CN101838863B - Polysiloxane fibers and preparation method thereof - Google Patents
Polysiloxane fibers and preparation method thereof Download PDFInfo
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- CN101838863B CN101838863B CN 201010162260 CN201010162260A CN101838863B CN 101838863 B CN101838863 B CN 101838863B CN 201010162260 CN201010162260 CN 201010162260 CN 201010162260 A CN201010162260 A CN 201010162260A CN 101838863 B CN101838863 B CN 101838863B
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Abstract
The invention relates to polysiloxane fibers and a preparation method thereof. The method comprises the steps of: performing polycondensation on alpha, omega-bi-organic radical polysiloxane and an organic silicon resin into a polysiloxane polymer at a certain temperature and under a catalytic action; and performing high-pressure spinning process on the polysiloxane polymer to obtain the polysiloxane fibers. The polysiloxane fibers prepared by the method have the characteristics of good physical and mechanical performance, better elasticity, high temperature resistance, low temperature resistance, water proofing property and air permeability, grease prevention, weathering aging resistance and physiological inertia, recoverability and recyclability, and environment protection.
Description
Technical field:
The invention belongs to the synthetic fiber technical field, particularly a kind of polysiloxane fibers and preparation method thereof.
Background technology:
At present, the synthetic fiber that we commonly use have polypropylene fibre (polypropylene fibre), polyacrylonitrile fibre (acrylic fibers), vinylon (vinylon), polyamide fiber (polyamide fibre), polyethylene terephthalate (terylene) etc., and the base stock of producing synthetic fiber comes from oil.And the resource of oil is limited, and the frequent fluctuation of price is given the unstability of bringing price as the synthetic fiber of textile raw material, can not degrade rapidly and recycle and reuse, also causes the burden of environment.
Polysiloxanes has excellent high and low temperature resistance, weatherability, electric insulating quality and physiology inertia etc.It has silicone oil, and the various forms of silicon rubber and silicones etc. are widely used in Aero-Space, and are electric, building, and industry and the health cares such as automobile mechanical, the every field of daily life, recycling can circulate.Its main raw material is elemental silicon, sodium chloride and methyl alcohol, and wide material sources easily obtain.
Publication number is the production method that the Chinese patent of CN1710162A also discloses a kind of organo silicon polymer synthetic fiber, organosilicon polymer rubber synthetic fiber dosing wherein is the addition-type silicon rubber composition system, the platinum series compound sulphurized catalyst contains S when running into, N, P, during the compound of Sn etc., easily poison and lose catalytic activity, so that composition can't solidify.Spinning appts sprays silk at normal temperatures in its production technology, because this dosing composition still is can flowing liquid at normal temperatures, so before entering heater, easily distortion or fracture, very unaccommodated spray silk production technology, and after solidifying, silk is sprayed in melting more again.
Publication number is the preparation method that the Chinese patent of CN101177595A discloses a kind of moisture curing organic pressure-sensitive gel, use the synthetic organic pressure-sensitive gel of hydroxy—terminated silicone rubbre and nano MQ silicon resin reaction, because the condensation reaction between the hydroxyl is not thorough, so that the organosilicon polymer that produces is not suitable for spinning very strong viscosity is initially arranged.
Summary of the invention:
For the problem that exists in the above organosilicon synthetic fiber production process, the purpose of this invention is to provide a kind of new polysiloxanes hot-melt polymer, and easily spinning manufacturing technique, good spinnability during spinning is difficult for fracture of wire, produces simple.For solving the problems of the technologies described above, adopt following technical scheme:
A kind of hot melt material of polysiloxane fibers is synthetic, its raw material is by α, ω-diorganopolysiloxaneand, organic siliconresin, catalyst, dialkyl siloxane polymer and pigment form, and raw materials used mass ratio is when synthetic: α, and ω-two organic group gathers radical siloxane 10%～78%, organic siliconresin 10%～70%, catalyst 0.01%～10%, dialkyl siloxane polymer 0%～30%, pigment 0%～10%.
Described α, ω-diorganopolysiloxaneand is linear polysiloxanes, its structural formula is as follows:
Wherein, R
1Being the alkyl of 1～6 carbon, can be identical or different, n=1000～50000, R
2Be wherein a kind of of alkoxyl and ammonia alkyl, the best is methoxyl group or aminopropyl.
Organic siliconresin described in the raw material, its averaging unit molecular formula is as follows:
〔R
3SiO
1/2〕
a〔R
2SiO
2/2〕
b〔RSiO
3/2〕
c〔SiO
4/2〕
d
Wherein, R can be identical or different optional substituted any monovalent organic radical group, comprises methyl, phenyl, glycidol ether propyl group, aminopropyl, the organic groups such as trifluoro propyl, (a+b+c)/d=0.4～4.0, a/b/c/d=0.1～1.5/0～0.5/0.1～2.0/1.Organic siliconresin and α, ω-diorganopolysiloxaneand carries out polycondensation reaction, generates high molecular, the polymer with certain network structure.α, ω-dimethoxy polysiloxanes or α, ω-two aminopropyl polysiloxanes has preferably reactivity, and with the polycondensation reaction that Si-OH on the silicones carries out, speed is faster, reacts more thorough.
The viscosity of described dialkyl siloxane polymer is 50～500000mm
2/ s, its structural formula is as follows:
Wherein, R
1Being the alkyl of 1～6 carbon, can be identical or different, comprising: methyl, ethyl, phenyl etc.Dialkyl siloxane polymer plays adjusting viscosity and increases mobile effect, is beneficial to carrying out smoothly of spinning.
Described catalyst is the catalyst for the polycondensation synthetic reaction, can accelerate condensation reaction speed, is mainly to contain ammonia (amine) based compound, and boric acid ester compound, comprise ammonia, monoethanolamine, aminopropyl triethoxysilane, aminopropyl methyldiethoxysilane, triproylborate etc.
The present invention also provides a kind of preparation method of polysiloxane fibers, prepares first the heat molten type polysiloxane polymer, then hot-melt polymer is carried out spinning, and the preparation method comprises the steps:
The preparation of step 1, heat molten type polysiloxane polymer:
With α, ω-diorganopolysiloxaneand, organic siliconresin and catalyst successively join the powerful mixing device, add after the available alkane solvents dilution in case of necessity, heat to 90 ℃～220 ℃, kept 1 hour～12 hours, carry out polycondensation reaction, then vacuumize and remove low molecule and solvent, or add dialkyl siloxane polymer and pigment, mixed 0.5 hour～5 hours.Start the screw rod material discharging machine, send into screw extruder by utilidor.
Step 2, melt spinning:
Screw extruder is sent into the polysiloxane polymer of melting and is carried out spinning in the spinning manifold, oils by oil pump through blowing the crosswind cooling forming.
Step 3, coiling and molding:
Fiber obtained above is namely got the polysiloxane fibers finished product by the winding head coiling and molding.
The fusion point of the heat molten type polysiloxane polymer described in the above technical scheme is 130 ℃～200 ℃, used powerful mixing device, to be equipped with 2 or a plurality of strong stirring oar, can carry out mixing of high viscosity materials matter, this device has the heating and cooling function, and at least with a screw rod discharge device, one can water-oil separating reflux condenser and one can remove low molecular condenser.The screw rod discharge device can be sent into screw extruder from intensive mixer with reacted product, carries out follow-up spinning operation.Moisture and solvent separated the backflow of solvent when reflux condenser can keep reacting.
Screw extruder and extruder head, pipeline and spinning manifold all adopt the high temperature heat conductive oil insulation, and the conduction oil temperature is 150 ℃～240 ℃, guarantee that polymer is in the flowability of device interior.The temperature of the lateral blowing of spinning cooling is 15 ℃～35 ℃.
The present invention compares with traditional synthetic fiber, has the following advantages:
1, polysiloxane fibers has waterproof and breathable, and is grease proofing, anti-ultraviolet ageing, and good weatherability, harmless.
2, basic material source easily can cycling and reutilization, and energy-conserving and environment-protective do not rely on oil.
3, fusing point is lower, and energy consumption is low, easily spinning, and production technology is simple.
The specific embodiment:
The below enumerates embodiment, further specifically describes the present invention.
Embodiment 1:
With about 500,000 the α of weight average molecular weight, ω-dimethoxy dimethyl silicone polymer 100kg joins in the 500L three axle banburies methyl silicon resin ((CH
3)
3SiO
1/2)
0.6(CH
3SiO
3/2)
0.1(SiO
4/2)
190kg dissolves rear with toluene and the 1kg aminopropyl triethoxysilane adds together, heat to 140 ℃, keep backflow in 3 hours, carry out polycondensation reaction, then being warming up to 185 ℃ vacuumizes and removes low molecule, moisture and solvent add 10000mpa.s dimethyl silicone polymer 5kg as required, mix 1 hour.The holding temperature of setting conduction oil is 220 ℃, starts the screw rod material discharging machine, sends into screw extruder by utilidor.Screw extruder is sent into polymer and is carried out spinning in the spinning manifold, through blowing the crosswind cooling forming by the oil pump coiling and molding that oils.
Embodiment 2:
With about 350,000 the α of weight average molecular weight, ω-dimethoxy dimethyl silicone polymer 100kg joins in the 500L three axle banburies methyl phenyl silicone resin (CH
3SiO
1/2)
0.4(C
6H
5SiO
3/2)
0.2(SiO
4/2)
180kg and 2kg aminopropyl methyldiethoxysilane add together, heat to 130 ℃, keep backflow in 4 hours, carry out polycondensation reaction, then being warming up to 190 ℃ vacuumizes and removes low molecule, moisture and solvent add 50000mpa.s dimethyl silicone polymer 10kg as required, mix 1.5 hours.The holding temperature of setting conduction oil is 200 ℃, starts the screw rod material discharging machine, sends into screw extruder by utilidor.Screw extruder is sent into polymer and is carried out spinning in the spinning manifold, through blowing the crosswind cooling forming by the oil pump coiling and molding that oils.
Embodiment 3:
With about 700,000 the α of weight average molecular weight, ω two aminopropyl dimethyl silicone polymer 120kg join in the 500L three axle banburies ((CH
3)
3SiO
1/2)
0.2((CH
3)
2SiO
2/2)
0.3(CH
3SiO
3/2)
0.2(SiO
4/2)
1Methyl silicon resin 100kg dissolves rear with toluene and the 0.05kg triproylborate adds together, heat to 140 ℃, keep backflow in 3 hours, carry out polycondensation reaction, then being warming up to 190 ℃ vacuumizes and removes low molecule, moisture and solvent add 10000mpa.s dimethyl silicone polymer 10kg as required, mix 1 hour.Other are with embodiment 1.
Embodiment 4:
With about 500,000 the α of weight average molecular weight, ω-two aminopropyl dimethyl silicone polymer 100kg joins in the 500L three axle banburies methyl silicon resin ((CH
3)
3SiO
1/2)
0.4(CH
3SiO
3/2)
0.4(SiO
4/2)
185kg dissolves rear with toluene and the 0.04kg triproylborate adds together, heat to 140 ℃, keep backflow in 3 hours, carry out polycondensation reaction, then be warming up to 185 ℃ and vacuumize and remove low molecule, moisture and solvent add 50000mpa.s dimethyl silicone polymer 5kg as required, Chinese white 2kg mixed 1 hour.Other are with embodiment 1.
The result:
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Fusing point (℃) | 185 | 160 | 165 | 170 |
| Fiber number (dtex) | 9.8 | 8.6 | 7.8 | 9.0 |
| Denier irregularity (%) | 2.5 | 3.0 | 2.8 | 2.7 |
| Fracture strength (cN/dtex) | 7 | 5.2 | 3 | 3.5 |
| Elongation at break (%) | 90 | 95 | 80 | 70 |
The above only is better embodiment of the present invention, therefore all equivalences of doing according to the described structure of patent claim of the present invention, feature and principle change or modify, is included in the patent claim of the present invention.
Claims (8)
1. polysiloxane fibers is characterized in that: the raw material of synthetic polysiloxane fibers is comprised of the material of following mass percent:
α, ω-diorganopolysiloxaneand 10%～78%
Organic siliconresin 10%～70%
Catalyst 0.01%～10%
Dialkyl siloxane polymer 0%～30%
Pigment 0%～10%
Wherein, α in the raw material, ω-diorganopolysiloxaneand, its structural formula is as follows:
Wherein, R
1Being the alkyl of 1～6 carbon, can be identical or different, n=1000～50000, R
2Wherein a kind of for alkoxyl and ammonia alkyl;
Organic siliconresin in the described raw material, its averaging unit molecular formula is as follows:
〔R
3 Si O
1/2〕
a〔R
2Si O
2/2〕
b〔R Si O
3/2〕
c〔Si O
4/2〕
d
Wherein, R can be identical or different optional substituted any monovalent organic radical group, (a+b+c)/d=0.4 ~ 4.0, a/b/c/d=0.1 ~ 1.5/0 ~ 0.5/0.1 ~ 2.0/1.
2. a kind of polysiloxane fibers according to claim 1, it is characterized in that: the viscosity of the dialkyl siloxane polymer of described raw material is 50～500000mm
2/ s, its structural formula is as follows:
Wherein, R
1Being the alkyl of 1～6 carbon, can be identical or different.
3. a kind of polysiloxane fibers according to claim 1, it is characterized in that: catalyst is for containing amino-compound, boric acid ester compound in the described raw material.
4. the preparation method of a polysiloxane fibers claimed in claim 1, it is characterized in that: the preparation method may further comprise the steps:
The preparation of step 1, heat molten type polysiloxane polymer: with α, ω-diorganopolysiloxaneand, organic siliconresin and catalyst successively join the powerful mixing device, add after the available alkane solvents dilution, heat to 90 ℃～220 ℃, kept 1 hour～12 hours, and carried out polycondensation reaction, then vacuumize and remove low molecule and solvent, add dialkyl siloxane polymer and pigment, mixed 0.5 hour～5 hours, and started the screw rod material discharging machine, send into screw extruder by utilidor;
Step 2, melt spinning: screw extruder is sent into the polysiloxane polymer of melting and is carried out spinning in the spinning manifold, oils after blowing the crosswind cooling forming;
Step 3, coiling and molding: fiber obtained above is namely got the polysiloxane fibers finished product by the winding head coiling and molding.
5. a kind of polysiloxane fibers preparation method according to claim 4 is characterized in that: prepared heat molten type polysiloxane polymer is used for a kind of manufacturing of synthetic fiber in the step 1, and its fusion point is 130 ℃～200 ℃.
6. a kind of polysiloxane fibers preparation method according to claim 4, it is characterized in that: used powerful mixing device in the step 1, to be equipped with 2 or a plurality of strong stirring oar, equipment with heating and cooling function, and at least with a screw rod discharge device, one can water-oil separating reflux condenser and one can remove low molecular condenser.
7. a kind of polysiloxane fibers preparation method according to claim 4, it is characterized in that: the temperature of the lateral blowing described in the step 2 is 15 ℃～35 ℃.
8. a kind of polysiloxane fibers preparation method according to claim 4 is characterized in that: the screw extruder described in the step 2 and extruder head, pipeline and spinning manifold all adopt the high temperature heat conductive oil insulation, and the conduction oil temperature is 150 ℃～240 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010162260 CN101838863B (en) | 2010-04-27 | 2010-04-27 | Polysiloxane fibers and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010162260 CN101838863B (en) | 2010-04-27 | 2010-04-27 | Polysiloxane fibers and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101838863A CN101838863A (en) | 2010-09-22 |
| CN101838863B true CN101838863B (en) | 2013-04-10 |
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|---|---|---|---|
| CN 201010162260 Active CN101838863B (en) | 2010-04-27 | 2010-04-27 | Polysiloxane fibers and preparation method thereof |
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| CN104550308B (en) * | 2013-10-25 | 2017-08-25 | 中国石油化工股份有限公司 | A kind of preparation method of ultrafine metal fibers and its ultrafine metal fibers of preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3907954A (en) * | 1971-02-12 | 1975-09-23 | Bayer Ag | Production of fibers containing silicon-oxygen bonds |
| US4094690A (en) * | 1972-08-07 | 1978-06-13 | Imperial Chemical Industries Limited | Liquid composition |
| DE3607288A1 (en) * | 1986-03-06 | 1987-09-10 | Bayer Ag | MIXTURES OF POLYCARBONATE POLYSILOXANE BLOCK COCONDENSATES AND THERMOTROPENE POLYMERS, METHOD FOR THE PRODUCTION THEREOF AND THEIR USE FOR THE PRODUCTION OF MOLDED BODIES, FILAMENTS, FIBERS AND FILMS |
| JPH0959517A (en) * | 1995-06-12 | 1997-03-04 | Fuji Syst Kk | Silicone rubber composition, hollow fiber using the same composition and production of the same hollow fiber |
| JPH09286920A (en) * | 1996-04-24 | 1997-11-04 | Fuji Syst Kk | Silicon rubber hollow fiber and its production |
| CN1314847C (en) * | 2005-06-03 | 2007-05-09 | 田文新 | Organo silicon polymer synthetic fiber and its production process |
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Effective date of registration: 20150522 Address after: 215550, Jiangsu, Changshu province Suzhou Economic Development Zone, East Zhou Road No. 12, Suzhou city high polymer materials Co., Ltd. Patentee after: Dongguan Betely New Materials Co., Ltd. Address before: 215550, Jiangsu, Changshu province Suzhou Economic Development Zone, East Zhou Road No. 12, Suzhou city high polymer materials Co., Ltd. Patentee before: Dongguan Betely New Materials Co., Ltd. Patentee before: Beiteli New Material Co., Ltd., Dongguan City |
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Address after: 215550, Jiangsu, Changshu province Suzhou Economic Development Zone, East Zhou Road No. 12, Suzhou city high polymer materials Co., Ltd. Patentee after: SUZHOU BEITELI POLYMER MATERIALS CO., LTD. Address before: 215550, Jiangsu, Changshu province Suzhou Economic Development Zone, East Zhou Road No. 12, Suzhou city high polymer materials Co., Ltd. Patentee before: Dongguan Betely New Materials Co., Ltd. |