CN102181046A - Preparation method of polyester chips for tangle film - Google Patents
Preparation method of polyester chips for tangle film Download PDFInfo
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- CN102181046A CN102181046A CN2011100525468A CN201110052546A CN102181046A CN 102181046 A CN102181046 A CN 102181046A CN 2011100525468 A CN2011100525468 A CN 2011100525468A CN 201110052546 A CN201110052546 A CN 201110052546A CN 102181046 A CN102181046 A CN 102181046A
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Abstract
The invention discloses a preparation method of polyester chips for a tangle film. The method comprises the following steps of: adding ethylene glycol into a beating kettle, and adding terephthalic acid and iso-phthalic acid to prepare slurry; adding ethylene glycol into a catalyst preparation kettle, then adding an antimonous oxide catalyst, and stirring uniformly to prepare catalyst solution; adding ethylene glycol into an additive preparation kettle, then adding silicon dioxide, and stirring uniformly to prepare additive solution; adding the slurry and the catalyst solution into an esterification kettle, heating, and performing esterification reaction to obtain an esterification product; pressing the esterification product into a pre-condensation polymerization kettle, simultaneously pressing the additive solution, vacuumizing the pre-condensation polymerization reaction process, and discharging the excessive ethylene glycol; pressing the pre-condensation polymerization product to a final condensation polymerization kettle to obtain a melt; cooling and slicing the melt; conveying the slices to a crystallizer, heating the slices to the temperature of between 150 and 160 DEG C, and performing crystallization; then conveying the slices to a solid phase reactor, vacuumizing and heating to further increase the viscosity; and discharging and packing. The prepared slices improve the resilience of the polyester film.
Description
Technical field
The present invention relates to a kind of preparation method of polyester slice, particularly a kind of torsion film preparation method of polyester slice.
Background technology
At present, the torsion film of packaged confectionary or fruit generally uses glassine paper, PVC torsion film and PET torsion film, involving great expense of glassine paper, cost is very high, not large batch of as yet at home popularization and application, and if use the PVC torsion film, then have food safety hidden danger, because though the PVC film has good acid-fast alkali-proof, but, be heated and the situation of illumination under, the PVC film can decompose and discharges deleterious muriate, wherein may comprise strong carcinogenic substance two dislike because of, therefore, the application of PVC torsion film aspect food product pack is restricted day by day, and the PET torsion film then has safety, the superiority that transparency is high, it is receiving concern more and more widely.
The polyester slice that present China is produced is general purpose grade mostly, and rebound resilience is relatively poor, and when being applied to the food product pack field, effect is not fine.The torsion film polyester slice of the present invention's preparation will effectively solve polyester film rebound resilience problem exactly, to substitute the PVC film more.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of torsion film with polyester slice.
The technical scheme that the inventive method is taked is:
A kind of torsion film preparation method of polyester slice may further comprise the steps:
1) with ethylene glycol input making beating still, adds terephthalic acid, m-phthalic acid then, make slurries;
2) ethylene glycol is dropped into the catalyst preparation still, add The catalytic antimony trioxide then, stir and make catalyzer liquid; Ethylene glycol is dropped into additive preparation still, add silicon-dioxide then, stir and make additive liquid;
3) slurries and catalyzer liquid are dropped into esterifying kettle, esterification is carried out in heating, obtains carboxylate;
4) after the esterification carboxylate is pressed into the preshrunk still, is pressed into additive liquid simultaneously, vacuumize in the prepolymerization reaction process, excessive ethylene glycol is discharged;
5) product with precondensation is pressed into whole polycondensation vessel, further carry out final minification poly-react to the polymerization degree be 90-110, obtain melt;
6) with melt cooling, section;
7) section is delivered in the crystallizer, is heated to 150～160 ℃, crystallization;
8) be delivered to solid phase reactor then, vacuumize and heat, further increase viscosity;
9) discharging, packing.
The add-on of m-phthalic acid is 10～20% of a raw materials quality.
The consumption of silicon-dioxide is 0.1～0.2% of a raw material total mass.
The total consumption of terephthalic acid and m-phthalic acid and the consumption mol ratio of ethylene glycol are 1:1.2～1.3.
The consumption of antimonous oxide is 0.03～0.04% of a raw material total mass.
Esterification reaction temperature is 250～255 ℃.
The prepolymerization reaction temperature is 255～260 ℃.
The poly-temperature of reaction of final minification is 280～285 ℃.
The tackify temperature is 230～235 ℃.
The invention has the beneficial effects as follows: polyester slice prepared according to the methods of the invention, product has not only kept the physical chemistry mechanical property of original polyester slice, and improved the rebound resilience of polyester film greatly, not only reach customer requirement aspect rebound resilience, PET also can replace the PVC torsion film as a kind of feature of environmental protection material simultaneously.Product has been filled up domestic blank, and quality reaches international like product level.
Embodiment
Below in conjunction with example, further specify the present invention.
In following examples, per 100 liters of ethylene glycol are equivalent to about 1820mol ethylene glycol; Every 100kg terephthalic acid and m-phthalic acid are equivalent to about 600mol terephthalic acid.
1) with 1540～1700 liters of ethylene glycol input making beating stills, adds terephthalic acid and m-phthalic acid that total mass is 4400kg then, make slurries;
2) 100 liters of ethylene glycol are dropped into the catalyst preparation still, add the antimonous oxide that accounts for raw material total mass 0.03～0.04% then, stir and make catalyzer liquid;
3) will account for the silicon-dioxide of raw material total mass 0.1～0.2%, mix, make additive liquid with 100 liters of ethylene glycol;
4) slurries and catalyzer liquid are dropped into esterifying kettle, be heated to 250～255 ℃ and carry out esterification, stir in the process of reaction, reaction 3.5～4.5h obtains carboxylate;
5) after the esterification, carboxylate is pressed into the preshrunk still, adds additive liquid, be heated to 255～260 ℃ of reaction 0.8～1.2h, vacuumize in the reaction process, excessive ethylene glycol is discharged;
6) product with precondensation is pressed into whole polycondensation vessel, is heated to 280～285 ℃, reacts 4.5～5.0 hours, obtains melt;
7) with melt cooling, section;
8) section is delivered in the crystallizer, is heated to 150～160 ℃, crystallization, crystallization time is 12 hours;
9) be delivered to solid phase reactor then, vacuumize and heat, further increase viscosity;
10) discharging, packing.
Sample (the long 150mm of sample that makes at last according to the canonical measure polyester slice of GB/T1040.3-2006, the long strip shape of wide l5mm ± 0.1mm) Young's modulus, its Young's modulus is more than 3500MPa, be that it has bigger intensity in the elastic deformation scope, in other words, its rebound resilience is better.
Adopt standard GB/T17932--1999 " film grade polyester chip ", the product of the inventive method preparation is tested, Comparative Examples is the torsion film polyester slice of Japanese Supreme Being people company, and the result is as shown in the table.
Table 1, product performance comparison sheet:
From the table data as can be seen, the present invention has met or exceeded external like product, superior performance fully can import substitutes.The polyester slice of the inventive method preparation can satisfy the specific demand of packing aspect fully.
Claims (9)
1. a torsion film may further comprise the steps with the preparation method of polyester slice:
1) with ethylene glycol input making beating still, adds terephthalic acid, m-phthalic acid then, make slurries;
2) ethylene glycol is dropped into the catalyst preparation still, add The catalytic antimony trioxide then, stir and make catalyzer liquid; Ethylene glycol is dropped into additive preparation still, add silicon-dioxide then, stir and make additive liquid;
3) slurries and catalyzer liquid are dropped into esterifying kettle, esterification is carried out in heating, obtains carboxylate;
4) after the esterification carboxylate is pressed into the precondensation still, is pressed into additive liquid simultaneously, vacuumize in the prepolymerization reaction process, excessive ethylene glycol is discharged;
5) product with precondensation is pressed into whole polycondensation vessel, further carry out final minification poly-react to the polymerization degree be 90-110, obtain melt;
6) with melt cooling, section;
7) section is delivered in the crystallizer, is heated to 150～160 ℃, crystallization;
8) be delivered to solid phase reactor then, vacuumize and heat, further increase viscosity;
9) discharging, packing.
2. a kind of torsion film according to claim 1 preparation method of polyester slice, it is characterized in that: the add-on of m-phthalic acid is 10～20% of a raw materials quality.
3. a kind of torsion film according to claim 1 preparation method of polyester slice, it is characterized in that: the consumption of silicon-dioxide is 0.1～0.2% of a raw material total mass.
4. a kind of torsion film according to claim 1 preparation method of polyester slice, it is characterized in that: the total consumption of terephthalic acid and m-phthalic acid and the consumption mol ratio of ethylene glycol are 1:1.2～1.3.
5. a kind of torsion film according to claim 1 preparation method of polyester slice, it is characterized in that: the consumption of antimonous oxide is 0.03～0.04% of a raw material total mass.
6. a kind of torsion film according to claim 1 preparation method of polyester slice, it is characterized in that: esterification reaction temperature is 250～255 ℃.
7. a kind of torsion film according to claim 1 preparation method of polyester slice, it is characterized in that: the prepolymerization reaction temperature is 255～260 ℃.
8. a kind of torsion film according to claim 1 preparation method of polyester slice is characterized in that: the poly-temperature of reaction of final minification is 280～285 ℃.
9. a kind of torsion film according to claim 1 preparation method of polyester slice, it is characterized in that: the tackify temperature is 230～235 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100525468A CN102181046A (en) | 2011-03-05 | 2011-03-05 | Preparation method of polyester chips for tangle film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100525468A CN102181046A (en) | 2011-03-05 | 2011-03-05 | Preparation method of polyester chips for tangle film |
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| CN102181046A true CN102181046A (en) | 2011-09-14 |
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| CN2011100525468A Pending CN102181046A (en) | 2011-03-05 | 2011-03-05 | Preparation method of polyester chips for tangle film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665352A (en) * | 2013-12-27 | 2014-03-26 | 天津万华股份有限公司 | Preparation method of environment-friendly special modified polyester chip for iron coating |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57102317A (en) * | 1980-12-16 | 1982-06-25 | Gunze Ltd | Polyester based film for twist wrapping |
| JPH10139873A (en) * | 1996-09-12 | 1998-05-26 | Mitsui Chem Inc | Production of polyethylene terephthalate |
| CN1602330A (en) * | 2001-12-11 | 2005-03-30 | Skc株式会社 | Biaxially oriented polyester film |
| CN101100504A (en) * | 2006-07-07 | 2008-01-09 | 新疆屯河聚酯有限责任公司 | Low pressure resistant polyethylene terephthalate resin and producing method thereof |
| CN101130602A (en) * | 2006-08-22 | 2008-02-27 | 东丽纤维研究所（中国）有限公司 | Method for producing poly-p-benzene dicarboxylic acid trimethylene glycol ester |
| EP2143749A1 (en) * | 2008-07-12 | 2010-01-13 | Epc Industrial Engineering GmbH | Method for production of polyester, in particular linear polyester for textile threads, textile fibres and for bottles and assembly for carrying out the method |
| CN101787114A (en) * | 2010-02-09 | 2010-07-28 | 佛山鸿华聚酯切片有限公司 | Preparation method of special polyester chip for paper industry yarn |
-
2011
- 2011-03-05 CN CN2011100525468A patent/CN102181046A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57102317A (en) * | 1980-12-16 | 1982-06-25 | Gunze Ltd | Polyester based film for twist wrapping |
| JPH10139873A (en) * | 1996-09-12 | 1998-05-26 | Mitsui Chem Inc | Production of polyethylene terephthalate |
| CN1602330A (en) * | 2001-12-11 | 2005-03-30 | Skc株式会社 | Biaxially oriented polyester film |
| CN101100504A (en) * | 2006-07-07 | 2008-01-09 | 新疆屯河聚酯有限责任公司 | Low pressure resistant polyethylene terephthalate resin and producing method thereof |
| CN101130602A (en) * | 2006-08-22 | 2008-02-27 | 东丽纤维研究所（中国）有限公司 | Method for producing poly-p-benzene dicarboxylic acid trimethylene glycol ester |
| EP2143749A1 (en) * | 2008-07-12 | 2010-01-13 | Epc Industrial Engineering GmbH | Method for production of polyester, in particular linear polyester for textile threads, textile fibres and for bottles and assembly for carrying out the method |
| CN101787114A (en) * | 2010-02-09 | 2010-07-28 | 佛山鸿华聚酯切片有限公司 | Preparation method of special polyester chip for paper industry yarn |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665352A (en) * | 2013-12-27 | 2014-03-26 | 天津万华股份有限公司 | Preparation method of environment-friendly special modified polyester chip for iron coating |
| CN103665352B (en) * | 2013-12-27 | 2015-10-28 | 天津万华股份有限公司 | Environment-friendly type covers the preparation method of the dedicated modified polyester slice of iron |
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Application publication date: 20110914 |