CN103304791A - Preparation process of high-quality fusant - Google Patents
Preparation process of high-quality fusant Download PDFInfo
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- CN103304791A CN103304791A CN2013101654821A CN201310165482A CN103304791A CN 103304791 A CN103304791 A CN 103304791A CN 2013101654821 A CN2013101654821 A CN 2013101654821A CN 201310165482 A CN201310165482 A CN 201310165482A CN 103304791 A CN103304791 A CN 103304791A
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Abstract
The invention relates to a high-quality fusant and a preparation process of the high-quality fusant, and in particular relates to a preparation process of a high-quality fusant of terylene 30D/72FFDY. The fusant is prepared by using a flow of five kettles, namely a first esterification kettle, a second esterification kettle, a first pre-condensation kettle, a second pre-condensation kettle and a final polycondensation kettle; raw materials of the high-quality fusant comprise purified terephthalic acid, ethylene glycol, titanium dioxide and diethylene glycol. The fusant is stable in quality and uniform in viscosity, the range of viscosity fluctuation does not exceed 0.005dl/g, broken ends are effectively reduced in production of 30D/72F, the dyeing uniformity is good, and the evenness coefficient of variation (CV%) is small. The five-kettle process flow ensures good product uniformity and good quality stability and is easy to control and operate.
Description
Technical field
The present invention relates to a kind of preparation technology of high-quality melt, relate in particular to the preparation technology of the high-quality melt of a kind of terylene 30D/72F FDY.
Background technology
The final filament number of terylene 30D/72F FDY is 0.45dpf, melt quality is very large on the spinning property impact of this product, we show by a large amount of experiments, need adopt following method to be controlled to melt quality: the melt quality that 1. requires polyester to get is stable, viscosity is even, the viscosity fluctuation scope must not surpass 0.005dl/g, and the viscosity drop that is transported to behind the filament spinning component by pipeline is little; 2. impurity will lack in the melt, and the diameter of impurity particle is the smaller the better, requires to be aggregated in the strainer that will adopt 15um behind the terminal polymerization kettle.Select simultaneously suitable melt Conveying temperature and the regulating effect that takes full advantage of heat exchanger, to guarantee that melt is transported to spinning system under lower temperature, to reduce the degraded of melt in course of conveying.
High-quality melt quality is stable, and viscosity is even, and impurity is few in the melt, and the diameter of impurity particle is very little.Melt of the present invention adopts direct esterification to claim again PTA pure terephthalic acid method to produce polyester fondant, directly generate the BHET ethylene glycol terephthalate with PTA and EG glycol reaction, the centre did not need through this step of dimethyl terephthalate (DMT), then carried out polycondensation and generated PET.Its quality reaches the requirement of high-quality melt.
Summary of the invention
The present invention has researched and developed a kind of high-quality melt and preparation technology thereof in order to address the above problem, thereby improves production efficiency and the quality of terylene 30D/72F FDY.
Technical solution of the present invention:
A kind of high-quality melt and preparation technology thereof, this melt adopts five autoclaves process, i.e. the first esterifying kettle, second esterification kettle, the first precondensation still, the second precondensation still and whole polycondensation vessel, it is characterized in that: the starting material of high-quality melt are: pure terephthalic acid, ethylene glycol, titanium dioxide and glycol ether.
The accounting of described ethylene glycol, pure terephthalic acid, titanium dioxide and glycol ether is for being followed successively by: 21.84-21.87%, 75.56-76.45%, 0.30-0.34% and 1.27-1.37%.
A kind of high-quality melt preparation technology is characterized in that described technique comprises the steps:
One, with the melt slurry that configures, deliver into the first esterifying kettle through supply pump, carry out mass-and heat-transfer by agitator, the liquid phase heating agent by inside heats through spiral heater again, carries out esterification under the pressure of 250-262 ℃ temperature and 0.12-0.55bar (g);
Two, send into the second reaction kettle of the esterification by the material of bottom product pump after with the step 1 esterification, material is after the mistress of the second reaction kettle of the esterification enters inner room, relying on the second reaction kettle of the esterification agitator to stir with inner heating coil heats, under 257-268 ℃ temperature and 0.10-0.15bar (g) pressure, continue esterification, add the second reaction kettle of the esterification after simultaneously TITANIUM DIOXIDE DELUSTRANT suspension being measured through toothed gear pump;
Three, the material of the second reaction kettle of the esterification relies on potential difference and pressure reduction to enter the first Prepolycondensating reactor inner room, by inner coil pipe heating, is to continue reaction under the 130-90mbar condition in 263-270 ℃ temperature and vacuum tightness;
Four, material is behind the mistress, poor by the vacuum between the first and second Prepolycondensating reactors, material is admitted in the second Prepolycondensating reactor, stir by strengthening with the agitator of Frequency Converter Control, material is carried by pre-melt discharging pump after continuing to react the viscosity that reaches 0.29-0.34 dL/g, enters final polycondensation reactor after pre-melt strainer filters;
Five, the material from the second Prepolycondensating reactor enters through final polycondensation disk reactor bottom; 270-285 ℃ of temperature; under the agitation condition of high vacuum＜1.5mbar and 3.0 rev/mins; finish final polycondensation; reach viscosity 0.678 ± 0.002 dL/g of regulation; by melt Conveying pump and fondant filter, be sent to respectively long filament through Melt three-way valve and become section with the dicing machine pelletizing at last.
The gamma value of the esterification of step 1 is more than or equal to 92%.
The gamma value of the esterification of step 2 is more than or equal to 97%.
The water that generates in the step 2 esterification and the EG that is evaporated carry out fractionation by process tower, and the water of process tower fractionation enters the process tower backflash after the air-cooler condensation, then add catalyzer by under meter.
Described catalyzer is antimony acetate.
The vacuum condition of step 4 is to control by the additional nitrogen amount of vacuum controller control precondensation liquid-ring vacuum pump.
The high vacuum condition of step 5 is to control by the pneumatic adjusting valve door of three grades of injection systems that are connected to the poly-vacuum system of final minification.
The specification of step 5 middle filtrator is 15um, filters out diameter in the melt greater than the mechanical impurity particle of 15 ~ 20um, and has the effect of homogenize melt concurrently.
Beneficial effect of the present invention:
This melt quality is stable, and viscosity is even, and the viscosity fluctuation scope surpasses 0.005dl/g, effectively reduces broken end in producing 30D/72F, and dyeing uniformity is good, and bar is done the characteristics such as the CV% value is little.Five still technical process
Make the product good uniformity, quality stability is good, and operation easy to control.EG in the production equipment adopts inner loop mode in addition, has effectively reduced the consumption of EG; The poly-vacuum system of final minification adopts EG steam as ejection medium, and EG vapo(u)r blasting phlegma can directly be delivered to slurry preparation, has reduced the EG loss, has reduced sewage quantity.By system is added glycol ether, can regulate among the PET glycol ether content and keep constant, can strengthen the dyeing behavior of rear road trevira.
Description of drawings
Fig. 1 is melt preparation were established structural representation.
Embodiment
The present invention is described further below in conjunction with embodiment.
This melt adopts five autoclaves process, i.e. the first esterifying kettle, second esterification kettle, the first precondensation still, the second precondensation still and whole polycondensation vessel.The reaction in each stage of five autoclaves process is more even, and by product is few.
Through the melt slurry that configures, carry through the slurry supply pump, enter in the first esterifier 1 (approximately 140 cubic metres), rely on agitator 2 to carry out mass-and heat-transfer, inside is heated through spiral heater by the liquid phase heating agent, under the pressure of 250-262 ℃ temperature and 0.12-0.55bar (g), carry out esterification, and reach certain gamma value (approximately 92%), send into the second reaction kettle of the esterification 4 (approximately 58 cubic metres) by bottom product pump 3 again.
When material after the mistress of the second reaction kettle of the esterification 4 enters inner room, rely on stirring and the inner heating coil of the second reaction kettle of the esterification agitator 5 to heat, under 257-268 ℃ temperature and 0.10-0.15bar (g) pressure, continue reaction, reach gamma value (approximately 97%).TITANIUM DIOXIDE DELUSTRANT suspension also adds the second reaction kettle of the esterification 4 after measuring through toothed gear pump simultaneously.Two interior water that generate of reaction kettle of the esterification and the EG that is evaporated enter process tower and carry out rectifying: the cat head fraction is mainly water, enters the process tower backflash after the air-cooler condensation, then adds catalyzer by under meter.
The material of the second reaction kettle of the esterification 4 relies on potential difference and pressure reduction to enter approximately 42 cubic metres of the first Prepolycondensating reactor 6() inner room, by inner coil pipe heating, be to continue reaction under the 130-90mbar vacuum condition in 263-270 ℃ temperature and vacuum tightness, because material drops to negative pressure from malleation, more violent seething can appear in the low boilers vaporizations such as EG, so the first Prepolycondensating reactor does not arrange agitator, material is behind the mistress, poor by the vacuum between the first and second Prepolycondensating reactors, material is admitted to (horizontal disc reaction response device in the second Prepolycondensating reactor 7, approximately 69 cubic metres), by the agitator Final 8 stirring with Frequency Converter Control, material continues reaction and reaches 0.29-0.34 dL/g viscosity, is then carried by pre-melt discharging pump 9, enters final polycondensation reactor 11 after melt prefilter 10 filters.
The vacuum tightness of the first precondensation is to control by the additional nitrogen amount of vacuum controller control precondensation liquid-ring vacuum pump.
The vacuum tightness of the second precondensation is to control by the pneumatic adjusting valve door of three grades of injection systems that are connected to the poly-vacuum system of final minification.
Material from the second Prepolycondensating reactor is entered by final polycondensation disk reactor (approximately 163 cubic metres) bottom, 270-285 ℃ of temperature, under the agitation condition of high vacuum＜1.5mbar and 3.0 rev/mins, finish final polycondensation, reach viscosity 0.678 ± 0.002 dL/g of regulation.By melt Conveying pump 12 and fondant filter 13, be sent to respectively melt spinning 14 through Melt three-way valve and become section with dicing machine 15 pelletizings at last.
Adopt the strainer of 15um behind the terminal polymerization kettle, filter out diameter in the melt greater than the mechanical impurity particle of 15 ~ 20um, and have the effect of homogenize melt concurrently.
The melt quality index such as the table 1 that make
Table 1 melt quality index
Claims (10)
1. high-quality melt, this melt adopts five autoclaves process, i.e. the first esterifying kettle, second esterification kettle, the first precondensation still, the second precondensation still and whole polycondensation vessel, it is characterized in that: the starting material of high-quality melt are: pure terephthalic acid, ethylene glycol, titanium dioxide and glycol ether.
2. high-quality melt according to claim 1, it is characterized in that: the accounting of described ethylene glycol, pure terephthalic acid, titanium dioxide and glycol ether is for being followed successively by: 21.84-21.87%, 75.56-76.45%, 0.30-0.34% and 1.27-1.37%.
3. high-quality melt preparation technology is characterized in that, described technique comprises the steps:
One, with the melt slurry that configures, deliver into the first esterifying kettle through supply pump, carry out mass-and heat-transfer by agitator, the liquid phase heating agent by inside heats through spiral heater again, carries out esterification under the pressure of 250-262 ℃ temperature and 0.12-0.55bar (g);
Two, send into the second reaction kettle of the esterification by the material of bottom product pump after with the step 1 esterification, material is after the mistress of the second reaction kettle of the esterification enters inner room, relying on the second reaction kettle of the esterification agitator to stir with inner heating coil heats, under 257-268 ℃ temperature and 0.10-0.15bar (g) pressure, continue esterification, add the second reaction kettle of the esterification after simultaneously TITANIUM DIOXIDE DELUSTRANT suspension being measured through toothed gear pump;
Three, the material of the second reaction kettle of the esterification relies on potential difference and pressure reduction to enter the first Prepolycondensating reactor inner room, by inner coil pipe heating, is to continue reaction under the 130-90mbar condition in 263-270 ℃ temperature and vacuum tightness;
Four, material is behind the mistress, poor by the vacuum between the first and second Prepolycondensating reactors, material is admitted in the second Prepolycondensating reactor, stir by strengthening with the agitator of Frequency Converter Control, material is carried by pre-melt discharging pump after continuing to react the viscosity that reaches 0.29-0.34 dL/g, enters final polycondensation reactor after pre-melt strainer filters;
Five, the material from the second Prepolycondensating reactor enters through final polycondensation disk reactor bottom; 270-285 ℃ of temperature; under the agitation condition of high vacuum＜1.5mbar and 3.0 rev/mins; finish final polycondensation; reach viscosity 0.678 ± 0.002 dL/g of regulation; by melt Conveying pump and fondant filter, be sent to respectively long filament through Melt three-way valve and become section with the dicing machine pelletizing at last.
4. high-quality melt preparation technology according to claim 3, it is characterized in that: the gamma value of the esterification of step 1 is more than or equal to 92%.
5. high-quality melt preparation technology according to claim 3, it is characterized in that: the gamma value of the esterification of step 2 is more than or equal to 97%.
6. high-quality melt preparation technology according to claim 3, it is characterized in that: the water that generates in the step 2 esterification and the EG that is evaporated carry out fractionation by process tower, the water of process tower fractionation, after the air-cooler condensation, enter the process tower backflash, then add catalyzer by under meter.
7. high-quality melt preparation technology according to claim 6, it is characterized in that: described catalyzer is antimony acetate.
8. high-quality melt preparation technology according to claim 3 is characterized in that: the vacuum condition of step 4 is to control by the additional nitrogen amount of vacuum controller control precondensation liquid-ring vacuum pump.
9. high-quality melt preparation technology according to claim 3 is characterized in that: the high vacuum condition of step 5 is to control by the pneumatic adjusting valve door of three grades of injection systems that are connected to the poly-vacuum system of final minification.
10. high-quality melt preparation technology according to claim 3, it is characterized in that: the specification of step 5 middle filtrator is 15um, filters out diameter in the melt greater than the mechanical impurity particle of 15 ~ 20um, and has the effect of homogenize melt concurrently.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086756A (en) * | 2014-07-28 | 2014-10-08 | 营口康辉石化有限公司 | Production method of optical transparent film-level polyester |
| CN104086755A (en) * | 2014-07-28 | 2014-10-08 | 营口康辉石化有限公司 | Production method of sanitary environment-friendly film level polyester |
| CN106978638A (en) * | 2017-03-30 | 2017-07-25 | 桐昆集团股份有限公司 | A kind of integrated combined unit in Direct-spinning of PET Fiber workshop |
| CN107880073A (en) * | 2016-09-29 | 2018-04-06 | 中国石化仪征化纤有限责任公司 | A kind of continuous producing apparatus and its production method of copoly type flame-retardant monomer |
| CN107881580A (en) * | 2016-09-29 | 2018-04-06 | 中国石化仪征化纤有限责任公司 | A kind of continuous producing method of fire-retardant polyester fibre |
| CN109081911A (en) * | 2018-07-11 | 2018-12-25 | 桐昆集团浙江恒盛化纤有限公司 | A kind of polyester production device that stablizing dyeing and its production technology |
| CN109666134A (en) * | 2018-12-20 | 2019-04-23 | 营口康辉石化有限公司 | Polyester fondant and preparation method thereof |
| CN110528104A (en) * | 2019-08-27 | 2019-12-03 | 江苏德力化纤有限公司 | A kind of preparation method and polyester fiber of different dye type linnet polyester fiber |
| CN110938198A (en) * | 2019-11-20 | 2020-03-31 | 浙江佳人新材料有限公司 | Production process of regenerated low-viscosity slices |
| CN112724390A (en) * | 2020-12-29 | 2021-04-30 | 浙江恒逸石化有限公司 | Antimony-free polyester melt preparation system and method for preparing antimony-free polyester fine denier FDY fiber |
| CN114481335A (en) * | 2021-12-17 | 2022-05-13 | 桐昆集团浙江恒通化纤有限公司 | High-strength sunlight-resistant anti-aging terylene pre-oriented yarn for curtain and preparation method thereof |
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| CN101597813A (en) * | 2008-06-04 | 2009-12-09 | 江阴市华宏化纤有限公司 | The production method of fiber used for super bright high strength sewing threads |
| WO2010001252A2 (en) * | 2008-07-02 | 2010-01-07 | Invista Technologies S.A.R.L. | Copolyester for shrink film applications |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086756A (en) * | 2014-07-28 | 2014-10-08 | 营口康辉石化有限公司 | Production method of optical transparent film-level polyester |
| CN104086755A (en) * | 2014-07-28 | 2014-10-08 | 营口康辉石化有限公司 | Production method of sanitary environment-friendly film level polyester |
| CN107881580B (en) * | 2016-09-29 | 2020-05-01 | 中国石化仪征化纤有限责任公司 | Continuous production method of flame-retardant polyester fiber |
| CN107880073A (en) * | 2016-09-29 | 2018-04-06 | 中国石化仪征化纤有限责任公司 | A kind of continuous producing apparatus and its production method of copoly type flame-retardant monomer |
| CN107881580A (en) * | 2016-09-29 | 2018-04-06 | 中国石化仪征化纤有限责任公司 | A kind of continuous producing method of fire-retardant polyester fibre |
| CN107880073B (en) * | 2016-09-29 | 2020-05-01 | 中国石化仪征化纤有限责任公司 | Continuous production equipment and production method of copolymerization type flame-retardant monomer |
| CN106978638A (en) * | 2017-03-30 | 2017-07-25 | 桐昆集团股份有限公司 | A kind of integrated combined unit in Direct-spinning of PET Fiber workshop |
| CN109081911A (en) * | 2018-07-11 | 2018-12-25 | 桐昆集团浙江恒盛化纤有限公司 | A kind of polyester production device that stablizing dyeing and its production technology |
| CN109666134A (en) * | 2018-12-20 | 2019-04-23 | 营口康辉石化有限公司 | Polyester fondant and preparation method thereof |
| CN109666134B (en) * | 2018-12-20 | 2021-08-13 | 营口康辉石化有限公司 | Polyester melt and process for producing the same |
| CN110528104A (en) * | 2019-08-27 | 2019-12-03 | 江苏德力化纤有限公司 | A kind of preparation method and polyester fiber of different dye type linnet polyester fiber |
| CN110938198A (en) * | 2019-11-20 | 2020-03-31 | 浙江佳人新材料有限公司 | Production process of regenerated low-viscosity slices |
| CN112724390A (en) * | 2020-12-29 | 2021-04-30 | 浙江恒逸石化有限公司 | Antimony-free polyester melt preparation system and method for preparing antimony-free polyester fine denier FDY fiber |
| CN112724390B (en) * | 2020-12-29 | 2022-05-17 | 浙江恒逸石化有限公司 | Antimony-free polyester melt preparation system and method for preparing antimony-free polyester fine denier FDY fiber |
| CN114481335A (en) * | 2021-12-17 | 2022-05-13 | 桐昆集团浙江恒通化纤有限公司 | High-strength sunlight-resistant anti-aging terylene pre-oriented yarn for curtain and preparation method thereof |
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Application publication date: 20130918 |