CN117050284A - Polyester chip for producing single-sided heat-sealing film and preparation method thereof - Google Patents
Polyester chip for producing single-sided heat-sealing film and preparation method thereof Download PDFInfo
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- 238000007789 sealing Methods 0.000 title claims abstract description 52
- 229920000728 polyester Polymers 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000005886 esterification reaction Methods 0.000 claims abstract description 80
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 60
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 45
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 27
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims abstract description 19
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 18
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000003381 stabilizer Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000005266 casting Methods 0.000 claims abstract description 4
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 29
- 239000000377 silicon dioxide Substances 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000032050 esterification Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- WSXIMVDZMNWNRF-UHFFFAOYSA-N antimony;ethane-1,2-diol Chemical group [Sb].OCCO WSXIMVDZMNWNRF-UHFFFAOYSA-N 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000011268 mixed slurry Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000004537 pulping Methods 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical group COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000180 alkyd Polymers 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 abstract description 7
- 239000000543 intermediate Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 150000002148 esters Chemical class 0.000 abstract 3
- 239000000203 mixture Substances 0.000 abstract 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000155 melt Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 11
- 230000007547 defect Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 3
- 229940035437 1,3-propanediol Drugs 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 3
- 230000001360 synchronised effect Effects 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012775 heat-sealing material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a polyester chip for producing a single-sided heat-sealing film and a preparation method thereof, wherein a semi-continuous production synthesis device is adopted, terephthalic acid, ethylene glycol and a small amount of 1, 3-propylene glycol are added in a certain molar ratio in a single esterification reaction, and a first partial esterification reaction is carried out to generate an ester intermediate; adding isophthalic acid, diethylene glycol and 1, 4-cyclohexanedimethanol in a certain molar ratio in the di-esterification reaction to perform a second partial esterification reaction, and generating an ester intermediate; mixing the product of the first esterification reaction with the product of the second esterification reaction, continuing to react to generate a mixture of ester intermediates, adding a proper amount of modified silicon dioxide solution, a small amount of catalyst and stabilizer, introducing the mixture into a polycondensation reaction kettle through a melt filter after reaching a certain temperature, and synthesizing the target molecular polymer by controlling the temperature, the vacuum degree and the stirring power. The high-temperature melt passes through a casting belt head, underwater granulating equipment and drying equipment to obtain the polyester chip for producing the single-sided heat-sealing film.
Description
Technical Field
The invention relates to a polyester chip and a preparation method thereof, in particular to a polyester chip for producing a single-sided heat-sealing film and a preparation method thereof.
Background
The heat-sealing film is a very important direction of application of plastic film materials, is quite common in living aspects, but after the development and iteration of the heat-sealing film for many years, the main materials of the heat-sealing film always surround PE, PVC, EVA, PA, PP and the like, and the market of the heat-sealing film taking PET materials as the main materials is very little. And PET is an important environment-friendly engineering plastic, so that if the PET can be widely applied to the direction of heat-sealing films, the market of the heat-sealing films can be greatly enriched, and the influence on the environment in the using and recycling processes is reduced.
Disclosure of Invention
The invention aims to solve the technical problems of providing a polyester chip for producing a single-sided heat-sealing film and a preparation method thereof, and the heat-sealing film produced and processed by the polyester chip can realize excellent single-sided heat-sealing effect by matching with multi-layer coextrusion process treatment in the film drawing process, and the multi-layer coextrusion materials of the product are PET, so that the polyester chip has the same heat-sealing firmness as the material of the conventional heat-sealing film such as PVC, PP, PE, can be recycled in the later stage, and well solves the problem of environmental influence caused by the conventional heat-sealing film; furthermore, by introducing excellent opening agent, the problems of powder falling and heat sealing firmness attenuation in the common use process of the heat sealing film are well solved.
In order to realize the excellent characteristics of the product and to make up the defects of the existing processing technology and materials, the invention adopts the following technical scheme: a method for preparing a polyester chip for producing a single-sided heat-seal film, comprising the steps of:
(1) adding a certain amount of ethylene glycol and a small amount of 1, 3-propylene glycol into a pulping kettle, then adding a certain amount of terephthalic acid solid powder, preparing into viscous slurry, and pumping into an esterification reaction kettle through a slurry supply pump to start a first part of esterification reaction; wherein terephthalic acid accounts for 80-95% of the total acid mole ratio of the esterification reaction, ethylene glycol accounts for 80-93% of the total alcohol mole ratio of the esterification reaction, and 1, 3-propylene glycol accounts for 1-5% of the total alcohol mole ratio of the esterification reaction;
the reaction product was as follows:
wherein m: n= (16.8-88.5): 1
(2) Adding a certain amount of diethylene glycol and 1, 4-cyclohexanedimethanol solution into a feed port of a di-esterification reaction kettle, starting the di-esterification kettle to stir, adding a certain amount of isophthalic acid, capping the feed port, starting the temperature rise, and performing a second part of esterification reaction; wherein, the mole ratio of the intermediate phthalic acid to the total acid of the esterification reaction is 5-15%, the mole ratio of the diglycol to the total alcohol of the esterification reaction is 2-5%, and the mole ratio of the 1, 4-cyclohexanedimethanol to the total alcohol of the esterification reaction is 4-10%;
the reaction product was as follows:
wherein x: y=1: (1.5-2.7)
(3) After the raw materials added in (1) and (2) are reacted, introducing the esterified substance generated by the reaction in (1) into a di-esterification reaction kettle through a pipeline, mixing with the second part of esterified product in (2), starting the di-esterification kettle for stirring, heating to 230-250 ℃, uniformly adding the prepared silicon dioxide solution, and adding a proper amount of catalyst and stabilizer through an auxiliary agent port after the silicon dioxide solution is completely filled; the molar ratio of total acid to total alcohol of the two esterification reactions is 1: (1.15-1.35);
(4) after the reaction of the step (3) is finished and the temperature of the slurry is stabilized to 230-250 ℃, pressing the materials in the di-esterification reaction kettle into a polycondensation reaction kettle from high-purity nitrogen through a stainless steel filter with the diameter of 15-25 mu m;
(4) after the mixed slurry enters a polycondensation kettle, the temperature of the material is raised to 245-255 ℃, and the temperature is raised and the low vacuum is pumped; and (3) controlling the reaction temperature to 275-285 ℃ for negative pressure polymerization reaction, controlling stirring polycondensation current and power through equipment under the condition that the vacuum degree is less than or equal to 30Pa and the final temperature to 275-285 ℃, synthesizing a high-viscosity polyester slice melt with the intrinsic viscosity of 0.660-0.680dl/g, and finally obtaining the polyester slice for producing the single-sided heat-sealing film through a belt casting head, an underwater granulator, a dryer and a vibrating screen.
The preparation method of the polyester chip for producing the single-sided heat-sealing film is characterized in that the molar ratio of the first part of esterification to the second part of esterification reaction alkyd is required to be more than 1, so that the acid esterification is ensured to be complete; the first part of the esterification reaction requires the reaction temperature to be controlled between 245 and 265 ℃, and the second part of the esterification reaction requires the reaction temperature to be controlled between 190 and 220 ℃.
The catalyst is ethylene glycol antimony, and the addition amount is 400-600ppm of the theoretical polyester chip yield; the stabilizer is trimethyl phosphate, and the addition amount is 50-100ppm of the theoretical polyester chip yield.
The silica solution is prepared by dispersing a certain amount of silica solids in a certain amount of glycol solution to prepare uniform slurry with the mass concentration of 5-15%, wherein the amount of the added silica solids is 0.03% -0.15% of the theoretical polyester chip yield; the silica solids used are required to have a median particle diameter of 1.0 μm and a normal particle diameter distribution of not more than 0.2 μm, i.e., a particle diameter in the range of 0.8 to 2.2 μm, are highly concentrated, and are subjected to an amino coating treatment.
The polyester chip for producing the single-sided heat-sealing film is prepared by the preparation method.
The beneficial effects of the invention are as follows:
1. through two parts of synchronous esterification reaction, a target monomer can be formed according to the reaction preset, wherein the first part of esterification reaction forms an initial skeleton of a high polymer, and the second part of esterification reaction forms a modified polyester chain segment, so that after materials are conveniently mixed, the polymer skeleton is connected in a polycondensation reaction stage, and uniform high polymer chains can be formed, and the consistency and uniformity of product characteristics are ensured;
2. the diethylene glycol is introduced to replace the traditional ethylene glycol, so that the fluidity of the polyester chip after being processed into a film can be greatly improved, the fluidity guarantee is provided for the subsequent realization of lower-temperature adhesion, the contact and fusion area of materials in fixed heat sealing heating time is increased, and the firmness guarantee is provided;
3. by introducing a proper amount of 1, 3-propanediol monomer, 1, 4-cyclohexanedimethanol and isophthalic acid, the melting point of the polyester chip is greatly reduced by utilizing the synergistic effect of the three, a necessary structural basis is provided for realizing low-temperature heat sealing, and meanwhile, the polyester chip is also a determining factor for replacing PVC, PE, PP and other traditional heat sealing materials;
4. the opening performance of the subsequent film drawing can be greatly improved by introducing the silica subjected to specific treatment, meanwhile, the added silica has the excellent characteristic of extremely narrow particle size distribution, so that powerful guarantee is provided for uniformity of the film surface, and the silica can be better integrated with the heat-sealing film through organic treatment, is not easy to fall off, and does not have the defect that the traditional opening agent is used for a long time to fall off powder.
Detailed Description
The invention is described in further detail below in connection with the following detailed description:
the invention relates to a preparation method of a polyester chip for producing a single-sided heat-sealing film, which comprises the following steps:
(1) adding a certain amount of ethylene glycol and a small amount of 1, 3-propylene glycol into a pulping kettle, then adding a certain amount of terephthalic acid solid powder, preparing into viscous slurry, and pumping into an esterification reaction kettle through a slurry supply pump to start a first part of esterification reaction; wherein terephthalic acid accounts for 80-95% of the total acid mole ratio of the esterification reaction, ethylene glycol accounts for 80-93% of the total alcohol mole ratio of the esterification reaction, and 1, 3-propylene glycol accounts for 1-5% of the total alcohol mole ratio of the esterification reaction;
(2) adding a certain amount of diethylene glycol and 1, 4-cyclohexanedimethanol solution into a feed port of a di-esterification reaction kettle, starting the di-esterification kettle to stir, adding a certain amount of isophthalic acid, capping the feed port, starting the temperature rise, and performing a second part of esterification reaction; wherein, the mole ratio of the intermediate phthalic acid to the total acid of the esterification reaction is 5-15%, the mole ratio of the diglycol to the total alcohol of the esterification reaction is 2-5%, and the mole ratio of the 1, 4-cyclohexanedimethanol to the total alcohol of the esterification reaction is 4-10%;
(3) after the raw materials added in (1) and (2) are reacted, introducing the esterified substance generated by the reaction in (1) into a di-esterification reaction kettle through a pipeline, mixing with the second part of esterified product in (2), starting the di-esterification kettle for stirring, heating to 230-250 ℃, uniformly adding the prepared silicon dioxide solution, and adding a proper amount of catalyst and stabilizer through an auxiliary agent port after the silicon dioxide solution is completely filled; the molar ratio of total acid to total alcohol of the two esterification reactions is 1: (1.15-1.35);
(4) after the reaction of the step (3) is finished and the temperature of the slurry is stabilized to 230-250 ℃, pressing the materials in the di-esterification reaction kettle into a polycondensation reaction kettle from high-purity nitrogen through a stainless steel filter with the diameter of 15-25 mu m;
(4) after the mixed slurry enters a polycondensation kettle, the temperature of the material is raised to 245-255 ℃, and the temperature is raised and the low vacuum is pumped; and (3) controlling the reaction temperature to 275-285 ℃ for negative pressure polymerization reaction, controlling stirring polycondensation current and power through equipment under the condition that the vacuum degree is less than or equal to 30Pa and the final temperature to 275-285 ℃, synthesizing a high-viscosity polyester slice melt with the intrinsic viscosity of 0.660-0.680dl/g, and finally obtaining the polyester slice for producing the single-sided heat-sealing film through a belt casting head, an underwater granulator, a dryer and a vibrating screen.
The molar ratio of the first part of esterification to the second part of esterification reaction alkyd is required to be more than 1, so that the acid esterification is ensured to be complete; the first part of the esterification reaction requires the reaction temperature to be controlled between 245 and 265 ℃, and the second part of the esterification reaction requires the reaction temperature to be controlled between 190 and 220 ℃.
The catalyst used in the synthesis process is ethylene glycol antimony, and the addition amount is 400-600ppm of the theoretical polyester chip yield; the stabilizer is trimethyl phosphate and the addition amount is 50-100ppm of theoretical polyester chip yield.
The silica solution mentioned in the synthesis process is prepared by dispersing a certain amount of silica solids in a certain amount of glycol solution to prepare uniform slurry with the mass concentration of 5-15%, wherein the amount of the added silica solids is 0.03% -0.15% of the theoretical polyester chip yield; the silica solids used are required to have a median particle diameter of 1.0 μm and a normal particle diameter distribution of not more than 0.2 μm, i.e., a particle diameter in the range of 0.8 to 2.2 μm, are highly concentrated, and are subjected to an amino coating treatment.
The polyester chip for producing the single-sided heat-sealing film is finally prepared by the preparation method.
Compared with the heat-sealing film processed and produced by the product, the heat-sealing film made of the conventional material has the following main defects:
1. the conventional heat-sealing film drawing process is more complex, multiple layers and multiple materials are generally required to be compounded, the requirements on film drawing equipment and process control are more severe, and the film forming difficulty is high;
2. the heat sealing film made of the conventional material is compounded by single material or multiple materials, particularly the multiple materials, is difficult to recycle after being used later, has a great discount on environmental protection property compared with the heat sealing film made of PET material, has poor environmental friendliness, and is a waste of materials due to difficult recycling;
3. the heat sealing film made of the conventional material is required to realize single-sided heat sealing by complex compounding, coating and the like, and the heat sealing film produced by the product can realize excellent single-sided heat sealing by only utilizing the most common BOPET film production line to carry out multi-layer PET material melting coextrusion;
4. the conventional heat-sealing film has the defects of poor uniformity, poor opening effect, repeated processing or powder falling during use.
The polyester chip prepared by the invention solves the problems of using pain and difficulty, and synchronous control of various indexes is needed to be implemented in the synthesis of the product of the invention:
1. stable chain structure and uniform performance
The target monomer can be formed according to the reaction preset by controlling the synchronous esterification reaction of the two parts, wherein the first part of the esterification reaction forms an initial skeleton of the high polymer, and the second part of the esterification reaction forms a modified polyester chain segment, so that after materials are conveniently mixed, the polymer skeleton is connected in the polycondensation reaction stage, and uniform high polymer chains can be formed, and the consistency and uniformity of the product characteristics are ensured;
2. excellent heat sealability and heat seal strength
The diethylene glycol is introduced to replace the traditional ethylene glycol, so that the fluidity of the polyester chip after being processed into a film can be greatly improved, the fluidity guarantee is provided for the subsequent realization of lower-temperature adhesion, the contact and fusion area of materials in fixed heat sealing heating time is increased, and the firmness guarantee is provided;
3. heat sealing temperature comparable to the bid:
by introducing a proper amount of 1, 3-propanediol monomer, 1, 4-cyclohexanedimethanol and isophthalic acid, the melting point of the polyester chip is greatly reduced by utilizing the synergistic effect of the three, and the lowest melting point of the product can be reduced to about 150 ℃ from about 260 ℃ in the prior art, so that necessary conditions are provided for realizing low-temperature heat sealing, and convenience is provided for early popularization of the product;
4. stable film face opening performance:
through introducing the silica through specific treatment, the opening performance of the subsequent film drawing can be greatly improved, meanwhile, the added silica has the excellent characteristic of extremely narrow particle size distribution, the uniformity of the film surface is effectively ensured, and the silica can be better integrated with a heat sealing film through organic treatment, is not easy to deviate from, does not have the defect that the traditional opening agent is used for a long time to fall off powder, and indirectly improves the heat sealing effect in the use process.
Example 1
(1) Adding 800Kg of ethylene glycol and 35Kg of 1, 3-propylene glycol into a pulping kettle, then adding 1750Kg of terephthalic acid solid powder to prepare viscous slurry, and pumping into an esterification reaction kettle through a slurry supply pump to start a first part of esterification reaction;
(2) adding 55Kg of diethylene glycol and 160Kg of 1, 4-cyclohexanedimethanol solution into a feed port of a di-esterification reaction kettle, starting the di-esterification kettle to stir, then adding 250Kg of isophthalic acid, covering the feed port, starting heating, and carrying out a second part of esterification reaction; the method comprises the steps of carrying out a first treatment on the surface of the
(3) After the raw materials added in (1) and (2) are reacted, introducing the esterified substance generated by the reaction in (1) into a di-esterification reaction kettle through a pipeline, mixing with the second part of esterified product in (2), starting the di-esterification kettle to stir, heating to 240 ℃, uniformly adding 240Kg of prepared silicon dioxide solution with the solid content of 10%, and adding 1200g of ethylene glycol antimony catalyst and 200g of trimethyl phosphate stabilizer through an auxiliary agent port after the silicon dioxide solution is completely filled;
(4) after the reaction of the step (3) is finished and the temperature of the slurry is stabilized to 240 ℃, pressing the materials in the di-esterification reaction kettle into a polycondensation reaction kettle through a 25 mu m stainless steel filter by high-purity nitrogen;
(4) after the mixed slurry enters a polycondensation kettle, the temperature of the material is raised to 250 ℃, and the temperature is raised and the low vacuum is pumped; and (3) carrying out negative pressure polymerization reaction at the final reaction temperature of 280 ℃, and discharging after reaching the preset power after the vacuum degree of 25Pa and 3.5 hours, wherein the intrinsic viscosity of the tested product is 0.668dl/g.
The preparation method of the silicon dioxide solution with the solid content of 10 percent comprises the following steps: 50Kg of amino-coated modified silica slurry with 50% of solid content (amino-coated modified silica product provided by Taiwan Changxing chemical industry Co., ltd.) is taken and added into a dispersion tank, 200Kg of ethylene glycol is then counted, the dispersion tank and a colloid mill device are started after the addition of the ethylene glycol is finished, and the slurry is subjected to high-speed dispersion for 2-2.5 hours until stable and uniform slurry is formed for production and use.
Other examples 2-4 were carried out according to the methods of steps (1) to (4), and specific data are shown in Table 1:
table 1:
| parameter item | Example 1 | Example 2 | Example 3 | Example 4 |
| Terephthalic acid/Kg | 1750 | 1650 | 1900 | 1700 |
| Isophthalic acid/Kg | 250 | 350 | 100 | 300 |
| Ethylene glycol/Kg | 800 | 700 | 900 | 750 |
| Diethylene glycol/Kg | 55 | 80 | 30 | 65 |
| 1, 3-propanediol/Kg | 35 | 60 | 12 | 40 |
| 1, 4-cyclohexanedimethanol | 160 | 220 | 80 | 180 |
The polyester chip for producing the single-sided heat-sealing film has similar heat-sealing temperature and more excellent heat-sealing firmness under the same heat-sealing condition compared with the conventional polyester chip for producing the single-sided heat-sealing film, and meanwhile, the defects of powder falling and difficult recovery of the heat-sealing film are overcome.
The following description is made in connection with specific embodiments:
the polyester chips for producing the single-sided heat-seal film in the above examples 1 to 4 were processed into 25 μm films by passing the polyester chips for single-sided heat-seal film through an ABC three-layer co-extrusion BOPET film line according to a single-sided addition of 12%, and the test results were summarized in the following table 2 by comparing the test indexes of each example at 120 ℃ for 110n,1s of heat-seal time:
table 2:
the above-described embodiments are only for illustrating the technical spirit and features of the present invention, and it is intended to enable those skilled in the art to understand the content of the present invention and to implement it accordingly, and the scope of the present invention is not limited to the embodiments, i.e. equivalent changes or modifications to the spirit of the present invention are still within the scope of the present invention.
Claims (7)
1. A method for producing a polyester chip for producing a single-sided heat-seal film, comprising the steps of:
(1) adding a certain amount of ethylene glycol and a small amount of 1, 3-propylene glycol into a pulping kettle, then adding a certain amount of terephthalic acid solid powder, preparing into viscous slurry, and pumping into an esterification reaction kettle through a slurry supply pump to start a first part of esterification reaction; wherein terephthalic acid accounts for 80-95% of the total acid mole ratio of the esterification reaction, ethylene glycol accounts for 80-93% of the total alcohol mole ratio of the esterification reaction, and 1, 3-propylene glycol accounts for 1-5% of the total alcohol mole ratio of the esterification reaction;
(2) adding a certain amount of diethylene glycol and 1, 4-cyclohexanedimethanol solution into a feed port of a di-esterification reaction kettle, starting the di-esterification kettle to stir, adding a certain amount of isophthalic acid, capping the feed port, starting the temperature rise, and performing a second part of esterification reaction; wherein, the mole ratio of the intermediate phthalic acid to the total acid of the esterification reaction is 5-15%, the mole ratio of the diglycol to the total alcohol of the esterification reaction is 2-5%, and the mole ratio of the 1, 4-cyclohexanedimethanol to the total alcohol of the esterification reaction is 4-10%;
(3) after the raw materials added in (1) and (2) are reacted, introducing the esterified substance generated by the reaction in (1) into a di-esterification reaction kettle through a pipeline, mixing with the second part of esterified product in (2), starting the di-esterification kettle for stirring, heating to 230-250 ℃, uniformly adding the prepared silicon dioxide solution, and adding a proper amount of catalyst and stabilizer through an auxiliary agent port after the silicon dioxide solution is completely filled; the molar ratio of total acid to total alcohol of the two esterification reactions is 1: (1.15-1.35);
(4) after the reaction of the step (3) is finished and the temperature of the slurry is stabilized to 230-250 ℃, pressing the materials in the di-esterification reaction kettle into a polycondensation reaction kettle from high-purity nitrogen through a stainless steel filter with the diameter of 15-25 mu m;
(4) after the mixed slurry enters a polycondensation kettle, the temperature of the material is raised to 245-255 ℃, and the temperature is raised and the low vacuum is pumped; and (3) controlling the reaction temperature to 275-285 ℃ for negative pressure polymerization reaction, controlling stirring polycondensation current and power through equipment under the condition that the vacuum degree is less than or equal to 30Pa and the final temperature to 275-285 ℃, synthesizing a high-viscosity polyester slice melt with the intrinsic viscosity of 0.660-0.680dl/g, and finally obtaining the polyester slice for producing the single-sided heat-sealing film through a belt casting head, an underwater granulator, a dryer and a vibrating screen.
2. The method for producing a polyester chip for producing a single-sided heat-seal film according to claim 1, wherein the molar ratio of the first partial esterification to the second partial esterification alkyd is required to be greater than 1, ensuring that the acid esterification is complete.
3. The method for producing a polyester chip for producing a single-sided heat-seal film according to claim 1, wherein the first partial esterification reaction requires a reaction temperature of 245 to 265 ℃ and the second partial esterification reaction requires a temperature of 190 to 220 ℃.
4. The method for producing a polyester chip for producing a single-sided heat-seal film according to claim 1, wherein the catalyst is ethylene glycol antimony in an amount of 400 to 600ppm based on the theoretical polyester chip yield; the stabilizer is trimethyl phosphate, and the addition amount is 50-100ppm of the theoretical polyester chip yield.
5. The method for producing a polyester chip for a single-sided heat-sealing film according to claim 1, wherein the silica solution is a uniform slurry prepared by dispersing a certain amount of silica solids in a certain amount of glycol solution in a mass concentration of 5 to 15%, and the amount of the added silica solids is 0.03 to 0.15% of the theoretical yield of the polyester chip.
6. The method for producing a polyester chip for producing a single-sided heat-sealing film according to claim 5, wherein the silica slurry is formulated such that the silica solids used require a median particle diameter of 1.0 μm and a normal distribution range of the particle diameter of not more than 0.2 μm, i.e., a particle diameter range of 0.8 to 2.2 μm, are highly concentrated, and the silica solids used are subjected to an amino coating treatment.
7. A polyester chip for producing a single-sided heat-seal film produced by the production method according to any one of claims 1 to 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311045123.2A CN117050284A (en) | 2023-08-18 | 2023-08-18 | Polyester chip for producing single-sided heat-sealing film and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311045123.2A CN117050284A (en) | 2023-08-18 | 2023-08-18 | Polyester chip for producing single-sided heat-sealing film and preparation method thereof |
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| CN117050284A true CN117050284A (en) | 2023-11-14 |
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| CN202311045123.2A Pending CN117050284A (en) | 2023-08-18 | 2023-08-18 | Polyester chip for producing single-sided heat-sealing film and preparation method thereof |
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| Country | Link |
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| CN (1) | CN117050284A (en) |
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- 2023-08-18 CN CN202311045123.2A patent/CN117050284A/en active Pending
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