CN100395385C - Preparation method of lyocell fiber used for cord thread - Google Patents
Preparation method of lyocell fiber used for cord thread Download PDFInfo
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- CN100395385C CN100395385C CNB2005101104013A CN200510110401A CN100395385C CN 100395385 C CN100395385 C CN 100395385C CN B2005101104013 A CNB2005101104013 A CN B2005101104013A CN 200510110401 A CN200510110401 A CN 200510110401A CN 100395385 C CN100395385 C CN 100395385C
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Abstract
The present invention relates to a preparation method of Lyocell fibres for cord threads in chemical fibre production, which comprises following steps: mixing dry pulp of which the polymerization degrees are from 1000 to 1450 and from 600 to 850 by the weight ratio of 100: 0 to 50; adding the mixed pulp and concentrated aqueous solutions of N-methylmorpholines-N-oxide into a dissolving device by the weight ratio of 5: 110 to 10: 105, after static swelling and strong stirring at the temperature of 70 DEG C to 110 DEG C, heating up to the temperature of 80DEG C to 125 DEG C; stirring and executing reduced pressure distillation until the water content of the aqueous solutions of N-methylmorpholines-N-oxide in systems reaches 12% to 14%, and then gaining brown transparent spinning stock solutions; solidifying the stock solutions into fibres through a dry-wet spinning method; leading the fibres in a multistage leaching roller; leaching for 2 to 20 minutes by water; finally, winding into bobbins after continuously drying at the temperature of 80DEG C to 160 DEG C under the tension of 0 to 1.0 cN/tax. The Lyocell fibres produced by the method have the advantages of large strength, high modulus, low elongation and low thermal shrinkage, which can be used as novel cord threads with good quality.
Description
Technical field
The present invention relates to the preparation method of tire cord in the chemical fibre industry, be meant that especially employing N-methylmorpholine-N-oxide (NMMO) aqueous solution is the technology that solvent spins Lyocell (Lyocell) fiber as cord fabric thread.
Background technology
Cord fabric thread is to make the required a kind of important framework material of tire, itself and rubber adhesion can be improved together the intensity and the DIMENSIONAL STABILITY of rubber tyre.As the skeleton structure material of tire, cord fabric thread must have following physical property: 1) intensity and elastic modelling quantity height; 2) good heat resistance, damp and hot and xeothermic being difficult for down degrades; 3) fatigue durability is good; 4) DIMENSIONAL STABILITY is good; 5) cohesiveness with rubber is good.At present, the material as cord fabric thread mainly contains regenerated celulose fibre (being viscose), polyester fiber, polyamide fibre, aromatic polyamide fibre, glass fibre and the steel wire of being produced by traditional adhering process etc.These materials are used for cord fabric thread to have carried out a large amount of research and has formed many patents, and the patent that wherein relates to the viscose glue cord fabric thread has GB756709, US2626887, US3282039, CN1180334 etc.
The viscose glue cord fabric thread is the cord fabric thread that is applied to rubber industry the earliest, have that fracture strength and modulus are higher, good heat resistance, hardly exist xeothermic contraction, DIMENSIONAL STABILITY is splendid, raw material is easy to get, with advantages such as rubber adhesion is good, be the good framework material of manufacturing exotic performance car radial.But it is, also more and more higher to the requirement of cord fabric thread along with the needs of the development and the scorch of automotive engineering.Because being adhering process, traditional regenerated celulose fibre production technology can only use the cellulose pulp of the degree of polymerization lower (general DP is 500～800) as raw material, the especially dried wet modulus of the mechanical property of gained viscose glue cord fabric thread is all not high enough, still can not satisfy the requirement of high-performance tire.In addition, the production technology of viscose has been used corrosive substances such as a large amount of alkali and acid, and can emit toxic gas and zinc-containing waters such as carbon disulfide and hydrogen sulfide in process of production, environmental pollution is more serious, and technological process is long, energy consumption is high, causes its development as cord fabric thread to be subjected to certain restriction.
The Lyocell fiber is a kind of new type of regenerated cellulose fibers and features, and it is cellulose pulp directly to be dissolved in nontoxic N-methylmorpholine-N-oxide (NMMO) aqueous solution form cellulose solution, makes by dry-wet spinning then.Some characteristics such as with traditional regenerated celulose fibre is that viscose is compared, and the Lyocell fiber has intensity and modulus is higher, elongation is little, DIMENSIONAL STABILITY good, heat resistance is good, production technology is environmentally friendly.In addition, the Lyocell fibre technology can directly adopt the cellulose pulp of the degree of polymerization higher (as DP＞1000) to carry out spinning, and this is that adhering process is beyond one's reach.Existing result of study shows that the Lyocell fibrous mechanical property of the cellulose spinning of high polymerization degree can significantly improve, and especially modulus can significantly improve.Therefore, the Lyocell fiber is expected to as a kind of high-performance tire cord fabric thread tencel cellulose fiber.
The patent that at present relevant Lyocell fiber is used for cord fabric thread is few, wherein EP1433881-A2, JP2004211277-A, US2004126577-A1, CA2438445-A1, CN1511980-A, KR2004057550-A, US6852413-B2, the US2005079348-A1 of the applications such as LEE T of Korea S disclose a kind of Lyocell multifilament and manufacture method thereof that is used for cotton tyre cord, it is that the mixed-powder of dissolving cellulos and polyvinyl alcohol in NMMO solution is with the preparation spinning solution, then by the Lyocell multifilament of dry-wet spinning preparation as cord fabric thread.Because employed NMMO solvent cost an arm and a leg during Lyocell produced, need recycling use in the production.But this method has also been added polyvinyl alcohol except that cellulosic material, and the polyvinyl alcohol of these addings is along with the carrying out of spinning, and a part can accumulate in coagulating bath gradually, and this will cause difficulty to the recovery of NMMO solvent in the coagulating bath.In addition, the EP1493850-A1 of application such as the KWON I of Korea S, JP2005023508-A, US2005066646-A1 discloses a kind of method for preparing the cellulose cord fabric thread from cellulose/NMMO solution, this method is earlier cellulose dissolution to be formed 0.01～3% initial soln in NMMO, the solidification temperature of NMMO solution is descended, and then more cellulose dissolution obtained Lyocell fiber as cord fabric thread by dry-wet spinning in this initial soln, this patent adopts two step dissolution process to produce the Lyocell fiber, increased the complexity of technology, and it is not applied for a patent in China.
The present invention proposes with adding the cellulose pulp of a certain proportion of middle high molecular weight (degree of polymerization 600～850) in the cellulose pulp of high molecular weight (degree of polymerization 1000～1450) as raw material, and adopt distinctive swelling-dissolution process to prepare spinnability spinning solution preferably, the mechanical property such as intensity, modulus of the Lyocell cord fabric thread of spinning is significantly improved.This law be with pure cellulose pulp as raw material, do not add other raw materials, this not only makes cord fabric thread simpler with the preparation technology of Lyocell fiber, and makes the recovery of solvent NMMO also very convenient, thereby can reduce production costs greatly.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who is used for the Lyocell fibers of cord fabric thread.
For addressing this problem, adopt following technical scheme:
1. be that 1000～1450 the high molecular weight and the degree of polymerization are the cellulose pulp of 600～850 medium relative molecular mass with the degree of polymerization, be cut to the small pieces of 0.5～4cm * 0.5～4cm respectively, with these small pieces desiccated balance 6～12 hours under reduced pressure, making its moisture content is 2～4% then;
With N-methylmorpholine-N-oxide (NMMO) aqueous solution inspissation to moisture under reduced pressure is 24～28%.
With in above-mentioned 1 the degree of polymerization of desiccated balance be respectively 1000～1450 and 600～850 pulp and mix with 100: 100/11～50 weight ratio, to mix in pulp and above-mentioned 1 the NMMO aqueous solution of inspissation then adds in the dissolver with 5: 110～10: 105 weight ratio, after stirring through the brute force of the quiet swelling of 20～40min, 20～60min under 70～110 ℃, be warming up to 80～125 ℃ again, through stir, decompression distillation moisture of the NMMO aqueous solution to the system is 12%～14%, promptly forms brown transparent Lyocell fiber spinning dope.
3. above-mentioned 2 resulting spinning solutions are sprayed by spinnerets, behind the air gap by 5～300mm (being the air layer between spinnerets surface and the coagulating bath face), enter weight percent concentration and be solidificating fiber in 0～20% the NMMO aqueous solution.
4. above-mentioned 3 gained fibers are imported multistage drip washing roller, and with water wash 2～20 minutes.
With the fiber of the drip washing of above-mentioned 4 gained under the tension force of 0～1.0cN/dtex, behind 80～160 ℃ continuous drying, be wound into bobbin.
Advantage of the present invention is that the cellulose pulp of employing high molecular weight (degree of polymerization 1000～1450) is a body material, and the mechanical property of the Lyocell fiber of spinning is significantly improved; And the method that adopts the cellulose pulp that adds a certain proportion of medium relative molecular mass (degree of polymerization 600～850) is beneficial to improve the spinnability of high polymerization degree cellulose spinning fluid; The used solvent N-methylmorpholine-N-oxide (NMMO) of the present invention has nontoxic and characteristics such as rate of recovery height, and is environmentally friendly; The present invention is a raw material with pure cellulose pulp, does not add other auxiliary material, and adopts distinctive swelling-dissolution process, makes the preparation of spinning solution, the production and the simple more advanced person of NMMO solvent recovery process of Lyocell cord fabric thread; The Lyocell fibre strength and the modulus height of the present invention preparation, DIMENSIONAL STABILITY is good, heat resistance is good, can be used as good tire cord, has opened up the Application Areas of Lyocell fiber.
The specific embodiment
Embodiment 1
The degree of polymerization is respectively 1418 and 823 cellulose pulp and is cut to the small pieces of 2cm * 2cm with the pulp shredding machine, with these small pieces in vacuum-9 * 10
4It is 2% that Pa and 50 ℃ of following desiccated balances made its moisture content in 10 hours; With the 65.4kg moisture is that 50% the NMMO aqueous solution distills under reduced pressure, obtains the 44.2kg moisture and be 26% the NMMO aqueous solution.
The 2kg degree of polymerization that dried is crossed is 1418 cellulose pulp with the 0.4kg degree of polymerization is that 823 pulp mixes, and place dissolution kettle with the NMMO aqueous solution of above-mentioned inspissation, after the brute force of 100 ℃ of following quiet swellings through 40min, 40min stirs, be warming up to 110 ℃ again, through stir, decompression distillation moisture of the NMMO aqueous solution to the system is 13%, obtains brown transparent spinning solution.
Spinning solution with gained is sprayed by spinnerets then, be the air gap layer of 7cm by length after, enter weight percent concentration and be solidificating fiber in 10% the NMMO aqueous solution.The gained fiber is imported multistage drip washing roller, and with water wash 15 minutes.
Again with the fiber of drip washing under the tension force of 0.2cN/dtex, be to be wound into bobbin behind 100 ℃ the hot-rolling continuous drying through temperature.
Doing of the Lyocell fiber of gained is that 105.3cN/dtex, extension at break are 7.2% for 6.84cN/dtex, initial modulus (3%) by force.This fiber has good DIMENSIONAL STABILITY, and its boiling water shrinkage is 0.9%, and the fiber heat resistance is splendid, xeothermic contraction＜1.5% under 180 ℃.
Embodiment 2
The degree of polymerization is respectively 1260 and 657 cellulose pulp and is cut to the small pieces of 3cm * 3cm with the pulp shredding machine, with these small pieces in vacuum-9 * 10
4It is 3% that Pa and 50 ℃ of following desiccated balances made its moisture content in 8 hours; With the 62.6kg moisture is that 50% the NMMO aqueous solution distills under reduced pressure, obtains the 43.5kg moisture and be 28% the NMMO aqueous solution.
The 3.3kg degree of polymerization that dried is crossed is 1260 cellulose pulp with the 0.3kg degree of polymerization is that 657 pulp mixes, and place dissolution kettle with the NMMO aqueous solution of above-mentioned inspissation, after the brute force of 80 ℃ of following quiet swellings through 30min, 30min stirs, be warming up to 90 ℃ again, through stir, decompression distillation moisture of the NMMO aqueous solution to the system is 14%, obtains brown transparent spinning solution.
Spinning solution with gained is sprayed by spinnerets then, be the air gap layer of 5cm by length after, enter weight percent concentration and be solidificating fiber in 17% the NMMO aqueous solution.The gained fiber is imported multistage drip washing roller, and with water wash 20 minutes.
Again with the fiber of drip washing under the tension force of 0.5cN/dtex, be to be wound into bobbin behind 140 ℃ the hot-rolling continuous drying through temperature.
Doing of the Lyocell fiber of gained is that 86.2cN/dtex, extension at break are 8.1% for 6.24cN/dtex, initial modulus (3%) by force.This fiber has good DIMENSIONAL STABILITY, and its boiling water shrinkage is 1%, and the fiber heat resistance is also fabulous, xeothermic contraction＜1.5% under 180 ℃.
Embodiment 3
The degree of polymerization is respectively 1130 and 728 cellulose pulp and is cut to the small pieces of 2cm * 2cm with the pulp shredding machine, with these small pieces in vacuum-9 * 10
4It is 2% that Pa and 50 ℃ of following desiccated balances made its moisture content in 6 hours; With the 64.8kg moisture is that 50% the NMMO aqueous solution distills under reduced pressure, obtains the 42.6kg moisture and be 24% the NMMO aqueous solution.
The 2.3kg degree of polymerization that dried is crossed is 1130 cellulose pulp with the 0.9kg degree of polymerization is that 728 pulp mixes, and place dissolution kettle with the NMMO aqueous solution of above-mentioned inspissation, after the brute force of 93 ℃ of following quiet swellings through 20min, 50min stirs, be warming up to 100 ℃ again, through stir, decompression distillation moisture of the NMMO aqueous solution to the system is 12%, obtains brown transparent spinning solution.
Spinning solution with gained is sprayed by spinnerets then, be the air gap layer of 5cm by length after, enter solidificating fiber in the pure water solution.The gained fiber is imported multistage drip washing roller, and with water wash 8 minutes.
Again with the fiber of drip washing under the tension force of 0.8cN/dtex, be to be wound into bobbin behind 120 ℃ the hot-rolling continuous drying through temperature.
Doing of the Lyocell fiber of gained is that 71.6cN/dtex, extension at break are 8.5% for 6.05cN/dtex, initial modulus (3%) by force.This fiber has good DIMENSIONAL STABILITY, and its boiling water shrinkage is 1%, and the fiber heat resistance is also fabulous, xeothermic contraction＜1.5% under 180 ℃.
Claims (6)
1. be used for the preparation method of the Lyocell fibers of cord fabric thread, it is characterized in that:
A) will be the moisture content of desiccated balance be 2～4%, the degree of polymerization is respectively 1000～1450 and 600～850 cellulose pulp and mixes with 100: 100/11～50 weight ratio; To be N-methylmorpholine-N-oxide water solution of 24～28% add in the dissolver with 5: 110～10: 105 weight ratio for said mixture and moisture, after 70～110 ℃ the quiet swelling of process stirs with brute force down, be warming up to 80～125 ℃ again, through stir, decompression distillation moisture of N-methylmorpholine-N-oxide water solution to the system is 12%～14%, promptly forms brown transparent Lyocell fibers spinning solution;
B) with above-mentioned A) the Lyocell fibers spinning solution that obtains sprays by spinnerets, and behind one section air gap, enter weight percent concentration and be in N-methylmorpholine-N-oxide water solution of 0～20% and be frozen into Lyocell fibers;
C) with above-mentioned B) fiber that obtains imports multistage drip washing roller, and with water wash 2～20 minutes;
D) with above-mentioned C) be wound into bobbin behind the Lyocell fibers continuous drying of the drip washing that obtains.
2. the preparation method who is used for the Lyocell fibers of cord fabric thread as claimed in claim 1, it is characterized in that above-mentioned A) described in the degree of polymerization be that 1000～1450 or 600～850 cellulose pulp is the small pieces that are cut to 0.5～4cm * 0.5～4cm, desiccated balance obtained after 6～12 hours under reduced pressure.
3. the preparation method who is used for the Lyocell fibers of cord fabric thread as claimed in claim 1 is characterized in that above-mentioned A) described in N-methylmorpholine-N-oxide water solution be in advance under reduced pressure inspissation to moisture be 24～28%.
4. the preparation method who is used for the Lyocell fibers of cord fabric thread as claimed in claim 1, it is characterized in that above-mentioned A) described in quiet swelling and powerful the stirring be to be N-methylmorpholine-N-oxide water solution of 24～28% quiet swelling 20～40 minutes in dissolver with pulp mixture and moisture, powerful then stirring 20～60 minutes.
5. the preparation method who is used for the Lyocell fibers of cord fabric thread as claimed in claim 1 is characterized in that above-mentioned B) described in the surface and the air gap between the coagulating bath face of spinnerets be 5～300mm.
6. the preparation method who is used for the Lyocell fibers of cord fabric thread as claimed in claim 1 is characterized in that above-mentioned D) described in continuous drying be under the tension force of 0.2～1.0cN/dtex, 80～160 ℃ continuous drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005101104013A CN100395385C (en) | 2005-11-16 | 2005-11-16 | Preparation method of lyocell fiber used for cord thread |
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| CNB2005101104013A CN100395385C (en) | 2005-11-16 | 2005-11-16 | Preparation method of lyocell fiber used for cord thread |
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| CN100395385C true CN100395385C (en) | 2008-06-18 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102317515B (en) * | 2007-08-31 | 2015-06-10 | 可隆工业株式会社 | Preparation method for lyocell filament fibers, lyocell filament fibers, tire cord, and preparation method for tire cord |
| CN101195933B (en) * | 2007-12-06 | 2010-06-09 | 东华大学 | Method for producing Lyocell fibre for tire cord |
| US20130171450A1 (en) * | 2010-08-05 | 2013-07-04 | Cordenka Gmbh & Co. Kg | Cords made of cellulosic multifilament yarns having an increased linear density of individual filaments |
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| GB650896A (en) * | 1948-05-11 | 1951-03-07 | Comptoir Textiles Artificiels | Improvements in or relating to the production of viscose rayon |
| US20020041961A1 (en) * | 1996-08-23 | 2002-04-11 | Weyerhaeuser Company | Process for making a composition for conversion to lyocell fiber from an alkaline pulp having low average degree of polymerization values |
| CN1184364C (en) * | 2001-09-11 | 2005-01-12 | 东华大学 | Prepn process of spinning dope for producing cellulose fibre through solvent process |
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