CN103387802A - Flame-retardant acetate fiber tape and preparation method of acetate fiber - Google Patents
Flame-retardant acetate fiber tape and preparation method of acetate fiber Download PDFInfo
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Abstract
The invention belongs to the field of fiber preparation, relates to a flame-retardant acetate fiber tape and a preparation method of acetate fiber in the flame-retardant acetate fiber tape and particularly relates to a preparation method which comprises the steps of carrying out plasticizing modification on cellulose acetate by using ionic liquid serving as a plasticizer, and then, carrying out melt spinning so as to obtain the acetate fiber with high strength. The flame-retardant acetate fiber tape comprises acetate fiber cloth, a flame-retardant rubber type adhesive and an anti-sticking agent, wherein the adhesive is coated on one face of the acetate fiber cloth and the anti-sticking agent is coated on the other face of the acetate fiber cloth. The flame-retardant acetate fiber tape is characterized in that the acetate fiber is prepared by a method which comprises the steps of mixing of cellulose acetate, drying, melt spinning, winding and the like.
Description
Technical field
The invention belongs to the fiber preparation field, relate to a kind of Anti-flaming acetate fiber tape, and the preparation method of cellulose acetate wherein, particularly relate to and a kind ofly take ionic liquid as softening agent Dichlorodiphenyl Acetate Mierocrystalline cellulose, carry out plasticization and modification, and then melt-spinning prepares the preparation method of the cellulose acetate with higher-strength.
Background technology
At present, the wire insulation shielding that is widely used in plasma (PDP) and liquid crystal (LCD) TV, indicating meter is fixing, the insulation of the DY of chromoscope (CRT) and indicating meter (CDT), deflector coil (DT) is fixed, the layer insulation of transformer (FBT) and motor, the parcel shielding of wire harness and the fixing adhesive tape of various electronic devices and components, it is high temperature resistant, high pressure, insulation, fire-retardant, anti-dissolubility is good, anti-aging and antistatic property is poor, and its quality is bad, adhere to insecure, the time slightly length can warp.
Cellulose acetate is one of most important kind of derivatived cellulose, mainly by the Mierocrystalline cellulose take cotton or timber as raw material, carries out acetylize and makes, and the hydroxyl on the cellulose macromolecule chain is replaced by acyl group, therefore is called again cellulose acetate.Present widely used cellulose acetate is that the acyl substituted degree is that 2.22～2.76 Cellulose diacetate and substitution value are 2.76～3 cellulosetri-acetate (ISO/FDIS2076:1999 (E) is about the cellulose acetate definition).The introducing of acyl group weaken on the one hand in the cellulose acetate macromolecular chain and macromolecular chain between Hyarogen-bonding, the regularity of saboteur's chain to a certain extent, make cellulose acetate show totally different in cellulosic physicochemical property on the other hand.Can survey as the cellulose acetate fusing point, possess certain thermoplasticity, and Mierocrystalline cellulose first decomposed before melting, can't record fusing point.The acyl substituted degree is different, and resulting cellulose acetate physicochemical property also are not quite similar.
The cellulose acetate dissolving spinning can be obtained cellulose acetate.Cellulose acetate is to develop one of man-made fiber early, with traditional viscose fiber, compares, and cellulose acetate not only has the characteristics of cellulosic fibre, also shows the character of synthon.Cellulose acetate has cellulose acetate filament, acetate staple fiber and three kinds of series of acetate tow.The character that is similar to the natural fiber cotton with viscose fiber is compared, and the cellulose acetate filament performance more approaches with real silk: gloss is graceful, and soft, light weight, good springiness etc. are commonly used for the substitute of silk.The cellulose acetate filament of same specification and viscose rayon filament yarn contrast, product performance/cost ratio is highly competititve.The cost of " weaving product performance and the application of cellulose acetate filament " (" synthon " second phase in 2006) domestic viscose rayon filament yarn 83dtex of data presentation is 3.6 ten thousand yuan/t approximately, price is 4.7 ten thousand yuan/t, the cost of acetate filament 83dtex is about 3.0 ten thousand yuan/t, and market price is 5.1 ten thousand yuan/t.The cellulose acetate fabric not only has the water absorbability of appropriateness, rapid-drying properties, and good drape, anti-pilling and dimensional stability, also have high-grade luxurious style, as high-grade fabric, lining and dress ornament.Acetate tow is made the cigarette filter material, and good springiness is nontoxic, and is tasteless, Heat stability is good, resistance to suction is little, the cut-off filter effect significantly, objectionable constituent in the absorption cigarette optionally, kept again certain nicotine simultaneously and do not lost the cigarette flavor; The non-woven fabrics that acetate staple fiber is made can be used for the surgical operation wrapping, do not stick with wound, and be senior medical and health; Acetate staple fiber also can be with cotton or close fine blending, make the fabric of various excellent propertys.
Due to resource consumption problems such as the severe contamination problem that exists in traditional production process of viscose fiber and water, electricity, raw materials, some developed countries such as the U.S. have stopped most of viscose fiber production in recent years, then with cellulose acetate, substitute; Particularly along with the world clothing market competition is day by day fierce, garment material is superior, the requirement of comfortableization also further impels weaving sharply to enlarge with the cellulose acetate filament market requirement, and market outlook are good.The cellulose acetate production technology is monopolized by several transnational companys few in number at present, mainly contain U.S. Celanese company and Eastman ChemicaLl company, gondola Novaceta company, MIT and Supreme Being people company and Britain Acordis company and French Rodia company etc.These company's cellulose acetate ultimate productions account for 90% left and right of global ultimate production.Domestic cellulose acetate main manufacturer has the fine company of Nantong vinegar, the fine company of Zhuhai vinegar, the fine company of Kunming vinegar and Xi'an favour major company, prepared cellulose acetate is used as cigarette filter tip materials, but there is the situation that supply falls short of demand for a long time, weaving is with the cellulose acetate filament import that places one's entire reliance upon, state's internal consumption cellulose acetate filament was approximately 6000 tons in 2003, consume 3,000 ten thousand dollars, the cellulose acetate filament of import simultaneously fabric consumes Renminbi over 1,000,000,000 yuan.
Main cellulose acetate manufacturing enterprise all takes the dry-spinning technology to produce cellulose acetate both at home and abroad at present.The existing prepared cellulose acetate shortcoming of dry-spinning technology is that fibre strength is lower, and the Cellulose diacetate long filament that the report dry-spinning is produced in " acetate silk product performance, production technology and market outlook " (" World Textile Leader " S1 phase in 2002) is done and is about by force 1.06～1.23cN/dtex.Although this low brute force does not limit its application in the traditional dress field, but because post-treatment difficulty such as being out of shape, weaving is larger, simultaneously also make the durability of cellulose acetate fabric poor, thereby the application in field of textiles and popularization are subject to certain restrictions.For guaranteeing to be out of shape, weave, the manufacturing procedure such as printing and dyeing carries out and quality product smoothly, need to manage to improve the brute force of cellulose acetate.Existing cellulose acetate production is take the stronger acetone of volatility as solvent in addition, and the acetone boiling point is 56 ℃, and flash-point is-20 ℃, explosive in air, and production brings certain danger to cellulose acetate for this, and unhelpful in environment; Simultaneously be difficult to take acetone as the dissolution with solvents cellulose acetate obtain the high cellulose acetate mass fraction spinning solution of (as greater than 30%), production efficiency is low.
In order to reduce the disadvantageous effect of bringing to environment in production process, improve cellulose acetate production efficiency, although carrying out the research of melt-spinning after plasticization and modification, the Dichlorodiphenyl Acetate Mierocrystalline cellulose has been reported, but the technology that provides not is effective plasticization and modification technology, can't apply as cellulose acetate melt-spinning production technology.Japanese Patent 5046921,5442420,62250215,978339,9291414,10317228,11506175 grades are added the simple plasticizers such as glycerine, polyoxyethylene glycol, ε caprolactone derivative to the cellulose acetate ester composition and are made fiber, but there are the problems such as plasticizer exudation or volatilization in this technology in preparing the fiber process, and fibre number is larger, diameter, at 200～300um, is not to be applicable to prepare the technology of garment material with fiber.Patent US6984631B2 take D-ALPHA-Hydroxypropionic acid and/or Pfansteihl as monomer and cellulose diacetate carry out carrying out melt-spinning after graft polymerization, yet resulting fiber lacks slippery feeling, especially when poly(lactic acid) grafting amount is too much, there are the problems such as the deterioration of fiber thermotolerance, fragility increase and poor processability.Another Japanese Patent 58225101, the patents such as 5986621,7179662,11255801 are grafted to the 6-caprolactone open loop on the cellulose acetate main chain, be prone to the side chain flow phenomenon due to graft product when the low temperature, thereby can't apply as the cellulose acetate production technology.Chinese patent 201110142220.4 discloses the method for preparing cellulose acetate with the ion liquid dissolving cellulose acetate, prepared tensile fiber breaking tenacity is 1.5～3.5cN/dtex, yet this patent adopts the dry-jet wet-spinning spining technology, spinning solution concentration not high (mass ratio of cellulose acetate and ionic liquid is 1:2～20), spinning efficiency is not high.
In sum, existing cellulose acetate production technique exists production efficiency low, the shortcomings such as carrying capacity of environment is large, and fibre breakage intensity is low, mechanical property is bad, and prior art do not provide by melt-spinning prepare good mechanical properties, the method for the cellulose acetate that is suitable for taking.
Summary of the invention
For problem and blemish in existing in prior art, the object of the present invention is to provide a kind ofly have high temperature resistant, high pressure, insulation, fire-retardant, anti-dissolubility is good, anti-aging and antistatic characteristics, the quality softness is smooth, gloss is graceful, easily tear fracture, adhere to the firmly smooth Anti-flaming acetate fiber tape that does not warp.
The technical scheme that realizes the foregoing invention purpose is: a kind of Anti-flaming acetate fiber tape, comprise acetate fibre cloth, flame retardant rubber type tackiness agent, release agent, it is characterized in that, at the fire-retardant pressure sensitive elastomer type tackiness agent of one side coating of acetate fibre cloth, another side has applied the release agent of buffer action.
Take the acetate fibre cloth of high-quality as base material,, through specifically typing, fire-retardant, embrittlement treatment process, adopts novel coating technique, simultaneously apply fire-retardant pressure sensitive elastomer type tackiness agent, another side has applied the release agent of buffer action and has made.
The objective of the invention is to solve prior art existing fibrous mechanical property be poor in cellulose acetate dry-spinning process, breaking tenacity is low and cellulose acetate plasticized melt-spinning process in because of plasticizer exudation or volatilization, the problem such as cellulose acetate graft copolymer fragility is large, processing difficulties causes fibre number is large, intensity is lower, obtain the high strength cellulose acetate.
Anti-flaming acetate fiber tape of the present invention, comprise acetate fibre cloth, flame retardant rubber type sizing agent, release agent, wherein the one side at acetate fibre cloth is coated with sizing agent, and the other side applies release agent, it is characterized in that, described cellulose acetate prepares by the following method:
(1) cellulose acetate evenly mixes with ionic liquid after pulverizing, and mixture is fed twin screw blend instrument blending extrusion, obtains water white transparency or is flaxen spinning material;
(2) with the spinning material in 35 ℃～130 ℃ lower continuous vacuum drying 20～70h;
(3) melt-spinning: dried spinning material, through the filament spinning component melt-spinning, then passes through hot-rolling drawing-off, extraction liquid, washing;
(4) again through oiling, drying and coiling operation, obtain the cellulose acetate that fibre breakage intensity is 2.5～6cN/dtex;
Described ionic liquid is comprised of positively charged ion and negatively charged ion; Described positively charged ion is a kind of in 1,3-dialkylimidazolium or 1-R1-3-R2-dialkyl imidazoles, and wherein R1 is the alkyl that meets following rule: (1) contains two carbon atoms at least, (2) no more than 20 carbon atoms, and (3) contain a two key at least; R2 is the saturated or undersaturated alkyl that contains 1～4 carbon atom; Described negatively charged ion is halide-ions, tetrafluoroborate, hexafluoro-phosphate radical or fluoroform yellow acid root;
The temperature of described melt blending is 160 ℃～250 ℃;
Described melt-spinning speed is 100m/min～1000m/min, and spinning temperature is 160 ℃～280 ℃;
Described extraction liquid is the mixing solutions of water and ionic liquid, and wherein the ionic liquid massfraction is no more than 30%; The extraction liquid temperature is 10 ℃～60 ℃.
As preferred technical scheme:
The preparation method of a kind of cellulose acetate as above, described cellulose acetate weight-average molecular weight is 100000～400000, and the cellulose acetate polymerization degree is 200～1000, and cellulose acetate acyl substituted degree is 2.0～2.6.
The preparation method of a kind of cellulose acetate as above, the mass ratio of described cellulose acetate and ionic liquid is 7～2:1.
The preparation method of a kind of cellulose acetate as above, the temperature of feeding section, melt zone, metering zone and the head of described twin screw blend instrument screw extrusion press is respectively 160～250 ℃, and 160～250 ℃, 160～240 ℃, 160～240 ℃; Rotating speed is 10～120 rev/mins.
The preparation method of a kind of cellulose acetate as above, the granularity after described cellulose acetate is pulverized is less than 300 orders.
The preparation method of a kind of cellulose acetate as above, described hot-rolling drafting multiple is 1.1～6 times, drawing temperature is 40～120 ℃.
The preparation method of a kind of cellulose acetate as above, described washing is ultrasonic washing, in water washing process, the temperature of water is 30～100 ℃.
The preparation method of a kind of cellulose acetate as above, described drying temperature is at 30～100 ℃.
The preparation method of a kind of cellulose acetate as above, the filament number of described cellulose acetate are 5～50.0dtex; Described cellulose acetate comprises long filament, staple fibre and tow.
The preparation method of a kind of cellulose acetate as above, the fibre section of described cellulose acetate is circle, trilateral, pentagon, trilobal, quatrefoil, five leaf, fan-shaped or hollow shape.
Beneficial effect:
(1) need not in the fiber preparation process through as harmful organic solvent dissolutions such as acetone, DMAc, DMF, chloroforms, ionic liquid is nontoxic, and is non-volatile, avoided the pollution to environment, is conducive to improve production environment.
(2) carry out plasticization and modification take ionic liquid as softening agent Dichlorodiphenyl Acetate Mierocrystalline cellulose, complete processing is simple, and processing parameter is selected comparatively flexibly and be easy to control, and process energy consumption and process cost are low.The ionic liquid non-volatility, be easy to reclaim, and extraction liquid is water or ionic liquid aqueous solution, meets the requirement of green production.
(3) cellulose acetate of the present invention's preparation has the high quality umber, and the cellulose acetate cellulose content can significantly improve the production efficiency of cellulose acetate up to 66.7～87.5%, and cellulose acetate has mechanical property and breaking tenacity preferably.
(4) preparation method of the present invention adopts the melt-spinning technology, and technical process is short, flexible parameter selection and more easy to control, and fibre modification is convenient, is applicable to continuous production.
Description of drawings
Fig. 1 is the longitudinal sectional drawing of Anti-flaming acetate fiber tape of the present invention.
Embodiment
, below in conjunction with embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for explanation the present 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 limited range equally.
(1) with substitution value be 2.2, the polymerization degree be 260 and weight-average molecular weight be that 181800 cellulose acetate is crushed to 280 orders, mixes than 2:1 is even according to massfraction with 1-butyl-3-methyl imidazolium tetrafluoroborate (BMIMBF4) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 160 ℃～170 ℃, 170 ℃, 160～170 ℃, 160 ℃, the forcing machine rotating speed is 10～50 rev/mins.Obtain the water white transparency spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 60 ℃ of lower continuous vacuum drying 70h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 170 ℃.The orifice of spinning spinneret is the triangle star of distortion.Spinning speed is 400m/min.The hot-rolling drafting multiple is 2.6 times, and drawing temperature is 60 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 30 ℃, and obtaining cross section is leg-of-mutton fiber, and its breaking tenacity is 2.7cN/dtex, and the fibre single thread fiber number is 18dtex.
(1) with substitution value be 2.3, the polymerization degree be 360 and weight-average molecular weight be that 235000 cellulose acetate is crushed to 250 orders, mixes than 2:1 is even according to massfraction with 1-butyl-3-methyl imidazolium tetrafluoroborate (BMIMBF4) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 170 ℃～180 ℃, 190 ℃, 160～170 ℃, 160 ℃, the forcing machine rotating speed is 50～120 rev/mins.Obtain the water white transparency spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 60 ℃ of lower continuous vacuum drying 70h;
(3) the spinning material carries out melt-spinning after metering, 190 ℃ of spinning temperatures.Spinning speed is 1000m/min.The hot-rolling drafting multiple is 3 times, and drawing temperature is 60 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 30 ℃, obtains circular-section fibers, and its breaking tenacity is 6cN/dtex, and the fibre single thread fiber number is 5dtex.
(1) with substitution value be 2.6, the polymerization degree be 1000 and weight-average molecular weight be that 400000 cellulose acetate is crushed to 300 orders, mixes than 7:1 is even according to massfraction with 1-butyl-3-methyl imidazolium tetrafluoroborate (BMIMBF4) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 230 ℃～240 ℃, and 240 ℃, 230～240 ℃, 230 ℃.The forcing machine rotating speed is 10～30 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 120 ℃ of lower continuous vacuum drying 30h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 260 ℃.Spinning speed is 500m/min.The hot-rolling drafting multiple is 6 times, and drawing temperature is 120 ℃.Take water as extraction liquid, the extraction liquid temperature is 60 ℃; Through ultrasonic washing, ultrasonic washing temperature is 100 ℃ again;
(4) after oiling, drying is reeled again when temperature is 100 ℃, obtains circular-section fibers, and its breaking tenacity is 4.2cN/dtex, and the fibre single thread fiber number is 10dtex.
Embodiment 4
(1) with substitution value be 2.0, the polymerization degree be 200 and weight-average molecular weight be that 100000 cellulose acetate is crushed to 250 orders, mixes than 4:1 is even according to massfraction with 1-butyl-3-methyl imidazolium tetrafluoroborate (BMIMBF4) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 170 ℃～180 ℃, 170 ℃, 170～180 ℃, 170 ℃, the forcing machine rotating speed is 10～50 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 90 ℃ of lower continuous vacuum drying 70h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 220 ℃.The orifice of spinning spinneret is bifurcation shape.Spinning speed is 200m/min.The hot-rolling drafting multiple is 2.25 times, and drawing temperature is 90 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 50 ℃, obtains the fiber that cross section is trilobal, and its breaking tenacity is 2.3cN/dtex, and the fibre single thread fiber number is 27dtex.
Embodiment 5
(1) with substitution value be 2.4, the polymerization degree be 600 and weight-average molecular weight be that 282300 cellulose acetate is crushed to 240 orders, mixes than 2:1 is even according to massfraction with 1-butyl-3-Methylimidazole fluoroform sulphonate (BMIMOTF) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 170 ℃～180 ℃, 190 ℃, 160～170 ℃, 160 ℃, the forcing machine rotating speed is 10～50 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 70 ℃ of lower continuous vacuum drying 40h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 200 ℃.Spinning speed is 450m/min.The orifice of spinning spinneret is star.The hot-rolling drafting multiple is 1.5 times, and drawing temperature is 70 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 70 ℃, and obtaining cross section is pentagonal fiber, and its breaking tenacity is 2.8cN/dtex, and the fibre single thread fiber number is 19dtex.
Embodiment 6
(1) with substitution value be 2.3, the polymerization degree be 430 and weight-average molecular weight be that 235000 cellulose acetate is crushed to 280 orders, mixes than 4:1 is even according to massfraction with 1-butyl-3-Methylimidazole fluoroform sulphonate (BMIMOTF) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 210～220 ℃, 210 ℃, 210～220 ℃, 210 ℃,, the forcing machine rotating speed is 10～50 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 100 ℃ of lower continuous vacuum drying 40h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 240 ℃.Spinning speed is 700m/min.The hot-rolling drafting multiple is 3.7 times, and drawing temperature is 100 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 70 ℃, and obtaining cross section is round fiber, and its breaking tenacity is 3.5cN/dtex, and the fibre single thread fiber number is 12dtex.
Embodiment 7
(1) with substitution value be 2.1, the polymerization degree be 400 and weight-average molecular weight be that 205000 cellulose acetate is crushed to 280 orders, mixes than 3:1 is even according to massfraction with 1-butyl-3-Methylimidazole fluoroform sulphonate (BMIMOTF) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 220～230 ℃, 230 ℃, 220～230 ℃, 210 ℃,, the forcing machine rotating speed is 10～50 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 100 ℃ of lower continuous vacuum drying 40h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 230 ℃.Spinning speed is 400m/min.The orifice of spinning spinneret is X-shaped.The hot-rolling drafting multiple is 2.3 times, and drawing temperature is 100 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 70 ℃, obtains the fiber that cross section is quatrefoil, and its breaking tenacity is 2.7cN/dtex, and the fibre single thread fiber number is 24dtex.
Embodiment 8
(1) with substitution value be 2.3, the polymerization degree be 450 and weight-average molecular weight be that 262300 cellulose acetate is crushed to 250 orders, mixes than 3:1 is even according to massfraction with 1-butyl-3-Methylimidazole fluoroform sulphonate (BMIMOTF) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 190 ℃～200 ℃, 200 ℃, 190～200 ℃, 190 ℃, the forcing machine rotating speed is 10～50 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 100 ℃ of lower continuous vacuum drying 40h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 210 ℃.Spinning speed is 400m/min.The orifice of spinning spinneret is C shape.The hot-rolling drafting multiple is 1.5 times, and drawing temperature is 100 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 70 ℃, obtains tubular fibre, and its breaking tenacity is 2.8cN/dtex, and the fibre single thread fiber number is 16dtex.
Embodiment 9
(1) with substitution value be 2.5, the polymerization degree be 450 and weight-average molecular weight be that 291000 cellulose acetate is crushed to 280 orders, mixes than 2:1 is even according to massfraction with 1-butyl-3-Methylimidazole hexafluorophosphate (BMIMPF6) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 180 ℃～190 ℃, 190 ℃, 170～180 ℃, 170 ℃, the forcing machine rotating speed is 10～50 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 70 ℃ of lower continuous vacuum drying 30h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 210 ℃.Spinning speed is 720m/min.The hot-rolling drafting multiple is 1.1 times, and drawing temperature is 70 ℃.With water and ionic liquid 1-butyl, 3 methyl-imidazoles villaumite mixed solution is extraction liquid, and ionic liquid content is 30%; The extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 70 ℃, obtains cross section and is circular fiber, and its breaking tenacity is 3.0cN/dtex, and the fibre single thread fiber number is 13dtex.
Embodiment 10
(1) with substitution value be 2.1, the polymerization degree be 850 and weight-average molecular weight be that 331200 cellulose acetate is crushed to 280 orders, mixes than 2:1 is even according to massfraction with 1-butyl-3-Methylimidazole hexafluorophosphate (BMIMPF6) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 180 ℃～190 ℃, 190 ℃, 170～180 ℃, 170 ℃, the forcing machine rotating speed is 50～80 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 70 ℃ of lower continuous vacuum drying 30h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 210 ℃.Spinning speed is 200m/min.The orifice of spinning spinneret is five leaf.The roller drafting multiple is 1.1 times, and drawing temperature is 70 ℃.With water and ionic liquid 1-butyl, 3 methyl-imidazoles villaumite mixed solution is extraction liquid, and ionic liquid content is 30%; The extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 70 ℃, and obtaining cross section is five leaf fibers, and its breaking tenacity is 2.3cN/dtex, and the fibre single thread fiber number is 28dtex.
Embodiment 11
(1) with substitution value be 2.4, the polymerization degree be 750 and weight-average molecular weight be that 305400 cellulose acetate is crushed to 230 orders, mixes than 3:1 is even according to massfraction with 1-butyl-3-Methylimidazole hexafluorophosphate (BMIMPF6) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 190 ℃～200 ℃, 210 ℃, 190～200 ℃, 190 ℃, the forcing machine rotating speed is 50～80 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 90 ℃ of lower continuous vacuum drying 30h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 220 ℃.Spinning speed is 150m/min.The orifice of spinning spinneret is fan-shaped.The roller drafting multiple is 1.4 times, and drawing temperature is 90 ℃.With water and ionic liquid 1-butyl, 3 methyl-imidazoles villaumite mixed solution is extraction liquid, and ionic liquid content is 30%; The extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 70 ℃, and obtaining cross section is fan-shaped fiber, and its breaking tenacity is 2.2cN/dtex, and the fibre single thread fiber number is 35dtex.
Embodiment 12
(1) with substitution value be 2.2, the polymerization degree be 240 and weight-average molecular weight be that 201500 cellulose acetate is crushed to 280 orders, mixes than 2:1 is even according to massfraction with 1-butyl-3-Methylimidazole villaumite (BMIMCl) after dry.Mixture is fed twin screw blend instrument blending extrusion, section, and twin screw blend instrument adopts screw rod blending extrusion in the same way, and wherein feeding section, melt zone, metering zone and head temperature are respectively 180 ℃～190 ℃, 190 ℃, 170～180 ℃, 170 ℃, the forcing machine rotating speed is 10～50 rev/mins.Obtain faint yellow transparent spinning material.
(2) the spinning material is put into and vacuumized baking oven, in 70 ℃ of lower continuous vacuum drying 70h;
(3) the spinning material carries out melt-spinning after metering, and spinning temperature is 230 ℃.Spinning speed is 350m/min.The hot-rolling drafting multiple is 1.8 times, and drawing temperature is 70 ℃.Take water as extraction liquid, the extraction liquid temperature is 10 ℃; Through ultrasonic washing, ultrasonic washing temperature is 30 ℃ again;
(4) after oiling, drying is reeled again when temperature is 80 ℃, obtains cross section and is circular fiber, and its breaking tenacity is 2.3cN/dtex, and the fibre single thread fiber number is 20dtex.
Claims (10)
1. Anti-flaming acetate fiber tape, comprise acetate fibre cloth, flame retardant rubber type sizing agent, release agent, wherein the one side at acetate fibre cloth is coated with sizing agent, and the other side applies release agent, it is characterized in that, described cellulose acetate prepares by the following method:
(1) cellulose acetate evenly mixes with ionic liquid after pulverizing, and mixture is fed twin screw blend instrument blending extrusion, obtains water white transparency or is flaxen spinning material;
(2) with the spinning material in 35 ℃～130 ℃ lower continuous vacuum drying 20～70h;
(3) melt-spinning: dried spinning material, through the filament spinning component melt-spinning, then passes through hot-rolling drawing-off, extraction liquid, washing;
(4) again through oiling, drying and coiling operation, obtain the cellulose acetate that fibre breakage intensity is 2.5～6cN/dtex;
Described ionic liquid is comprised of positively charged ion and negatively charged ion; Described positively charged ion is a kind of in 1,3-dialkylimidazolium or 1-R1-3-R2-dialkyl imidazoles, and wherein R1 is the alkyl that meets following rule: (1) contains two carbon atoms at least, (2) no more than 20 carbon atoms, and (3) contain a two key at least; R2 is the saturated or undersaturated alkyl that contains 1～4 carbon atom; Described negatively charged ion is halide-ions, tetrafluoroborate, hexafluoro-phosphate radical or fluoroform yellow acid root;
The temperature of described melt blending is 160 ℃～250 ℃;
Described melt-spinning speed is 100m/min～1000m/min, and spinning temperature is 160 ℃～280 ℃;
Described extraction liquid is the mixing solutions of water and ionic liquid, and wherein the ionic liquid massfraction is no more than 30%; The extraction liquid temperature is 10 ℃～60 ℃.
2. Anti-flaming acetate fiber tape according to claim 1, is characterized in that, described cellulose acetate weight-average molecular weight is 100000～400000, and the cellulose acetate polymerization degree is 200～1000, and cellulose acetate acyl substituted degree is 2.0～2.6.
3. the Anti-flaming acetate fiber tape described according to claim 1, is characterized in that, the mass ratio of described cellulose acetate and ionic liquid is 7～2:1.
4. the Anti-flaming acetate fiber tape described according to claim 1, is characterized in that, the temperature of feeding section, melt zone, metering zone and the head of described twin screw blend instrument is respectively 160～250 ℃, 160～250 ℃, and 160～240 ℃, 160～240 ℃; Rotating speed is 10～120 rev/mins.
5. the Anti-flaming acetate fiber tape described according to claim 1, is characterized in that, the granularity after described cellulose acetate is pulverized is less than 300 orders.
6. Anti-flaming acetate fiber tape according to claim 1, is characterized in that, described hot-rolling drafting multiple is 1.1～6 times, and drawing temperature is 40～120 ℃.
7. Anti-flaming acetate fiber tape according to claim 1, is characterized in that, described washing is ultrasonic washing, and in water washing process, the temperature of water is 30～100 ℃.
8. the Anti-flaming acetate fiber tape of a kind of cellulose acetate described according to claim 1, is characterized in that, described drying temperature is at 30～100 ℃.
9. the Anti-flaming acetate fiber tape described according to claim 1, is characterized in that, the filament number of described cellulose acetate is 5～35dtex; Described cellulose acetate comprises long filament, staple fibre and tow.
10. the Anti-flaming acetate fiber tape described according to claim 1, is characterized in that, the fibre section of described cellulose acetate is circle, trilateral, pentagon, trilobal, quatrefoil, five leaf, fan-shaped or hollow shape.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105297443A (en) * | 2015-11-30 | 2016-02-03 | 浙江超凡制衣有限公司 | Blended material with high acetate fiber content and preparation method of blended material |
| CN110079240A (en) * | 2019-03-26 | 2019-08-02 | 宁波太古新材料科技有限公司 | A kind of adhesive tape and preparation method thereof with fire-retardant electro-magnetic screen function |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5341515A (en) * | 1976-09-27 | 1978-04-15 | Mitsubishi Rayon Co Ltd | Production of flame-retardant cellulose acetate f ibers |
| CN201390723Y (en) * | 2009-04-20 | 2010-01-27 | 陕西彩桥电子材料股份有限公司 | Anti-flaming acetate fiber tape |
| CN103014892A (en) * | 2012-12-26 | 2013-04-03 | 东华大学 | Preparation method of cellulose acetate fiber |
-
2013
- 2013-08-15 CN CN2013103564745A patent/CN103387802A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5341515A (en) * | 1976-09-27 | 1978-04-15 | Mitsubishi Rayon Co Ltd | Production of flame-retardant cellulose acetate f ibers |
| CN201390723Y (en) * | 2009-04-20 | 2010-01-27 | 陕西彩桥电子材料股份有限公司 | Anti-flaming acetate fiber tape |
| CN103014892A (en) * | 2012-12-26 | 2013-04-03 | 东华大学 | Preparation method of cellulose acetate fiber |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105297443A (en) * | 2015-11-30 | 2016-02-03 | 浙江超凡制衣有限公司 | Blended material with high acetate fiber content and preparation method of blended material |
| CN105297443B (en) * | 2015-11-30 | 2017-09-26 | 浙江超凡制衣有限公司 | A kind of blended material of high acetic acid fiber content and preparation method thereof |
| CN110079240A (en) * | 2019-03-26 | 2019-08-02 | 宁波太古新材料科技有限公司 | A kind of adhesive tape and preparation method thereof with fire-retardant electro-magnetic screen function |
| CN110079240B (en) * | 2019-03-26 | 2021-07-09 | 宁波太古新材料科技有限公司 | Adhesive tape with flame-retardant electromagnetic shielding function and preparation method thereof |
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Application publication date: 20131113 |