CN101230495A - Solvent preparation of cellulose fiber releasing anion and use thereof - Google Patents
Solvent preparation of cellulose fiber releasing anion and use thereof Download PDFInfo
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- CN101230495A CN101230495A CNA2008100337912A CN200810033791A CN101230495A CN 101230495 A CN101230495 A CN 101230495A CN A2008100337912 A CNA2008100337912 A CN A2008100337912A CN 200810033791 A CN200810033791 A CN 200810033791A CN 101230495 A CN101230495 A CN 101230495A
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- cellulose
- fibre
- tourmaline powder
- solvent method
- spinning
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Abstract
The invention relates to a method of preparing a cellulose fibre releasing anions by using the solvent method and the application. The method has the following steps: firstly, the comminuted cellulose, tourmaline powder and addition agent are well mixed with an ironic liquid, dissolved at a temperature of 35 to 160 DEG C, deaerated for 1 to 120 hours and a homogeneous and stable spinning solution with a total solid content of 3 to 30 percent is formed, wherein, the mixed mass ratio of the tourmaline powder is 0.01 to 20 percent and the added mass ratio of the addition agent is 0 to 10 percent; secondly, the spinning solution is filtered, deaerated, spinned and solidified through a coagulation bath; and thirdly, a composite fibre of cellulose and tourmaline powder is obtained after the procedures of stretching, water cleaning, bleaching, oiling and drying. The composite fibre has the functions of releasing anions, generating far infrared radiation, generating biocurrent and suppressing bacteria and is applicable to the fields of garments, ornaments and medical textiles. The ironic liquid used in the invention has high production efficiency, is easy for callback and conforms to the requirement of a green production. The prepared composite fibre has excellent mechanical strength and mechanical property, and the fabric made of the composite fibre can release anions, resist bacteria and prevent mildew.
Description
Technical field
The invention belongs to the cellulose fibre field, particularly relate to the solvent method preparation and the application of the cellulose fibre that discharges anion.
Background technology
Not only storage level is big for cellulose in all substances of occurring in nature, and huge amount of recovery is arranged.Have only few cellulose to be made into fiber at present.Be used to make the cellulose amount of fiber and film, 4% of the cellulose output of producing no more than world industry.Along with the mankind to the deepening continuously and the worsening shortages of resources such as oil, coal, natural gas of nature understanding, cellulosic utilization also will enlarge gradually.Cellulose fibre is because raw cellulose can be changed into steam and carbon dioxide by biological decomposition or safe combustion, and the destruction environmental problem that is caused by discarded object is few.Therefore it is very necessary developing cellulose fibre.Wherein, make the semi-products of regenerated celulose fibre---the raw material source of pulp is also quite extensive, from the needlebush of high-quality and cotton linter to leaf wood, fast growing wood, bamboo and various herbaceous plant (as bagasse, reed, jute bar etc.).
What at present produce cellulose fibers mainly adopted is viscose process, and production process is tediously long and complicated, energy consumption and operating cost height, and exist waste gas, waste water, waste residue pollution, handle multinomial problem such as recovery.And ionic liquid exists with liquid state in the scope of broad as a kind of novel cellulose solvent, and has good heat endurance, and nontoxic, non-volatility helps environmental protection and operator ' s health.Can change its physicochemical properties by the yin, yang ion population of selecting to suit, be the good solvent of many organic matters, inorganic matter and macromolecular material.Many ionic liquids are very big to cellulosic solubility, some in addition reach 35%; Be no more than 10% and adopt cellulose yellow method to produce the cellulose concentration that viscose adopted, therefore adopt the ionic liquid produce cellulose fibers to enhance productivity greatly.
Along with the progress of society and the raising of people's living standard, the fashion of textile garment, ecological property and the functional theme that becomes current textile garment industry.Consider that surrounding air intermediate ion concentration and balance thereof can influence biological tissue, comprise tissue.It is reported, high-negative ion concentration to the influence of human body comprise lax, lessen fatigue, nervous and constrain.By in fabric, adding the anion propellant, generate anion in the body temperature heating or with the human body friction.In addition, the anion fabric has the antibacterial and mouldproof effect.
The cellulose negative-ion fiber report that sees report at present mainly contains following two classes:
1. Chinese patent 01128377.7 discloses a kind of functional rayon staple that adopts viscose process production can discharge anion.
2. Chinese patent CN1385565 discloses a kind of anion viscose fibre and manufacture method thereof.
Summary of the invention
The present invention aims to provide a kind of solvent method preparation and application that discharges the cellulose fibre of anion, by being that solvent comes dissolving cellulos and tourmaline powder to prepare composite fibre with the ionic liquid, solved the problem of environmental pollution that present employing viscose process produce cellulose fibers is brought, and bring the function that cellulose discharges anion, satisfy and produce needs.
A kind of solvent method preparation that discharges the cellulose fibre of anion of the present invention comprises step:
(1) comminuted fibres element, tourmaline powder, auxiliary agent and ionic liquid are mixed, dissolving, deaeration are 1～120 hour under 35～160 ℃ of temperature, the formation total solid content is 3～30% stable homogeneous spinning solution, wherein the mass mixing ratio of tourmaline powder is 0.01～20%, the interpolation quality of auxiliary agent is 0-10%, microwave radiation, applies the dissolving that certain vacuum etc. helps pulp;
(2) after filtration, after the deaeration, adopt wet spinning, dry-jet wet spinning or melt and spray wet spinning and carry out spinning, coagulating bath is solidified, and wherein coagulating bath is the ionic liquid aqueous solution of water or 0～60%, and coagulation bath temperature is 0～90 ℃, and spinning speed is 5～150 meters/minute;
(3) drawn, washing, bleaching again, thoroughly to remove the various impurity in the fiber, again through oiling, operation such as drying, obtain cellulose/tourmaline powder composite fibre.
Described comminuted fibres element is the degree of polymerization 300～2500, the native cellulose (comprising bamboo pulp, wood pulps, the cotton pulp dregs of rice, reed pulp, bagasse pulp, waste of flax slurry etc.) of alpha-cellulose content 90%～100%, bacteria cellulose, cotton, cellulose acetate etc. are through mechanical crushing, and pulp is through activation processing or do not process.
Described tourmaline powder is a tourmaline powder, and granularity can reach 10～400nm.
Described auxiliary agent is aliphatic acid, silane coupler, titanate esters.
Described ionic liquid is made up of CATION and anion, and CATION is that substituting group is hydrogen, C
1～C
6Alkyl, vinyl, propenyl, cyclobutenyl, ethoxy, hydroxypropyl, alkoxyl in one or more quaternary ammonium alkyl ion, alkyl quaternary phosphonium ion, alkyl imidazole ion or alkyl pyridine ion; Described anion is halide ion, BF
4 -, PF
4 -, SCN
-, CN
-, OCN
-, CNO
-, CF
3SO
3 -, CF
3COO
-, (CF
3SO
2)
2N
-Or (CF
3SO
2)
2Cl
-In a kind of.
Described stretching is that fiber stretches through one or more combinations such as nervous stretching, jet stretch, plasticization drawing, air bath after-drawing or retractions, and total extensibility is 3～200%.
Described composite fibre comprises blend staple fibre and long filament, and fibre strength is 2～5cN/dtex, and the cross sectional shape of fiber has routine and abnormity.
This composite fibre also has the far infrared radiation of generation, produces functions such as bioelectricity and inhibition bacterium except having negative ion-releasing function, is applicable to clothes, decoration, medical textile field.
Tourmaline is a kind of boron aluminium sulfate among the present invention, its chemical composition comprises: boron oxide, aluminium oxide, iron oxide, magnesia, sodium oxide molybdena, calcium oxide etc., the thermoelectricity characteristic of calcium carbide crystal makes it can produce electrical potential difference when extraneous temperature and pressure changes, generation is up to the electrostatic pressure of 1,000,000 electron volts, and the generation electric field.Excited electron combines with neutral molecule or atom on every side, thereby produces anion.External heat or impulsive force all can make tourmaline generate anion.Every mL tourmaline powder can produce 1175～4997 ions.Significant pyroelectricity and piezoelectricity are arranged.The tourmaline powder has permanent electrode, and ultra-fine powder has the positive and negative polarities characteristic, can produce the bioelectricity that is consistent with human body, and human body is produced stimulation and health-care function is arranged.Because the special construction of tourmaline powder, its permanent electrode is had an effect to the bacterial cell epidermis, and Escherichia coli, Candida albicans are had the inhibition effect, and bacteriostasis rate is more than 70%.
Beneficial effect of the present invention:
(1) adopt ionic liquid to prepare cellulose/inorganic mineral powder composite fibre, avoided the tediously long and complicated production process of viscose process, production process obviously shortens, process energy consumption and operating cost are low, and ionic liquid is as a kind of novel cellulose solvent, nontoxic, non-volatility, help environmental protection and operator ' s health, the ion liquid aqueous solution also can be used as coagulating bath, and ionic liquid is easy to reclaim, and meets the requirement of green production;
(2) the preparation-obtained cellulose of the present invention/tourmaline powder composite fibre has excellent mechanical intensity, and its mechanical performance is suitable with conventional viscose;
(3) fabric that cellulose/the tourmaline powder composite fibre is made can discharge anion, and has the antibacterial and mouldproof effect.
The specific embodiment
Below in conjunction with 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.
Umber among each embodiment is parts by weight.
Embodiment 1
9 parts of native celluloses pulverizing, 1 part of tourmaline powder are mixed with 100 parts of [BMIM] Cl (1-butyl-3-methylimidazole hydrochloride) ionic liquid,, obtain spinning solution 45 ℃ of stirrings 24 hours down.
Spinning solution after filtration, after the deaeration, enter into through the porous spinnerets and to contain 5% ion liquid coagulating bath, coagulation bath temperature is 25 ℃.After 10% stretching, again through wash, bleach, oil, dry supervisor, spinning speed is 5 meters/minute, obtains the fiber that intensity is 2.5cN/dtex.
Embodiment 2
10 parts of bacteria celluloses, 0.1 part of tourmaline powder and 90 parts of [BMIM] Cl ionic liquids of pulverizing are mixed, stirred 120 hours down, obtain spinning solution at 100 ℃.
Spinning solution after filtration, after the deaeration, enter into the water coagulating bath through the porous spinnerets, coagulation bath temperature is 15 ℃.After 3% stretching, again through wash, bleach, oil, dry supervisor, spinning speed is 20 meters/minute, obtains the fiber that intensity is 3.3cN/dtex.
Embodiment 3
1 portion of cotton pulverizing, 0.2 part of tourmaline powder are mixed with 3 parts of [AMIM] Cl (1-allyl-3-methylimidazole hydrochloride) ionic liquid,, obtain spinning solution 60 ℃ of stirrings 80 hours down.
Spinning solution after filtration, after the deaeration, enter into through the porous spinnerets and to contain 25% ion liquid coagulating bath, coagulation bath temperature is 55 ℃.Behind 8% plasticization drawing, again through wash, bleach, oil, dry supervisor, spinning speed is 30 meters/minute, obtains the fiber that intensity is 2.1cN/dtex.
Claims (8)
1. solvent method preparation that discharges the cellulose fibre of anion comprises step:
(1) comminuted fibres element, tourmaline powder, auxiliary agent and ionic liquid are mixed, dissolving, deaeration are 1～120 hour under 35～160 ℃ of temperature, the formation total solid content is 3～30% stable homogeneous spinning solution, wherein the mass mixing ratio of tourmaline powder is 0.01～20%, and the interpolation quality of auxiliary agent is 0～10%;
(2) after filtration, after the deaeration, spinning, coagulating bath is solidified;
(3) drawn, washing, bleaching again, again through oiling, drying process, cellulose/tourmaline powder composite fibre.
2. the preparation of the solvent method of the cellulose fibre of release anion according to claim 1 is characterized in that: described comminuted fibres element is the degree of polymerization 300～2500, native cellulose, bacteria cellulose, cotton or the cellulose acetate of alpha-cellulose content 90%～100% be through mechanical crushing.
3. the solvent method preparation of the cellulose fibre of release anion according to claim 1, it is characterized in that: described tourmaline powder is a tourmaline powder, granularity 10～400nm.
4. the solvent method preparation of the cellulose fibre of release anion according to claim 1, it is characterized in that: described auxiliary agent is aliphatic acid, silane coupler, titanate esters.
5. the solvent method preparation of the cellulose fibre of release anion according to claim 1, it is characterized in that: described ionic liquid is made up of CATION and anion, and CATION is that substituting group is hydrogen, C
1～C
6Alkyl, vinyl, propenyl, cyclobutenyl, ethoxy, hydroxypropyl, alkoxyl in one or more quaternary ammonium alkyl ion, alkyl quaternary phosphonium ion, alkyl imidazole ion or alkyl pyridine ion;
Described anion is halide ion, BF
4 -, PF
4 -, SCN
-, CN
-, OCN
-, CNO
-, CF
3SO
3 -, CF
3COO
-, (CF
3SO
2)
2N-or (CF
3SO
2)
2Cl
-In a kind of.
6. the solvent method preparation of the cellulose fibre of release anion according to claim 1, it is characterized in that: the spinning in the described step (2) is wet spinning, dry-jet wet spinning or melts and sprays wet spinning and carry out spinning, wherein coagulating bath is the ionic liquid aqueous solution of water or 0～60%, coagulation bath temperature is 0～90 ℃, and spinning speed is 5～150 meters/minute.
7. the solvent method preparation of the cellulose fibre of release anion according to claim 1, it is characterized in that: the stretching in the described step (3) is that fiber stretches through the one or more combination in nervous stretching, jet stretch, plasticization drawing, air bath after-drawing or the retraction, and total extensibility is 3～200%.
8. the solvent method preparation of the cellulose fibre of release anion according to claim 1, it is characterized in that: described composite fibre is blend staple fibre or long filament, and fibre strength is 2～5cN/dtex, the cross sectional shape of fiber is conventional or special-shaped.
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| CNA2008100337912A CN101230495A (en) | 2008-02-22 | 2008-02-22 | Solvent preparation of cellulose fiber releasing anion and use thereof |
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|---|---|---|---|
| CNA2008100337912A CN101230495A (en) | 2008-02-22 | 2008-02-22 | Solvent preparation of cellulose fiber releasing anion and use thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660792A (en) * | 2012-04-10 | 2012-09-12 | 山东银鹰化纤有限公司 | Technology for preparing solar heat storage warming fibers through solvent method |
| CN102877153A (en) * | 2011-07-14 | 2013-01-16 | 广东柏堡龙股份有限公司 | Negative ion cool lining and method for preparing same |
| CN103866415A (en) * | 2014-02-07 | 2014-06-18 | 陈麒 | Anion viscose acetal fiber and preparation method thereof |
| DE102015105309A1 (en) | 2014-04-08 | 2015-10-08 | Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. | Cellulose shaped body with physiologically active minerals distributed therein |
| CN106435817A (en) * | 2016-09-21 | 2017-02-22 | 东华大学 | Preparation method of functional regenerated cellulose fiber |
| CN106435797A (en) * | 2016-09-21 | 2017-02-22 | 东华大学 | Preparation method of cellulose/carbon nanotube composite fiber |
| CN107460596A (en) * | 2017-08-04 | 2017-12-12 | 宁波黄古林工艺品有限公司 | A kind of bamboo fibre summer sleeping mat and preparation method thereof |
| CN108914563A (en) * | 2018-06-01 | 2018-11-30 | 吴江康欣医用敷料有限公司 | A kind of preparation method and applications of safety durable carbassus |
| CN113373528A (en) * | 2021-06-09 | 2021-09-10 | 温州市名达服饰有限公司 | Warm-keeping western-style trousers and warm-keeping layer thereof |
-
2008
- 2008-02-22 CN CNA2008100337912A patent/CN101230495A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102877153A (en) * | 2011-07-14 | 2013-01-16 | 广东柏堡龙股份有限公司 | Negative ion cool lining and method for preparing same |
| CN102660792A (en) * | 2012-04-10 | 2012-09-12 | 山东银鹰化纤有限公司 | Technology for preparing solar heat storage warming fibers through solvent method |
| CN102660792B (en) * | 2012-04-10 | 2014-11-19 | 山东银鹰化纤有限公司 | Technology for preparing solar heat storage warming fibers through solvent method |
| CN103866415A (en) * | 2014-02-07 | 2014-06-18 | 陈麒 | Anion viscose acetal fiber and preparation method thereof |
| DE102015105309A1 (en) | 2014-04-08 | 2015-10-08 | Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. | Cellulose shaped body with physiologically active minerals distributed therein |
| CN106435817A (en) * | 2016-09-21 | 2017-02-22 | 东华大学 | Preparation method of functional regenerated cellulose fiber |
| CN106435797A (en) * | 2016-09-21 | 2017-02-22 | 东华大学 | Preparation method of cellulose/carbon nanotube composite fiber |
| CN106435797B (en) * | 2016-09-21 | 2018-11-23 | 东华大学 | A kind of preparation method of cellulose/carbon nano composite fibre |
| CN106435817B (en) * | 2016-09-21 | 2019-01-15 | 东华大学 | A kind of preparation method of functional regeneration cellulose fibre |
| CN107460596A (en) * | 2017-08-04 | 2017-12-12 | 宁波黄古林工艺品有限公司 | A kind of bamboo fibre summer sleeping mat and preparation method thereof |
| CN108914563A (en) * | 2018-06-01 | 2018-11-30 | 吴江康欣医用敷料有限公司 | A kind of preparation method and applications of safety durable carbassus |
| CN113373528A (en) * | 2021-06-09 | 2021-09-10 | 温州市名达服饰有限公司 | Warm-keeping western-style trousers and warm-keeping layer thereof |
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Open date: 20080730 |