CN101671863A - Fluorescent poly terephthalic acid 1, 2-propylene glycol ester fiber - Google Patents
Fluorescent poly terephthalic acid 1, 2-propylene glycol ester fiber Download PDFInfo
- Publication number
- CN101671863A CN101671863A CN200910152549A CN200910152549A CN101671863A CN 101671863 A CN101671863 A CN 101671863A CN 200910152549 A CN200910152549 A CN 200910152549A CN 200910152549 A CN200910152549 A CN 200910152549A CN 101671863 A CN101671863 A CN 101671863A
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- Prior art keywords
- propylene glycol
- nano
- acid
- terephthalic acid
- temperature
- 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.)
- Granted
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- 239000000835 fiber Substances 0.000 title claims abstract description 20
- -1 poly terephthalic acid 1, 2-propylene glycol ester Chemical class 0.000 title claims abstract description 6
- 229920000728 polyester Polymers 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002074 melt spinning Methods 0.000 claims abstract description 6
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 48
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Substances CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 28
- 239000003054 catalyst Substances 0.000 claims description 18
- 230000032050 esterification Effects 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 10
- 239000003607 modifier Substances 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- 239000003063 flame retardant Substances 0.000 claims description 6
- 238000009998 heat setting Methods 0.000 claims description 6
- 238000009987 spinning Methods 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 claims description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 4
- GUPWNYUKYICHQX-UHFFFAOYSA-N carbonobromidic acid Chemical compound OC(Br)=O GUPWNYUKYICHQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 210000001170 unmyelinated nerve fiber Anatomy 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- NOJQSZZIXRYAFK-UHFFFAOYSA-N propane-1,2-diol;terephthalic acid Chemical compound CC(O)CO.OC(=O)C1=CC=C(C(O)=O)C=C1 NOJQSZZIXRYAFK-UHFFFAOYSA-N 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 6
- 229920000433 Lyocell Polymers 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
A fluorescent poly terephthalic acid 1, 2-propylene glycol ester fiber is characterized in that: according to the invention, 1-3% of nano-scale titanium dioxide and 1-3% of calcium aluminate are added in the synthesis of polyester to obtain nano modified polyester, and the polyester can be directly subjected to a melt spinning process to obtain the fluorescent poly (1, 2-propylene glycol terephthalate) fiber.
Description
Technical field
The present invention relates to the fiber production field, particularly a kind of fluorescence poly terephthalic acid 1,2-propylene glycol ester fiber.
Background technology
In today that textile technology makes rapid progress, the lining that various tencels are made progressively is applied in the exploitation of weaving face fabric by domestic textile enterprise, and the unique advantage of tencel has brought up functionalization, comfortableization and superior of weaving face fabric.Poly terephthalic acid 1, a kind of as in the tencel of 2-propylene glycol ester fiber just is being subjected to people's attention, continually develops the polyester fiber that makes new advances, poly terephthalic acid 1, the 2-propylene glycol ester can have industrial prospect by the synthetic aliphatic polyester of chemical technology, but also exists the shortcoming of self, fusing point is low, intensity is little, and the synthetic difficulty of high molecular weight polyesters limits its processing and application.
Summary of the invention
In order to continually develop tencel, utilize poly terephthalic acid 1, the 2-propylene glycol ester by the nano modification means, can be researched and developed tencel, enlarges its range of application.
A kind of fluorescence poly terephthalic acid 1, the 2-propylene glycol ester fiber, at first interpolation Nano titanium dioxide 1～3% and calcium aluminate 1～3% in polyester synthetic obtain nano-modified polyester, obtain the nano-modified polyester fiber by melt spinning technology.
Synthesizing of nano-modified polyester, raw material is 1,2-propylene glycol and terephthalic acid (TPA), raw material molar ratio of alcohol to acid 1.10～1.15, the catalyst and the auxiliary agent that use in synthetic are 1, what of 2-propylene glycol molar weight, catalyst and synthesis material are mixed with slurry together and enter esterification, nano modifier, stabilizing agent, synergist and fire retardant then add in the poly-stage of final minification, the synthetic poly terephthalic acid 1 that obtains the nano modification high molecular, 2-propylene glycol ester.
Catalyst p-methyl benzenesulfonic acid 50 * 10
-6
Catalyst silico-tungstic acid 50 * 10
-6
Catalyst metatitanic acid four butyl esters 300 * 10
-6
Nano modifier titanium dioxide 1～3%
Nano modifier calcium aluminate 1～3%
Stabilizing agent trimethyl phosphate 5～8 ‰
Fire retardant bromo carbonic acid ester 5～8 ‰
Synergist sodium antimonate 1～3 ‰
Poly terephthalic acid 1, the synthesis technique of 2-propylene glycol ester:
| Condition | Esterification I | Esterification II | Precondensation | Final minification is poly- |
| Reaction temperature/℃ | ??150～160 | 160～170 | ??250～260 | ??260～270 |
| Reaction pressure/Pa | ??(1.3～1.5)×10 5 | 60000～70000 | ??2500～3000 | ??50～100 |
| The time of staying/min | ??100～120 | 100～120 | ??60～90 | ??150～180 |
Modified poly ester can make fiber by spinning, first 260 ℃ of the draft temperatures that spin of melt spinning, and speed is 2000～2500m/min, the draw ratio 2.5～3.0 that stretches for one, 140 ℃ of temperature, heat setting temperature be at 100～110 ℃, the draw ratio 1.10～1.50 that two roads stretch, 120 ℃ of temperature, 80～90 ℃ of the temperature of curling reach below 40 ℃ fiber temperature through HEAT SETTING again, cut off, spinning obtains nano-carbon poly terephthalic acid (TPA) 1,2-propylene glycol ester fiber specification 1.60～1.65detx * 38mm.
Progressive meaning of the present invention is:
The poly terephthalic acid 1 that makes, the 2-propylene glycol ester fiber has fluorescent effect, and energy usable reflection light reaches antibiotic, wear-resisting, environmental-protection function when having good caution and safety precaution.
The specific embodiment
A kind of fluorescence poly terephthalic acid 1, the 2-propylene glycol ester fiber, interpolation Nano titanium dioxide 1～3% and calcium aluminate 1～3% in polyester synthetic obtain the polyester of nano modification, polyester can directly obtain nano modification poly terephthalic acid 1 by melt spinning technology, the 2-propylene glycol ester fiber.
Embodiment
1. the synthetic of polyester at first is the catalyst solution configuration: the present invention uses p-methyl benzenesulfonic acid, silico-tungstic acid and butyl titanate to be catalyst, determine 1 earlier, the consumption of 2-propylene glycol adds the catalyst dispensing containers to catalyst then, the addition of p-methyl benzenesulfonic acid is 1,50 * 10 of 2-propylene glycol amount
-6, the addition of silico-tungstic acid is 1,50 * 10 of 2-propylene glycol amount
-6, the butyl titanate addition is 1,300 * 10 of 2-propylene glycol amount
-6, inject a spot ofly 1, the 2-propylene glycol stirs, heating, make catalyst 100 ℃ 1, dissolve in the 2-propylene glycol, 1 after the dissolving, 2-propylene glycol catalyst solution enters cut-back tank, inject remaining 1, the 2-propylene glycol.Stir the content that catalyst is measured in the back, finish the configuration of catalyst solution.
2. be the slurry configuration then: the ratio of terephthalic acid (TPA) according to alkyd material ratio 1.12 joined in the slurry batch tank, injecting catalyst solution, through mixing form slurry, the slurry that configures is transported in the esterification device.Nano modifier, stabilizing agent, synergist and fire retardant then add in the poly-stage of final minification.
Nano modifier titanium dioxide 3%
Nano modifier calcium aluminate 3%
Stabilizing agent trimethyl phosphate 5 ‰
Fire retardant bromo carbonic acid ester 6 ‰
Synergist sodium antimonate 3 ‰
3. the synthesis technique of polyester comprises esterification and polycondensation reaction, and first step esterification is finished through two reaction kettle of the esterification, and polycondensation reaction is finished through prepolymerization reaction still and the poly-reactor of final minification.
| Condition | Esterification I | Esterification II | Precondensation | Final minification is poly- |
| Reaction temperature/℃ | ??150～160 | ??160～170 | ??250～260 | ??260～270 |
| Reaction pressure/Pa | ??1.45×10 5 | ??61000 | ??2600 | ??80 |
| The time of staying/min | ??100 | ??100 | ??70 | ??160 |
4. first 260 ℃ of the draft temperatures that spin of melt spinning, speed is 2000m/min, the draw ratio 2.6 of one stretching, 140 ℃ of temperature, heat setting temperature is at 100 ℃, the draw ratio 1.12 that two roads stretch, 120 ℃ of temperature, 80～90 ℃ of the temperature of curling, through HEAT SETTING fiber temperature is reached below 40 ℃ again, cut off, spinning obtains nano-carbon poly terephthalic acid (TPA) 1,2-propylene glycol ester fiber specification 1.60～1.65detx * 38mm.Spinning obtains nano modification poly terephthalic acid 1, the 2-propylene glycol ester fiber to the reflectivity of light 65～70%.
Claims (1)
1. fluorescence poly terephthalic acid 1, the 2-propylene glycol ester fiber is characterized in that:
At first interpolation Nano titanium dioxide and calcium aluminate in polyester synthetic, obtain the polyester of nano modification, raw material is 1,2-propylene glycol and terephthalic acid (TPA), molar ratio of alcohol to acid 1.10～1.15, what of pure molar weight the addition of auxiliary agent be in synthetic, and catalyst and polymer raw enter esterification together, and nano modifier, stabilizing agent, synergist and fire retardant then add in the poly-stage of final minification;
Catalyst p-methyl benzenesulfonic acid 50 * 10
-6
Catalyst silico-tungstic acid 50 * 10
-6
Catalyst metatitanic acid four butyl esters 300 * 10
-6
Nano modifier titanium dioxide 1～3%
Nano modifier calcium aluminate 1～3%
Stabilizing agent trimethyl phosphate 5～8 ‰
Fire retardant bromo carbonic acid ester 5～8 ‰
Synergist sodium antimonate 1～3 ‰
The polyester spinning of nano modification makes fiber then, first 260 ℃ of the draft temperatures that spin of melt spinning, speed is 2000～2500m/min, the draw ratio 2.5～3.0 that stretches for one, 140 ℃ of temperature, heat setting temperature is at 100～110 ℃, the draw ratio 1.10～1.50 that two roads stretch, 120 ℃ of temperature, 80～90 ℃ of the temperature of curling reach below 40 ℃ fiber temperature through HEAT SETTING again, cut off, spinning obtains nano-carbon poly terephthalic acid (TPA) 1,2-propylene glycol ester fiber specification 1.60～1.65detx * 38mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101525491A CN101671863B (en) | 2009-09-17 | 2009-09-17 | Fluorescent poly terephthalic acid 1, 2-propylene glycol ester fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101525491A CN101671863B (en) | 2009-09-17 | 2009-09-17 | Fluorescent poly terephthalic acid 1, 2-propylene glycol ester fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101671863A true CN101671863A (en) | 2010-03-17 |
| CN101671863B CN101671863B (en) | 2012-01-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101525491A Expired - Fee Related CN101671863B (en) | 2009-09-17 | 2009-09-17 | Fluorescent poly terephthalic acid 1, 2-propylene glycol ester fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101671863B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102330172A (en) * | 2011-05-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Nano titanium dioxide-modified terylene pre-oriented yarn |
| CN102787388A (en) * | 2011-05-16 | 2012-11-21 | 江苏鹰翔化纤股份有限公司 | Nano-titanium dioxide modified terylene low elastic interlaced yarn |
| CN102797069A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing nano titanium dioxide modified polyester fibers |
-
2009
- 2009-09-17 CN CN2009101525491A patent/CN101671863B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102787388A (en) * | 2011-05-16 | 2012-11-21 | 江苏鹰翔化纤股份有限公司 | Nano-titanium dioxide modified terylene low elastic interlaced yarn |
| CN102330172A (en) * | 2011-05-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Nano titanium dioxide-modified terylene pre-oriented yarn |
| CN102797069A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing nano titanium dioxide modified polyester fibers |
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| Publication number | Publication date |
|---|---|
| CN101671863B (en) | 2012-01-04 |
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Granted publication date: 20120104 Termination date: 20140917 |
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