CN102329481A - Method for preparing 1,2-butanediol modified terylene chips - Google Patents
Method for preparing 1,2-butanediol modified terylene chips Download PDFInfo
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- CN102329481A CN102329481A CN 201110164744 CN201110164744A CN102329481A CN 102329481 A CN102329481 A CN 102329481A CN 201110164744 CN201110164744 CN 201110164744 CN 201110164744 A CN201110164744 A CN 201110164744A CN 102329481 A CN102329481 A CN 102329481A
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- Prior art keywords
- esterification
- add
- terephthalic acid
- mol ratio
- butyleneglycol
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- 239000005020 polyethylene terephthalate Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 13
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical compound CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229920004933 Terylene® Polymers 0.000 title abstract description 4
- 239000000835 fiber Substances 0.000 claims abstract description 22
- 229920000728 polyester Polymers 0.000 claims abstract description 19
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 13
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 229920004934 Dacron® Polymers 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 13
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 8
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 8
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 235000011150 stannous chloride Nutrition 0.000 claims description 8
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 8
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010009 beating Methods 0.000 claims description 4
- 150000007942 carboxylates Chemical class 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000005453 pelletization Methods 0.000 claims description 4
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical group CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- 230000032050 esterification Effects 0.000 abstract description 14
- 238000005886 esterification reaction Methods 0.000 abstract description 14
- 238000009987 spinning Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000155 melt Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 14
- 229920004935 Trevira® Polymers 0.000 description 10
- 239000000463 material Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 230000008602 contraction Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention relates to a method for preparing 1,2-butanediol modified terylene chips. The method comprises two steps of esterification and polycondensation. A melt prepared by the process has stable quality and the chips have high spinning performance; and the prepared high-shrinkage polyester staple fibers have high shrinkage stability, and are uniformly dyed and low in production cost.
Description
Technical field
The present invention relates to the section of a kind of modified dacron, particularly, the present invention relates to preparation method a kind of 1, the section of 2-butyleneglycol modified dacron.
Background technology
Terylene is as one of the big main force of three in synthon fiber, because of its good physics and chemical property are widely used in garment material and other non-garment industry.Dacron product since coming out, also once with its drape is good, intensity is high, well-pressed and be used as main textile raw material by downstream user and weave all kinds of textiless.Along with economic globalization, the market internationalization, people are also increasingly high to the requirement of clothes; Not only to have comfortableness; Also will have functionally, lining just develops to light, gentle, functional direction, and composite fibre materials just need improve constantly performance and satisfy requirements of weaving process.
Over past ten years, the development of China polyester industrial rapidly, trevira output is 2,700 ten thousand tons of developing into for the year ends 2010 of 516.5 ten thousand tons at the beginning of 2000, average annual growth rate surpasses 25%, has accounted for 66% of global polyester output.Terylene has become the maximum synthon kind of output in the man-made fiber, is widely used in clothing, decoration, household textiles, fabrics for industrial use and national economy all respects such as national defence, industrial engineering.5 years from now on, also will keep increasing fast.But as textile materials, trevira also has significant disadvantages.Therefore, the working method of selection science, efficient, high-quality, energy-saving and environmental protection is to adapting to and promoting that the high speed Sustainable development of polyester industrial, polyster fibre is most important.
Though in synthon, trevira has the multiple performance of suitable textile applications and application in industry, thereby it has obtained amazing development since scale operation.But along with the development of World Science development of technology and world industry, trevira can not satisfy people's requirement fully on performance and function.The result of development and innovation makes people develop large quantities of differential, functionalization and high performance synthon.
The developing direction of PET industry has been represented in the development and application of present differential trevira new variety.The technology of differential polyester product exploitation roughly can reduce the following aspects:
(1) spining technology of compound spinning superfine fibre and spin pack design;
(2) the compound spining technology that spins two-pack functional fiber or differential fibre;
(3) fused mass directly spinning prepares the complete set technology of thin dawn, micro denier polyester fiber;
(4) spining technology of various cross section Design of spinneret and profile fibre;
The spining technology of (5) three different fibers and mix fine Design of spinneret with plate;
(6) different contraction mixed fiber yarn Combined Machining Technology;
(7) polymer modification prepares the preparation of functional polyester and fiber thereof;
(8) polymer modification prepares the Application and Development of intelligent fiber and intelligent lining;
(9) the nano-powder in-situ polymerization prepares functional polyester and fiber thereof;
(10) preparation of multiple organic or inorganic nanoparticle and dispersion technology;
(11) preparation and the spining technology of organic or inorganic nanoparticle/polymer-based carbon composite polyester material;
(12) natural fiber and synthon, chemical-fibres filaments and short fiber multidimensional combination technology.
Conventional trevira, percent crystallinity is higher, and percent thermal shrinkage is lower, generally is lower than 10%.Along with continually developing of the continuous expansion of trevira Application Areas, fabric product innovation, increasing than the demand of the high-shrinkage fiber of high shrinkage to having, all kinds of high-shrinkage fibers are succeeded in developing in succession.
Generally can improve the shrinking percentage of trevira through chemical modification method, promptly in the production process of normal polyester, pass through to add the 3rd monomer, destroy macromolecular regularity; Reduce crystallizing power; And the physically modified of combination spinning drafting process, make the high-shrinkage fibre that makes, boiling water shrinkage height and stable contraction rate; The strength and elongation index is good, satisfies the requirement of post-treatment better.The present inventor has accomplished the present invention through further improving the Technology of polyester and condensation reaction.
Summary of the invention
The objective of the invention is to continually develop functional trevira in order to satisfy many-sided needs of people to weaving face fabric, we carry out modification through adding the 3rd monomer 1,2-butyleneglycol to traditional trevira.The melt quality that adopts prepared of the present invention to obtain is stable, the chip spinning excellent property; The high-shrinkage polyester staple fibers stable contraction rate property that makes is good, even dyeing, and production cost is low.
To achieve these goals, the invention provides following technical scheme:
A kind of 1 preparation method of, 2-butyleneglycol modified dacron section,
At first; On continuous polycondensation equipment; With terephthalic acid (PTA), 1,2-butyleneglycol, terepthaloyl moietie (EG) monomer; According to terephthalic acid (PTA), 1,2-butyleneglycol, the monomeric mol ratio of terepthaloyl moietie (EG) is 1: the ratio of 0.08-0.016:1.12-1.18 is measured continuously and stably separately and is joined in the slurry still and pulls an oar; Add titanium sulfate, tin protochloride in the making beating still, wherein the mol ratio of the add-on of titanium sulfate and terephthalic acid is 0.03-0.05%, and the add-on of tin protochloride and the mol ratio of phthalic acid are 0.02-0.05%;
Then, above-mentioned slurry continous-stable is delivered in esterification-I, esterification-II, the esterification-III reaction kettle, adds stablizer in esterification-III reaction kettle; Carboxylate is pumped into polycondensation workshop section, gathers through precondensation and final minification under temperature 270-278 ℃ condition by polycondensating process and obtain the modified dacron melt; Polyester fondant obtains the modified dacron section through Cast Strip, pelletizing, drying.
Wherein, described stablizer is a triethyl phosphate, and the mol ratio of its add-on and terephthalic acid is 0.23-0.35%.
Wherein, the temperature of esterification-I reaction kettle is controlled at 255-257 ℃, and control still internal pressure is 0.38-0.47 MPa.
Wherein, the temperature of esterification-II reaction kettle is controlled at 259-262 ℃, and control still internal pressure is 0.29-0.35 MPa.
Wherein, the temperature of esterification-III reaction kettle is controlled at 263-266 ℃, and control still internal pressure is 0.13-0.19 MPa.
Wherein, esterification yield is 78-80% in control esterification-I reaction kettle.
Wherein, esterification yield is 88-91% in control esterification-II reaction kettle.
Wherein, esterification yield is 95-98% in control esterification-III reaction kettle.
Wherein, the temperature of prepolymerization reaction still is controlled at 270-273 ℃, and control still internal pressure is 3.2-8.9 KPa.
Wherein, the temperature that final minification gathers reaction kettle is controlled at 273-278 ℃, and control still internal pressure is 75-115 Pa.
Wherein, slice process carries out in water, and water temperature is 13-18 ℃.
The invention has the beneficial effects as follows, a kind of preparation technology of modified dacron polyester fondant section is provided.Through improving and strict control reaction parameter, the slicing characteristics viscosity dL/g value for preparing is 0.640 ± 0.010, and fusing point is higher than 260 ℃, and dry back moisture is lower than 0.4%; The section stable performance that makes, even dyeing, spinning properties is excellent.
Embodiment
To combine concrete embodiment that technical scheme of the present invention is done further to explain and explanation below.
Embodiment 1
At first on continuous polycondensation equipment; With terephthalic acid (PTA), 1,2-butyleneglycol, terepthaloyl moietie (EG) monomer; According to terephthalic acid (PTA), 1,2-butyleneglycol, the monomeric mol ratio of terepthaloyl moietie (EG) is 1: the ratio of 0.08:1.12 is measured continuously and stably separately and is joined in the slurry still and pulls an oar; Add titanium sulfate, tin protochloride in the making beating still; Wherein the mol ratio of the add-on of titanium sulfate and terephthalic acid is 0.03%, and the add-on of tin protochloride and the mol ratio of phthalic acid are 0.02%;
Then above-mentioned slurry continous-stable is delivered in esterification-I, esterification-II, the esterification-III reaction kettle, adds stablizer in esterification-III reaction kettle continuously; Carboxylate is pumped into polycondensation workshop section, gathers through precondensation and final minification and obtain the modified dacron melt; Polyester fondant obtains the modified dacron section through Cast Strip, pelletizing, drying.Wherein, concrete esterification and polycondensation condition are as shown in table 1.
Table 1 embodiment 1 modified poly ester esterification and polycondensation condition
| Condition | Esterification I | Esterification II | Esterification III | Precondensation I | Precondensation II |
| Temperature of reaction/℃ | 255 | 259 | 263 | 270 | 273 |
| Reaction pressure | 0.38 MPa | 0.29 MPa | 0.13 MPa | 3.2 KPa | 75 Pa |
Embodiment 2
At first on continuous polycondensation equipment; With terephthalic acid (PTA), 1,2-butyleneglycol, terepthaloyl moietie (EG) monomer; According to terephthalic acid (PTA), 1,2-butyleneglycol, the monomeric mol ratio of terepthaloyl moietie (EG) is 1: the ratio of 0.16:1.18 is measured continuously and stably separately and is joined in the slurry still and pulls an oar; Add titanium sulfate, tin protochloride in the making beating still; Wherein the mol ratio of the add-on of titanium sulfate and terephthalic acid is 0.05%, and the add-on of tin protochloride and the mol ratio of phthalic acid are 0.05%;
Then above-mentioned slurry continous-stable is delivered in esterification-I, esterification-II, the esterification-III reaction kettle, adds stablizer in esterification-III reaction kettle; Carboxylate is pumped into polycondensation workshop section, gathers through precondensation and final minification and obtain the modified dacron melt; Polyester fondant obtains the modified dacron section through Cast Strip, pelletizing, drying.Wherein, concrete esterification and polycondensation condition are as shown in table 2.
Table 2 embodiment 2 modified poly ester esterifications and polycondensation condition
| Condition | Esterification I | Esterification II | Esterification III | Precondensation | Final minification gathers |
| Temperature of reaction/℃ | 257 | 262 | 266 | 273 | 278 |
| Reaction pressure | 0.47 MPa | 0.35 MPa | 0.19 MPa | 8.9 KPa | 115 Pa |
The modified dacron that adopts method of the present invention to prepare is cut into slices stable in properties, particularly its limiting viscosity deviation in 0.010% scope, and the section fusing point for preparing also remains on more than 260 ℃; As long as strict control reaction parameter is in the framework of the present definition, the resulting modified dacron section of each batch index difference is very little.
Claims (6)
1. the preparation method of 2-butyleneglycol modified dacron section,
At first; On continuous polycondensation equipment; With terephthalic acid (PTA), 1,2-butyleneglycol, terepthaloyl moietie (EG) monomer; According to terephthalic acid (PTA), 1,2-butyleneglycol, the monomeric mol ratio of terepthaloyl moietie (EG) is 1: the ratio of 0.08-0.016:1.12-1.18 is measured continuously and stably separately and is joined in the slurry still and pulls an oar; Add titanium sulfate, tin protochloride in the making beating still, wherein the mol ratio of the add-on of titanium sulfate and terephthalic acid is 0.03-0.05%, and the add-on of tin protochloride and the mol ratio of phthalic acid are 0.02-0.05%;
Then, above-mentioned slurry continous-stable is delivered in esterification-I, esterification-II, the esterification-III reaction kettle, adds stablizer in esterification-III reaction kettle; Carboxylate is pumped into polycondensation workshop section, gathers through precondensation and final minification under temperature 270-278 ℃ condition by polycondensating process and obtain the modified dacron melt; Polyester fondant obtains the modified dacron section through Cast Strip, pelletizing, drying.
2. the described preparation method of claim 1 is characterized in that described stablizer is a triethyl phosphate, and the mol ratio of its add-on and terephthalic acid is 0.23-0.35%.
3. the described preparation method of claim 1 is characterized in that the temperature of prepolymerization reaction still is controlled at 270-273 ℃, and control still internal pressure is 3.2-8.9 KPa.
4. the described preparation method of claim 1 is characterized in that the temperature that final minification gathers reaction kettle is controlled at 273-278 ℃, and control still internal pressure is 75-115 Pa.
5. the described preparation method of claim 1 is characterized in that the fibre section is circle, trilobal, trilateral, cruciform, king's font, hollow shape or five leaf.
6. the described preparation method of claim 1 is characterized in that slice process carries out in water, and water temperature is 13-18 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110164744 CN102329481A (en) | 2011-06-20 | 2011-06-20 | Method for preparing 1,2-butanediol modified terylene chips |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110164744 CN102329481A (en) | 2011-06-20 | 2011-06-20 | Method for preparing 1,2-butanediol modified terylene chips |
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| Publication Number | Publication Date |
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| CN102329481A true CN102329481A (en) | 2012-01-25 |
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| CN 201110164744 Pending CN102329481A (en) | 2011-06-20 | 2011-06-20 | Method for preparing 1,2-butanediol modified terylene chips |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951977A (en) * | 2005-10-19 | 2007-04-25 | 东丽纤维研究所（中国）有限公司 | Process for producing polyester |
| US20070093615A1 (en) * | 2005-10-25 | 2007-04-26 | Callander Douglas D | Dispersions of High Carboxyl Polyamides Into Polyesters Using An Interfacial Tension Reducing Agent |
| CN101208371A (en) * | 2005-06-24 | 2008-06-25 | 东洋纺织株式会社 | Method for preparing polyester and polyester manufactured by the method as well as polyester formed body |
| CN101654513A (en) * | 2009-09-14 | 2010-02-24 | 江苏中鲈科技发展股份有限公司 | Method and device for continuously producing poly terephthalic acid-1, 3-propylene glycol ester |
-
2011
- 2011-06-20 CN CN 201110164744 patent/CN102329481A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101208371A (en) * | 2005-06-24 | 2008-06-25 | 东洋纺织株式会社 | Method for preparing polyester and polyester manufactured by the method as well as polyester formed body |
| CN1951977A (en) * | 2005-10-19 | 2007-04-25 | 东丽纤维研究所（中国）有限公司 | Process for producing polyester |
| US20070093615A1 (en) * | 2005-10-25 | 2007-04-26 | Callander Douglas D | Dispersions of High Carboxyl Polyamides Into Polyesters Using An Interfacial Tension Reducing Agent |
| CN101654513A (en) * | 2009-09-14 | 2010-02-24 | 江苏中鲈科技发展股份有限公司 | Method and device for continuously producing poly terephthalic acid-1, 3-propylene glycol ester |
Non-Patent Citations (1)
| Title |
|---|
| 《浙江化工》 19981231 徐奇君等 丁二醇改性PET的研制 24-26 1-6 第29卷, 第2期 * |
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Application publication date: 20120125 |