CN101660219A - Preparation method of acrylic fiber and polybutylene succinate parallel fiber - Google Patents
Preparation method of acrylic fiber and polybutylene succinate parallel fiber Download PDFInfo
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- CN101660219A CN101660219A CN200910144628A CN200910144628A CN101660219A CN 101660219 A CN101660219 A CN 101660219A CN 200910144628 A CN200910144628 A CN 200910144628A CN 200910144628 A CN200910144628 A CN 200910144628A CN 101660219 A CN101660219 A CN 101660219A
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- China
- Prior art keywords
- temperature
- fiber
- butanediol
- consumption
- acrylic fibers
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000835 fiber Substances 0.000 title claims abstract description 22
- 229920002972 Acrylic fiber Polymers 0.000 title claims abstract description 19
- -1 polybutylene succinate Polymers 0.000 title claims abstract description 18
- 229920002961 polybutylene succinate Polymers 0.000 title claims abstract description 18
- 239000004631 polybutylene succinate Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000009987 spinning Methods 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 21
- 230000032050 esterification Effects 0.000 claims description 13
- 238000005886 esterification reaction Methods 0.000 claims description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000009998 heat setting Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000003063 flame retardant Substances 0.000 claims description 8
- 239000003381 stabilizer Substances 0.000 claims description 8
- 230000002146 bilateral effect Effects 0.000 claims description 7
- 238000006068 polycondensation reaction Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 5
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- 239000001119 stannous chloride Substances 0.000 claims description 4
- 235000011150 stannous chloride Nutrition 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 238000002074 melt spinning Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 claims description 3
- HMENQNSSJFLQOP-UHFFFAOYSA-N 2-bromoprop-2-enoic acid Chemical compound OC(=O)C(Br)=C HMENQNSSJFLQOP-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 229920000728 polyester Polymers 0.000 description 6
- 239000004753 textile Substances 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 2
- 206010023126 Jaundice Diseases 0.000 description 1
- YMOONIIMQBGTDU-VOTSOKGWSA-N [(e)-2-bromoethenyl]benzene Chemical compound Br\C=C\C1=CC=CC=C1 YMOONIIMQBGTDU-VOTSOKGWSA-N 0.000 description 1
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical group CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
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- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
A preparation method of acrylic fiber and poly butylene succinate parallel fiber is characterized by comprising the following steps: the invention is a method for preparing polybutylene succinate through chemical polymerization, then spinning together with acrylic fibers, respectively melting two different polymers during spinning, and extruding and combining the two polymers into a parallel bicomponent fiber through a spinneret plate at the last moment.
Description
Technical field
The present invention relates to the fiber production field, the preparation method of particularly a kind of acrylic fibers and olybuthylenesuccinatcollateral collateral fiber.
Background technology
The kind of biodegradable fiber is various day by day, numerous areas such as that its application relates to is medical, take, fishery, building, health, decoration, industrial treatment.Aliphatic polyester is a class important in the degradable polyester, poly butylene succinate wherein, fusing point is 115 ℃, good stability, be difficult at room temperature decomposing, mechanical property is good, has the possibility of processed and applied, is the focus of present degradable polyester research, domestic synthetic poly butylene succinate molecular weight is lower at present, the color jaundice is applied in the plastics field more, and the application of poly-succinic acid-butanediol is also seldom seen in field of textiles.
Summary of the invention
In order to develop the application at field of textiles of poly butylene succinate, select acrylic fibers and poly butylene succinate cospinning, the fiber that obtains having fluffy performance.
The present invention relates to the preparation method of a kind of acrylic fibers and olybuthylenesuccinatcollateral collateral fiber, the poly butylene succinate that obtains by chemical polymerization, then with the common spinning of acrylic fibers, two kinds of different polymer fusions are respectively separately extruded by spinnerets at the eleventh hour and are combined into the parallel type bicomponent fibers during spinning.
The preparation of poly-succinic succinate: raw material is butanediol and succinic acid, adding mol ratio is 1.10～1.15, catalyst is toluene sulfonic acide and stannous chloride, polyester synthetic mainly contains esterification and two steps of polycondensation finish, esterification is finished by normal pressure and two esterifying kettles of decompression in the continuous polymerization technique, and polycondensation reaction is finished by precondensation and poly-two stills of final minification.
The synthesis technique of poly butylene succinate:
| Condition | Esterification I | Esterification II | Precondensation | Final minification is poly- |
| Reaction temperature/℃ | ??140～150 | ??150～160 | ??230～240 | ??230～240 |
| Reaction pressure/Pa | ??(1.3～1.5)×10 5 | ??60000～70000 | ??2500～3000 | ??50～100 |
| The time of staying/min | ??60～90 | ??60～90 | ??50～70 | ??120～150 |
The density of the acrylic fibers section of buying is 1.17g/cm3, form and aspect L value 〉=90, moisture≤0.15%.
Poly butylene succinate will add catalyst, delustering agent, stabilizing agent, synergist and fire retardant in synthetic, the addition of catalyst toluene sulfonic acide is 100 * 10 of a butanediol amount
-6, the addition of stannous chloride is 400 * 10 of a butanediol amount
-6The consumption of delustering agent silica is 3 of butanediol amount～5 ‰, the consumption of stabilizing agent phosphoric acid is 3 of butanediol amount～5 ‰, the consumption of fire retardant bromoacrylic acid is 5 of butanediol amount～8 ‰, the consumption of synergist sodium antimonate is 1 of butanediol amount～3 ‰, catalyst and polymer raw enter esterification together, and delustering agent, stabilizing agent, synergist and fire retardant then add in the final stage of polycondensation reaction.
When the preparation bilateral fibre, acrylic fibers and poly butylene succinate are from ester fusion respectively, last moment before extruding, two kinds of polyester fondants entered manifold, by regulating the separating element in the manifold and the relation of spinnerets, can obtaining the shared mass ratio of acrylic fibers is dissimilar bilateral fibres such as 30～35%, 35～40%, 40～45%, 45～50%.
Two-component polymer just be spun into behind the silk successively through one stretching, HEAT SETTING, two roads stretch, curl, HEAT SETTING, cut-out operation system.The draft temperature of melt spinning is 200 ℃, and spinning speed is 1000～2000m/min, and the draw ratio that stretches is 2.5～3.5 together, and draft temperature is 110 ℃, and heat setting temperature is at 90～100 ℃; The draw ratio that two roads stretch is 1.15～1.50, and draft temperature is 100 ℃, and curling temperature is 70～80 ℃, through HEAT SETTING fiber temperature is reached below 45 ℃ again, cuts off.
Progressive meaning of the present invention is:
Utilize the bilateral fibre with the preparation of acrylic fibers cospinning, fiber tool softness, bulk, easily dye, bright in colour, fast light, anti-microbial property, expanded the application at field of textiles of poly butylene succinate.
The specific embodiment
The preparation method of a kind of acrylic fibers and olybuthylenesuccinatcollateral collateral fiber, the poly butylene succinate that obtains by chemical polymerization, then with the common spinning of acrylic fibers, two kinds of different polymer fusions are respectively separately extruded by spinnerets at the eleventh hour and are combined into the parallel type bicomponent fibers during spinning.
Embodiment
1. the preparation of poly-succinic succinate: raw material is butanediol and succinic acid, adding mol ratio is 1.11, catalyst is p-methyl benzenesulfonic acid and butyl titanate, polyester synthetic mainly contains esterification and two steps of polycondensation finish, esterification is finished by normal pressure and two esterifying kettles of decompression in the continuous polymerization technique, and polycondensation reaction is finished by precondensation and poly-two stills of final minification.
The synthesis technique of poly butylene succinate:
| Condition | Esterification I | Esterification II | Precondensation | Final minification is poly- |
| Reaction temperature/℃ | ??140～150 | ??150～160 | ??230～240 | ??230～240 |
| Reaction pressure/Pa | ??1.3×10 5 | ??65000 | ??2800 | ??70 |
| The time of staying/min | ??70 | ??70 | ??60 | ??130 |
2. poly butylene succinate will add catalyst, delustering agent, stabilizing agent, synergist and fire retardant in synthetic, and the addition of catalyst toluene sulfonic acide is 100 * 10 of a butanediol amount
-6, the addition of stannous chloride is 400 * 10 of a butanediol amount
-6The consumption of delustering agent silica is 4 ‰ of a butanediol amount, the consumption of stabilizing agent trimethyl phosphate is 4 ‰ of a butanediol amount, the consumption of fire retardant bromostyrene is 4 ‰ of a butanediol amount, the consumption of synergist sodium antimonate is 2 ‰ of a butanediol amount, catalyst and polymer raw enter esterification together, and delustering agent, stabilizing agent, synergist and fire retardant then add in the final stage of polycondensation reaction.
3. when the preparation bilateral fibre, acrylic fibers and poly butylene succinate are from ester fusion respectively, last moment before extruding, two kinds of polyester fondants entered manifold, by regulating the separating element in the manifold and the relation of spinnerets, can obtaining the shared mass ratio of acrylic fibers is dissimilar bilateral fibres such as 30～35%, 35～40%, 40～45%, 45～50%.
Two-component polymer just be spun into behind the silk successively through one stretching, HEAT SETTING, two roads stretch, curl, HEAT SETTING, cut-out operation system.The draft temperature of melt spinning is 200 ℃, and spinning speed is 1800m/min, and the draw ratio that stretches is 2.6 together, and draft temperature is 110 ℃, and heat setting temperature is at 90～100 ℃; The draw ratio that two roads stretch is 1.30, and draft temperature is 100 ℃, and curling temperature is 70～80 ℃, through HEAT SETTING fiber temperature is reached below 45 ℃ again, cuts off.
5. Zhi Bei bilateral fibre, fiber tool softness, bulk, easily dye, bright in colour, fast light, anti-microbial property.
Claims (2)
1. the preparation method of acrylic fibers and olybuthylenesuccinatcollateral collateral fiber is characterized in that:
The poly butylene succinate that obtains by chemical polymerization at first, raw material is butanediol and succinic acid, adding mol ratio is 1.10～1.15, the synthesis technique of poly butylene succinate:
Wherein the addition of catalyst toluene sulfonic acide is 100 * 10 of a butanediol amount
-6, the addition of stannous chloride is 400 * 10 of a butanediol amount
-6The consumption of delustering agent silica is 3 of butanediol amount～5 ‰, the consumption of stabilizing agent phosphoric acid is 3 of butanediol amount～5 ‰, the consumption of fire retardant bromoacrylic acid is 5 of butanediol amount～8 ‰, the consumption of synergist sodium antimonate is 1 of butanediol amount～3 ‰, catalyst and polymer raw enter esterification together, and delustering agent, stabilizing agent, synergist and fire retardant then add in the final stage of polycondensation reaction;
Then with the common spinning of acrylic fibers, two kinds of different polymer fusions respectively separately during spinning, extrude by spinnerets at the eleventh hour and be combined into the parallel type bicomponent fibers, the draft temperature of melt spinning is 200 ℃, spinning speed is 1000～2000m/min, the draw ratio that stretches is 2.5～3.5 together, and draft temperature is 110 ℃, and heat setting temperature is at 90～100 ℃; The draw ratio that two roads stretch is 1.15～1.50, and draft temperature is 100 ℃, and curling temperature is 70～80 ℃, through HEAT SETTING fiber temperature is reached below 45 ℃ again, cuts off.
2. according to claim 1, it is characterized in that: by regulating the separating element in the manifold and the relation of spinnerets, can obtaining the shared mass ratio of acrylic fibers is dissimilar bilateral fibres such as 30～35%, 35～40%, 40～45%, 45～50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101446288A CN101660219B (en) | 2009-08-24 | 2009-08-24 | Preparation method of acrylon and olybuthylenesuccinate collateral fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101446288A CN101660219B (en) | 2009-08-24 | 2009-08-24 | Preparation method of acrylon and olybuthylenesuccinate collateral fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101660219A true CN101660219A (en) | 2010-03-03 |
| CN101660219B CN101660219B (en) | 2011-07-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101446288A Expired - Fee Related CN101660219B (en) | 2009-08-24 | 2009-08-24 | Preparation method of acrylon and olybuthylenesuccinate collateral fiber |
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| Country | Link |
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| CN (1) | CN101660219B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437429A (en) * | 2018-05-02 | 2019-11-12 | 中国石油化工股份有限公司 | A kind of preparation method of modified poly ester and preparation method thereof and its film |
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2009
- 2009-08-24 CN CN2009101446288A patent/CN101660219B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437429A (en) * | 2018-05-02 | 2019-11-12 | 中国石油化工股份有限公司 | A kind of preparation method of modified poly ester and preparation method thereof and its film |
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| Publication number | Publication date |
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| CN101660219B (en) | 2011-07-20 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
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Granted publication date: 20110720 Termination date: 20130824 |