hydroxypropyl, alkoxyl in more than one; Anion is halide ion, BF
4 -, PF
4 -, SCN
-, CN
-, OCN
-, CNO
-, CF
3SO
3 -, CFCOO
-, CH
3COO
-, (CF
3SO
2)
2N
-Or (CF
3SO
2)
2Cl
-Preferred ionic liquid is chlorination 1-allyl-3-methylimidazole ([AMIM] Cl), chlorination 1-butyl-3-methylimidazole ([BMIM] Cl), chlorination 1-ethyl-3-methylimidazole ([EMIM] Cl) or acetic acid 1-ethyl-3-methylimidazole ([EMIM] Ac).
Further feature of the present invention be when the accounting of ionic liquid in mixture when being lower than 40%, add dimethyl sulfoxide (DMSO) (DMSO), at this moment, the mass ratio of described cellulose: ionic liquid: DMSO is 6～8: 4～2: 0.5～3.3.
It is that the dilution ionic liquid reduces its viscosity that described DMSO mainly acts on, and also can partly play plasticization simultaneously.
(2) with the mixture feeding twin-screw spinning machine melt spinning that obtains in (1) step, spinning temperature is 100～170 ℃, wherein, the temperature of feeding section, melt zone, metering section and head section is respectively 100～110 ℃, 110～140 ℃, 110～160 ℃ and 120～170 ℃, screw speed is 10～100 rev/mins; The fiber filaments of extruding is directly carried out hot-stretch in hot dry wind, 80～140 ℃ of hot blast temperatures, draw ratio are 0.5～6 times;
(3) fiber after will stretching is washed, 50～90 ℃ of washing temperature, and HEAT SETTING, coiling promptly obtain cellulose fibre then.
Key of the present invention is to have adopted conventional method to think the melt spinning that can not prepare cellulose fibre, for making melting method go for the preparation of cellulose fibre, technical problem solved by the invention is under the situation that plasticizer adds, cellulosic fusing point is dropped to below the decomposition temperature, thereby can carry out melt spinning smoothly.Studies show that the adding of small amount of plasticizer can reduce the active force between cellulosic molecule, make the cellulose melt temperature drop to below the decomposition temperature, the cellulose of this moment just may carry out melt spinning.Concrete technical process is, plasticizer ionic liquid or the ionic liquid that contains dimethyl sulfoxide (DMSO) sneaked in the abundant comminuted fibres element, and mix, and feeds then in the twin-screw spinning machine of suitable process conditions to carry out melt spinning.
The present invention does not address part and is applicable to prior art.
Provide the specific embodiment of the invention below.The meaning of these embodiment only is to illustrate specific implementation method of the present invention, and the protection domain of unrestricted the present patent application claim.
Embodiment 1
To pulverize the following degree of polymerization of 1mm * 1mm and be 530 wood pulps 300g and 300g[AMIM] the Cl ionic liquid stirs into homogeneous mixture in blender, feed the double screw extruder melt spinning then, feeding section temperature is made as 100 ℃, melt zone, metering section and head section temperature are respectively 110 ℃, 130 ℃ and 140 ℃, rotating speed is 10 rev/mins, open vacuum pumping system after the discharging, through measuring pump and spinning head, the cellulose thread carries out xeothermic stretching through the hot blast path, 80 ℃ of path hot blast temperatures, 2 times of draw ratios, fiber after the stretching enters water bath and washes, 50 ℃ of washing temperature are carried out conventional HEAT SETTING and coiling then, promptly obtain fiber of the present invention.After testing, the TENSILE STRENGTH of gained cellulose fibre is 3.87cN/dtex.
Embodiment 2
To be crushed to the following degree of polymerization of 1mm * 1mm and be 530 wood pulps 300g and 200g[AMIM] Cl and 25gDMSO stir in blender, feed double screw extruder then, feeding section temperature is made as 110 ℃, melt zone, metering section and head section temperature are respectively 130 ℃, 150 ℃ and 160 ℃, rotating speed is 20 rev/mins, open vacuum pumping system after the discharging, through measuring pump and spinning head, the cellulose thread carries out xeothermic stretching through the hot blast path, wherein the path hot blast temperature is 140 ℃, 0.5 times of draw ratio, the back fiber that stretches enters water bath and washes, and 80 ℃ of washing temperature are carried out HEAT SETTING then, reel, promptly obtain described fiber, its TENSILE STRENGTH is 4.12cN/dtex.
Embodiment 3
To be crushed to the following degree of polymerization of 1mm * 1mm and be 1000 bamboo pulp 400g and 300g[BMIM] the Cl ionic liquid mixes in blender, feeds double screw extruder then.Feeding section temperature is made as 110 ℃, melt zone, metering section and head section temperature are respectively 130 ℃, 145 ℃ and 150 ℃, rotating speed is 30 rev/mins, open vacuum pumping system after the discharging, through measuring pump and spinning head, the cellulose thread carries out xeothermic stretching through the hot blast path, wherein the path hot blast temperature is 120 ℃, 3.2 times of draw ratios, the back fiber that stretches enters water bath and washes, and 90 ℃ of washing temperature are carried out HEAT SETTING, coiling then, promptly obtain described fiber, its TENSILE STRENGTH is 4.53cN/dtex.
Embodiment 4
To be crushed to the following degree of polymerization of 1mm * 1mm and be 800 cotton pulp dregs of rice 300g and 200g[BMIM] Cl ionic liquid and DMSO25g mix in blender, feed double screw extruder then, feeding section temperature is made as 100 ℃, melt zone, metering section and head temperature are respectively 120 ℃, 130 ℃ and 140 ℃, rotating speed is 30 rev/mins, open vacuum pumping system after the discharging, through measuring pump and spinning head, the cellulose thread carries out xeothermic stretching through the hot blast path, wherein the path hot blast temperature is 120 ℃, 2.5 times of draw ratios, the back fiber that stretches enters water bath and washes, and 90 ℃ of washing temperature are carried out HEAT SETTING then, reel, promptly obtain described fiber, its TENSILE STRENGTH is 4.17cN/dtex.
Embodiment 5
To be crushed to the following degree of polymerization of 1mm * 1mm and be 530 wood pulps 800g and 200g[EMIM] Ac ionic liquid and 330gDMSO stir in blender, feed double screw extruder then, feeding section temperature is made as 110 ℃, melt zone, metering section and head section temperature are respectively 145 ℃, 160 ℃ and 170 ℃, rotating speed is 100 rev/mins, open vacuum pumping system after the discharging, through measuring pump and spinning head, the cellulose thread carries out xeothermic stretching through the hot blast path, wherein the path hot blast temperature is 120 ℃, 6 times of draw ratios, the back fiber that stretches enters water bath and washes, and 90 ℃ of washing temperature are carried out HEAT SETTING then, reel, promptly obtain described fiber, its TENSILE STRENGTH is 4.57cN/dtex.
Embodiment 6
To be crushed to the following degree of polymerization of 1mm * 1mm and be 530 wood pulps 300g and 300g[EMIM] the Cl ionic liquid stirs in blender, feed double screw extruder then, feeding section temperature is made as 110 ℃, melt zone, metering section and head section temperature are respectively 135 ℃, 145 ℃ and 155 ℃, rotating speed is 60 rev/mins, open vacuum pumping system after the discharging, through measuring pump and spinning head, the cellulose thread carries out xeothermic stretching through the hot blast path, wherein the path hot blast temperature is 120 ℃, 4.5 times of draw ratios, the back fiber that stretches enters water bath and washes, and 70 ℃ of washing temperature are carried out HEAT SETTING then, reel, promptly obtain described fiber, its TENSILE STRENGTH is 4.23cN/dtex.
Claims (4)
1. the preparation method of a cellulose fibre, this preparation method adopts melt-spinning technology, comprises the following steps:
(1) in blender, with cellulose and ionic liquid solution by 5～8: 5～2 mass ratio is made homogeneous mixture,
Described cellulose is that the degree of polymerization is 400～1000 wood pulp, cotton pulp or bamboo pulp;
Described ionic liquid is made up of CATION and anion, and CATION is for containing substituent alkyl imidazole ion, and wherein substituting group is hydrogen, C
1～C
6Alkyl, vinyl, propenyl, cyclobutenyl, ethoxy, hydroxypropyl, alkoxyl in more than one; Anion is halide ion, BF
4 -, PF
4 -, SCN
-, CN
-, OCN
-, CNO
-, CF
3SO
3 -, CFCOO
-, CH
3COO
-, (CF
3SO
2)
2N
-Or (CF
3SO
2)
2C1
-
(2) with the mixture feeding twin-screw spinning machine melt spinning that obtains in (1) step, spinning temperature is 100～170 ℃, wherein, the temperature of feeding section, melt zone, metering section and head section is respectively 100～110 ℃, 110～140 ℃, 110～160 ℃ and 120～170 ℃, screw speed is 10～100 rev/mins; Directly hot-stretch in hot dry wind of the fiber filaments of extruding, 80～140 ℃ of hot blast temperatures, draw ratio are 0.5～6 times;
(3) fiber after will stretching is washed, 50～90 ℃ of washing temperature, and HEAT SETTING, coiling promptly obtain cellulose fibre then.
2. according to the preparation method of the described cellulose fibre of claim 1, it is characterized in that described ionic liquid is chlorination 1-allyl-3-methylimidazole, chlorination 1-butyl-3-methylimidazole, chlorination 1-ethyl-3-methylimidazole or acetic acid 1-ethyl-3-methylimidazole.
3. according to the preparation method of the described cellulose fibre of claim 1, before it is characterized in that mixing cellulose powder is broken into the following size of 1mm * 1mm.
4. according to the preparation method of claim 1,2 or 3 described cellulose fibres, it is characterized in that when the accounting of ionic liquid in mixture when being lower than 40%, add dimethyl sulfoxide (DMSO), cellulose: ionic liquid: the mass ratio of dimethyl sulfoxide (DMSO) is 6～8: 4～2: 0.5～3.3.
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|---|---|---|---|
| CN2010101647735A CN101838861B (en) | 2010-05-07 | 2010-05-07 | Method for preparing cellulose fiber |
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|---|---|---|---|
| CN2010101647735A CN101838861B (en) | 2010-05-07 | 2010-05-07 | Method for preparing cellulose fiber |
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| CN101838861B CN101838861B (en) | 2012-07-04 |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002762A (en) * | 2010-11-02 | 2011-04-06 | 山东海龙股份有限公司 | Method for preparing high-strength special-shape cellulose fiber |
| CN102154720A (en) * | 2010-12-21 | 2011-08-17 | 天津工业大学 | Preparation method of cellulose fibres |
| CN102477591A (en) * | 2010-11-19 | 2012-05-30 | 中国纺织科学研究院 | Cellulose fiber, preparation method thereof and equipment |
| CN102619026A (en) * | 2012-04-20 | 2012-08-01 | 天津工业大学 | Preparation method of nano micro cellulose fiber non-woven fabric |
| CN102964524A (en) * | 2012-11-28 | 2013-03-13 | 东华大学 | Method for extruding in-situ grafting modified cellulose through twin screws with ionic liquid serving as solvent |
| CN103014892A (en) * | 2012-12-26 | 2013-04-03 | 东华大学 | Preparation method of cellulose acetate fiber |
| CN103147145A (en) * | 2013-03-20 | 2013-06-12 | 天津工业大学 | Method for preparing modified cellulose fire-retardant fiber through reaction extrusion |
| CN103173932A (en) * | 2013-03-20 | 2013-06-26 | 天津工业大学 | Preparation method of antiflaming cellulose non-woven cloth |
| CN103305952A (en) * | 2013-05-03 | 2013-09-18 | 天津工业大学 | Preparation of cellulose spinning solution |
| CN103966695A (en) * | 2014-04-23 | 2014-08-06 | 安徽依采妮纤维材料科技有限公司 | Healthcare ramie fiber fabric and preparation method thereof |
| CN104047068A (en) * | 2014-07-04 | 2014-09-17 | 天津工业大学 | Method for preparing modified cellulose antibacterial fibers through reaction extrusion |
| CN104194059A (en) * | 2014-08-08 | 2014-12-10 | 华中科技大学 | Cellulose thermoplastic material and preparation method thereof |
| CN106149083A (en) * | 2015-04-02 | 2016-11-23 | 恒天海龙股份有限公司 | Functional graphene cellulose fiber prepared by melting method and preparation method thereof |
| CN106567150A (en) * | 2016-11-04 | 2017-04-19 | 天津工业大学 | Preparation method of plasticized cellulose carbamate fiber |
| CN109594150A (en) * | 2018-12-26 | 2019-04-09 | 李宁（中国）体育用品有限公司 | The foam material of polyester cotton prepares and regeneration spinning forming method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1920128A (en) * | 2006-09-12 | 2007-02-28 | 太原市伦嘉生物工程科技有限公司 | Novel function flame-proof fibre and preparation method thereof |
-
2010
- 2010-05-07 CN CN2010101647735A patent/CN101838861B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1920128A (en) * | 2006-09-12 | 2007-02-28 | 太原市伦嘉生物工程科技有限公司 | Novel function flame-proof fibre and preparation method thereof |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002762A (en) * | 2010-11-02 | 2011-04-06 | 山东海龙股份有限公司 | Method for preparing high-strength special-shape cellulose fiber |
| CN102477591B (en) * | 2010-11-19 | 2013-12-11 | 中国纺织科学研究院 | Cellulose fiber, preparation method thereof and equipment |
| CN102477591A (en) * | 2010-11-19 | 2012-05-30 | 中国纺织科学研究院 | Cellulose fiber, preparation method thereof and equipment |
| CN102154720A (en) * | 2010-12-21 | 2011-08-17 | 天津工业大学 | Preparation method of cellulose fibres |
| CN102619026A (en) * | 2012-04-20 | 2012-08-01 | 天津工业大学 | Preparation method of nano micro cellulose fiber non-woven fabric |
| CN102964524A (en) * | 2012-11-28 | 2013-03-13 | 东华大学 | Method for extruding in-situ grafting modified cellulose through twin screws with ionic liquid serving as solvent |
| CN102964524B (en) * | 2012-11-28 | 2015-05-13 | 东华大学 | Method for extruding in-situ grafting modified cellulose through twin screws with ionic liquid serving as solvent |
| CN103014892A (en) * | 2012-12-26 | 2013-04-03 | 东华大学 | Preparation method of cellulose acetate fiber |
| CN103014892B (en) * | 2012-12-26 | 2014-10-22 | 东华大学 | Preparation method of cellulose acetate fiber |
| CN103147145A (en) * | 2013-03-20 | 2013-06-12 | 天津工业大学 | Method for preparing modified cellulose fire-retardant fiber through reaction extrusion |
| CN103173932A (en) * | 2013-03-20 | 2013-06-26 | 天津工业大学 | Preparation method of antiflaming cellulose non-woven cloth |
| CN103305952A (en) * | 2013-05-03 | 2013-09-18 | 天津工业大学 | Preparation of cellulose spinning solution |
| CN103305952B (en) * | 2013-05-03 | 2017-02-08 | 天津工业大学 | Preparation of cellulose spinning solution |
| CN103966695A (en) * | 2014-04-23 | 2014-08-06 | 安徽依采妮纤维材料科技有限公司 | Healthcare ramie fiber fabric and preparation method thereof |
| CN103966695B (en) * | 2014-04-23 | 2016-02-10 | 安徽依采妮纤维材料科技有限公司 | A kind of health care ramee fabric and preparation method thereof |
| CN104047068A (en) * | 2014-07-04 | 2014-09-17 | 天津工业大学 | Method for preparing modified cellulose antibacterial fibers through reaction extrusion |
| CN104194059A (en) * | 2014-08-08 | 2014-12-10 | 华中科技大学 | Cellulose thermoplastic material and preparation method thereof |
| CN104194059B (en) * | 2014-08-08 | 2017-07-11 | 华中科技大学 | A kind of cellulose thermoplastic material and preparation method thereof |
| CN106149083A (en) * | 2015-04-02 | 2016-11-23 | 恒天海龙股份有限公司 | Functional graphene cellulose fiber prepared by melting method and preparation method thereof |
| CN106149083B (en) * | 2015-04-02 | 2018-05-15 | 恒天海龙（潍坊）新材料有限责任公司 | Functional graphene cellulose fiber prepared by melting method and preparation method thereof |
| CN106567150A (en) * | 2016-11-04 | 2017-04-19 | 天津工业大学 | Preparation method of plasticized cellulose carbamate fiber |
| CN109594150A (en) * | 2018-12-26 | 2019-04-09 | 李宁（中国）体育用品有限公司 | The foam material of polyester cotton prepares and regeneration spinning forming method |
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