CN1313512C - Process of preparing polyester slices for high transparent energy saving film - Google Patents
Process of preparing polyester slices for high transparent energy saving film Download PDFInfo
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- CN1313512C CN1313512C CNB2005100400414A CN200510040041A CN1313512C CN 1313512 C CN1313512 C CN 1313512C CN B2005100400414 A CNB2005100400414 A CN B2005100400414A CN 200510040041 A CN200510040041 A CN 200510040041A CN 1313512 C CN1313512 C CN 1313512C
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- China
- Prior art keywords
- kettle
- slurry
- red
- blue agent
- blue
- 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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- 229920000728 polyester Polymers 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 45
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000032050 esterification Effects 0.000 claims abstract description 19
- 238000005886 esterification reaction Methods 0.000 claims abstract description 19
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000002347 injection Methods 0.000 claims description 13
- 239000007924 injection Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 10
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 235000019239 indanthrene blue RS Nutrition 0.000 claims description 2
- UHOKSCJSTAHBSO-UHFFFAOYSA-N indanthrone blue Chemical compound C1=CC=C2C(=O)C3=CC=C4NC5=C6C(=O)C7=CC=CC=C7C(=O)C6=CC=C5NC4=C3C(=O)C2=C1 UHOKSCJSTAHBSO-UHFFFAOYSA-N 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 229940011182 cobalt acetate Drugs 0.000 abstract 3
- 239000010408 film Substances 0.000 abstract 3
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 abstract 3
- 239000008187 granular material Substances 0.000 abstract 1
- 150000001455 metallic ions Chemical class 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- -1 polyethylene terephthalate Polymers 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
Images
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- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to a method for preparing polyester slices for a high transparent energy saving film. The method comprises the steps: benzenethiol and ethylene glycol are stirred in a slurry mixing tank, slurry is pumped into a slurry feeding tank and enters an esterification kettle, and blue agents or/and red agents are added into the slurry before or/and after the slurry enters the esterification kettle; esterified oligomer and each additive on a pipeline are injected into a pre-polymerization kettle; when the material reaches the upper part of the pre-polymerization kettle, the material flows to a final polymerization kettle; after the final polymerization is carried out, band heads are removed, and the product reaches a granule cutter. The method is characterized in that the oligomer pipeline behind the esterification kettle is added with trace cobalt acetate which replaces parts of the blue agents or/and the red agents for toning, the cobalt content in the slices is controlled to less than 10 PPM, and the molecular formula of the cobalt acetate is CO (CH3COO)2.4H2O. As the oligomer pipeline behind the esterification kettle is added with the trace cobalt acetate which replaces parts of the blue agents or/and the red agents for toning, metallic ions in the slices are increased, and the resistance is small at thin film coiling time and electrostatic adsorption time. The film can be drawn at high speed, and the film has the advantages of good attaching property, low energy consumption, energy saving and high transparency.
Description
Technical field:
The present invention relates to the preparation method of a kind of energy-saving film with polyester slice.Especially relate to and a kind ofly can enhance the transparency and the preparation method of the polyethylene terephthalate of membrane speed.
Background technology:
Polyethylene terephthalate is mainly used in the base-material production of film grade pet chip, bottle grade pet chip and fibre-grade section.Its technological process of production is:
Pure terephthalic acid and ethylene glycol stir by density of setting or mol ratio in slurry mix tank, temperature is about 65 ℃, be pumped into the slurry feeding tank, the slurry feeding tank enters esterifying kettle through pump by the slurry injection nozzle, under about 275 ℃ temperature condition, by the circulation of thermosiphon, slurry in esterifying kettle, be uniformly mixed react oligopolymer, before esterifying kettle or/and blue agent is added in the back red dose, reacted water byproduct and oligopolymer are isolated through the esterification knockout tower.The oligopolymer that generates after the esterification injects prepolymerization kettle by the injection ratio of setting through toothed gear pump together with each additive on the pipeline.Prepolymerization kettle is a upflowing big gun cover tower, and temperature of reaction is at 280～290 ℃, and absolute pressure 19～20mmHg flows to terminal polymerization kettle after material arrives the prepolymerization kettle top.The temperature of reaction of terminal polymerization kettle is 285～295 ℃, absolute pressure≤1.3mmHg, and the online adjusting viscosity of online oscillation viscometer set(ting)value is set according to the chemical examination measured data.Product after poly-eventually goes end of extruded band to make section to dicing machine after fondant filter filters.It mainly has the following disadvantages:
Because the metal ion that contains is less in the section, during the film processed rolling when electrostatic adhesion resistance big, pasting property of film difference and can not the high speed membrane, the energy consumption height, transparency is low.
Summary of the invention:
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of can enhance the transparency and the energy-saving film of membrane speed with the preparation method of polyester slice.
The object of the present invention is achieved like this: a kind of energy-saving film preparation method of polyester slice; its processing step comprises: terephthalic acid and ethylene glycol stir by proportioning in slurry mix tank; be pumped into the slurry feeding tank; enter esterifying kettle through the slurry injection nozzle again; circulation by thermosiphon; slurry in esterifying kettle, be uniformly mixed react oligopolymer; before esterifying kettle or/and blue agent is added or/and red dose in the back; and control blue agent or/and the red dose of content＜1PPM in section; oligopolymer after pump is with esterification injects prepolymerization kettle together with each additive on the pipeline; after arriving the prepolymerization kettle top, material flows to terminal polymerization kettle; product after poly-eventually is after fondant filter filters; go end of extruded band to dicing machine, the temperature of reaction of esterification is at 260～280 ℃, and the prepolymerization reaction temperature is at 280～290 ℃; absolute pressure 19～20mmHg; the temperature of reaction of terminal polymerization kettle is 285～295 ℃, absolute pressure≤1.3mmHg, and the structural formula of its medium blue agent and red dose is respectively:
Red dose of blue agent
It is characterized in that: on the oligopolymer pipeline behind the esterifying kettle, add the acetate in minute cobalt, substitute a part of blue agent or/and red dose of toning, and the content＜10PPM of control cobalt in section, the molecular formula of Cobaltous diacetate is Co (CH
3COO)
24H
2O.
Because the present invention adds the acetate in minute cobalt on the oligopolymer pipeline behind the esterifying kettle, to substitute a part of blue agent or/and red dose of toning, therefore increased the metal ion in the section, during the film processed rolling when electrostatic adhesion resistance little, pasting property of film good and can high speed membrane, the transparency height, energy consumption is low, and is energy-conservation.
Cobaltous diacetate of the present invention substitutes or does not substitute the blue agent of part or/and being compared as follows after red dose:
| Content | Product of the present invention | Other products |
| Membrane speed | More than the 300m/min | 260～280m/min |
| Fondant filter filter core switching cycle | 80 days | 60 days |
The present invention has finally improved quality product by the improvement to " three stills " technical process, has under equal conditions obtained positively effect: increase membrane speed, prevent aspects such as rupture of membranes; The client shortens the production cycle for the downstream, has saved cost.In addition, the fondant filter switching cycle obviously prolongs.
Description of drawings:
Fig. 1 is added in the technological process of production figure of the oligopolymer pipeline behind the esterifying kettle for Cobaltous diacetate of the present invention.
Embodiment:
The present invention relates to a kind of preparation method that can improve the polyethylene terephthalate of membrane speed.Its technical process is referring to Fig. 1:
Terephthalic acid and ethylene glycol stir by density of setting or mol ratio in slurry mix tank, temperature is about 65 ℃, be pumped into the slurry feeding tank, slurry in the slurry feeding tank enters esterifying kettle through pump by the slurry injection nozzle, under 260～280 ℃ temperature condition, by the circulation of thermosiphon, the slurry reaction that in esterifying kettle, is uniformly mixed, reacted water byproduct and oligopolymer are isolated through the esterification knockout tower.The oligopolymer that generates after the esterification by the injection ratio of setting, injects prepolymerization kettle through toothed gear pump together with each additive on the pipeline (comprising Cobaltous diacetate and blue agent or/and red dose).Prepolymerization kettle is a upflowing big gun cover tower, and temperature of reaction is at 280～290 ℃, and absolute pressure 19～20mmHg flows to terminal polymerization kettle after material arrives the prepolymerization kettle top.The temperature of reaction of terminal polymerization kettle is 285～295 ℃, absolute pressure≤1.3mmHg, and the online adjusting viscosity of online oscillation viscometer set(ting)value is set according to the chemical examination measured data.Product after poly-eventually goes end of extruded band to dicing machine after fondant filter filters.Wherein, blue agent or/and red dose before esterifying kettle or/and add the back, and control its content＜1PPM in section; The acetate in minute cobalt adds on the oligopolymer pipeline behind the esterifying kettle, to substitute a part of blue agent or/and red dose of toning, and the content＜10PPM of control cobalt in section.Blue agent and red dose of structural formula are respectively:
Red dose of blue agent
The molecular formula of Cobaltous diacetate is Co (CH
3COO)
24H
2O.
Blue agent of the present invention and red dose of proportioning are 1.5～2.5: 1.Being with blue agent is mixed with mixed solution or/and red dose of powder adds earlier to stir in the part ethylene glycol, reinjects.
The Cobaltous diacetate that the present invention injects is the Cobaltous diacetate powder to be added part ethylene glycol earlier stir that to be mixed with concentration be mixed solution, reinjects.
Embodiment 1:
Cobaltous diacetate is injected into oligopolymer pipeline behind the esterifying kettle by 0.0025 ratio, and by the injection of 0.0025 ratio, esterification temperature is 270 ℃ in the slurry feeding tank for blue agent and red dose, the precondensation temperature is 285 ℃, absolute pressure 19～20mmHg, eventually poly-temperature is 287 ℃, absolute pressure≤1.3mmHg.The Cobaltous diacetate matched proportion density is 1.523%; Blue/blue agent of matched proportion density of red dose is 145ppm, and red dose is 72ppm.The mol ratio of blue agent and red dose is 1.5: 1.Wherein cobalt, blue agent and the red dose of content in section are respectively 9ppm, 0.36ppm and 0.18ppm.
Embodiment 2:
Cobaltous diacetate is injected into oligopolymer pipeline behind the esterifying kettle by 0.0020 ratio, and by the injection of 0.0030 ratio, esterification temperature is 260 ℃ in the slurry feeding tank in blue agent, the precondensation temperature is 290 ℃, absolute pressure 20mmHg, eventually poly-temperature is 285 ℃, absolute pressure≤1.3mmHg.The Cobaltous diacetate matched proportion density is 1.5%; The matched proportion density of blue agent is 145ppm.Wherein cobalt and the content of blue agent in section are respectively 7.2ppm and 0.36ppm.
Embodiment 3:
Cobaltous diacetate is injected into oligopolymer pipeline behind the esterifying kettle by 0.0015 ratio, red dose in the slurry feeding tank by the injection of 0.0028 ratio, esterification temperature is 280 ℃, the precondensation temperature is 280 ℃, absolute pressure 19.5mmHg, eventually poly-temperature is 295 ℃, absolute pressure≤1.3mmHg.The Cobaltous diacetate matched proportion density is 1.6%; Red dose matched proportion density is 72ppm.Wherein cobalt and the red dose of content in section are respectively 5.4ppm and 0.18ppm.
Embodiment 4:
Cobaltous diacetate is injected into oligopolymer pipeline behind the esterifying kettle by 0.0020 ratio, and by the injection of 0.0026 ratio, wherein cobalt, blue agent and the red dose of content in section are respectively 7.2ppm, 0.36ppm and 0.18ppm in the slurry feeding tank for blue agent and red dose.All the other are with example 1.
Embodiment 5:
Cobaltous diacetate is injected into oligopolymer pipeline behind the esterifying kettle by 0.0025 ratio, and by the injection of 0.0035 ratio, all the other are with example 1 on the oligopolymer pipeline between reaction kettle of the esterification and precondensation for blue agent and red dose.
Embodiment 6:
Cobaltous diacetate is injected into oligopolymer pipeline behind the esterifying kettle by 0.0025 ratio, and by the injection of 0.0030 ratio, all the other are with example 2 on the oligopolymer pipeline between reaction kettle of the esterification and precondensation in blue agent.
Embodiment 7:
Cobaltous diacetate is injected into the oligopolymer pipeline by 0.0020 ratio, injects by 0.0028 ratio on the oligopolymer pipeline between esterification and precondensation for red dose, and all the other are with example 3.
Embodiment 8:
Cobaltous diacetate is injected into oligopolymer pipeline behind the esterifying kettle by 0.0015 ratio, and by the injection of 0.0026 ratio, all the other are with example 4 on the oligopolymer pipeline between esterification and precondensation for blue agent and red dose.
Cobaltous diacetate of the present invention substitutes or does not substitute the blue agent of part or/and being compared as follows after red dose:
| Do not add blue agent, red dose and Cobaltous diacetate | Add blue agent, red dose, do not add Cobaltous diacetate | Do not add blue agent, red dose, add Cobaltous diacetate | Add blue agent, red dose and Cobaltous diacetate | |
| The L value | 68～70 | 64～67 | 60～63 | 63～65 |
| The b value | 5～6 | 2～3 | 2～3 | 2～3 |
| The a value | -2.3～-2.5 | -3.3～-3.5 | -1.8～-2.2 | -2.8～-3.2 |
Annotate: the L value is big more, and it is white more, bright more to cut into slices, good luster, transparency height.The b value is blue to yellow degree.The a value is green to red degree.For guaranteeing the whiteness of section, can not add Cobaltous diacetate separately.
Claims (4)
1; a kind of energy-saving film preparation method of polyester slice; its processing step comprises: terephthalic acid and ethylene glycol stir by proportioning in slurry mix tank; be pumped into the slurry feeding tank; enter esterifying kettle through the slurry injection nozzle again; circulation by thermosiphon; slurry in esterifying kettle, be uniformly mixed react oligopolymer; before esterifying kettle or/and blue agent is added or/and red dose in the back; and control blue agent or/and the red dose of content＜1PPM in section; oligopolymer after pump is with esterification injects prepolymerization kettle together with each additive on the pipeline; after arriving the prepolymerization kettle top, material flows to terminal polymerization kettle; product after poly-eventually filters the back to dicing machine; the temperature of reaction of esterification is at 260～280 ℃; the prepolymerization reaction temperature is at 280～290 ℃, absolute pressure 19～20mmHg, and the temperature of reaction of terminal polymerization kettle is 285～295 ℃; absolute pressure≤1.3mmHg, the structural formula of its medium blue agent and red dose is respectively:
Red dose of blue agent
It is characterized in that: on the oligopolymer pipeline behind the esterifying kettle, add the acetate in minute cobalt, substitute a part of blue agent or/and red dose of toning, and the content＜10PPM of control cobalt in section, the molecular formula of Cobaltous diacetate is Co (CH
3COO)
24H
2O.
2, a kind of energy-saving film according to claim 1 preparation method of polyester slice, it is characterized in that: blue agent and red dose of proportioning are 1.5～2.5: 1.
3, a kind of energy-saving film according to claim 2 preparation method of polyester slice is characterized in that: being with blue agent is mixed with mixed solution or/and red dose of powder adds earlier to stir in the part ethylene glycol, reinjects.
4, a kind of energy-saving film according to claim 2 is characterized in that with the preparation method of polyester slice: be the Cobaltous diacetate powder to be added earlier stir in the part ethylene glycol that to be mixed with concentration be mixed solution, reinject.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100400414A CN1313512C (en) | 2005-05-17 | 2005-05-17 | Process of preparing polyester slices for high transparent energy saving film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100400414A CN1313512C (en) | 2005-05-17 | 2005-05-17 | Process of preparing polyester slices for high transparent energy saving film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1693335A CN1693335A (en) | 2005-11-09 |
| CN1313512C true CN1313512C (en) | 2007-05-02 |
Family
ID=35352476
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100400414A Expired - Fee Related CN1313512C (en) | 2005-05-17 | 2005-05-17 | Process of preparing polyester slices for high transparent energy saving film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1313512C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100497435C (en) * | 2007-07-03 | 2009-06-10 | 卞平芳 | Method for preparing polyethylene terephthalate capable of effectively control products terminal carboxyl group |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4745174A (en) * | 1987-04-23 | 1988-05-17 | Eastman Kodak Company | Polyesters having improved whiteness |
| US5372864A (en) * | 1993-09-03 | 1994-12-13 | Eastman Chemical Company | Toners for polyesters |
| CN1139678A (en) * | 1995-07-04 | 1997-01-08 | 天津石油化工公司涤纶厂 | Production method of polyester for high-transparency ultra-thin film |
| CN1244545A (en) * | 1998-08-12 | 2000-02-16 | 天津石油化工公司研究所 | Preparation of violet ray resistant polyester |
| CN1422885A (en) * | 2001-02-27 | 2003-06-11 | 天津石油化工公司化纤厂 | New-type polyester continuous polymerization catalytic-stabilizing method |
| US6835333B2 (en) * | 2002-05-07 | 2004-12-28 | Milliken & Company | Combinations for use as toners in polyesters |
-
2005
- 2005-05-17 CN CNB2005100400414A patent/CN1313512C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4745174A (en) * | 1987-04-23 | 1988-05-17 | Eastman Kodak Company | Polyesters having improved whiteness |
| US5372864A (en) * | 1993-09-03 | 1994-12-13 | Eastman Chemical Company | Toners for polyesters |
| US5384377A (en) * | 1993-09-03 | 1995-01-24 | Eastman Chemical Company | Toners for polyesters |
| CN1139678A (en) * | 1995-07-04 | 1997-01-08 | 天津石油化工公司涤纶厂 | Production method of polyester for high-transparency ultra-thin film |
| CN1244545A (en) * | 1998-08-12 | 2000-02-16 | 天津石油化工公司研究所 | Preparation of violet ray resistant polyester |
| CN1422885A (en) * | 2001-02-27 | 2003-06-11 | 天津石油化工公司化纤厂 | New-type polyester continuous polymerization catalytic-stabilizing method |
| US6835333B2 (en) * | 2002-05-07 | 2004-12-28 | Milliken & Company | Combinations for use as toners in polyesters |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1693335A (en) | 2005-11-09 |
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Effective date of registration: 20090220 Address after: Jiangsu city in Jiangyin Province town of Zhouzhuang Shanyou No. 1 Patentee after: Jiangyin Jihua New Material Co., Ltd. Address before: The town of Zhouzhuang village in Jiangsu Province, Jiangyin city Sanfangxiang No. 6 Patentee before: Xue Jiliang |
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