CN104448726A - Method for producing toughened polyester film for coated iron - Google Patents
Method for producing toughened polyester film for coated iron Download PDFInfo
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- CN104448726A CN104448726A CN201410627394.3A CN201410627394A CN104448726A CN 104448726 A CN104448726 A CN 104448726A CN 201410627394 A CN201410627394 A CN 201410627394A CN 104448726 A CN104448726 A CN 104448726A
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- toughness reinforcing
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Abstract
The invention discloses a method for producing a toughened polyester film for coated iron. The method comprises the following steps: proportionally measuring terephthalic acid, glycol, a toughened monomer and a catalyst, sequentially adding in a reaction kettle according to the sequence of firstly liquid and then solid, and performing pulp beating for 10-20 minutes; then heating to perform esterification reaction, finishing the esterification reaction when the water output is equal to or larger than 90%, further heating to perform vacuum polycondensation reaction; mixing for vacuum polycondensation reaction after ionic comonomer containing active groups, a stabilizing agent and an anti-block agent are added in esterified prepolymer, then performing water cooling granulating to obtain toughened polyester for coated iron; drawing to obtain the toughened polyester film for coated iron; and compounding the polyester film obtained with a tin plate to obtain a composite material. Through the manner, the adhesion performance of the surface of the polyester film to the surface of the metal plate is improved, the flexibility of the film is controlled by adjusting the content of the toughened monomer; and the film can be attached to the surface of the tin plate without adhesives.
Description
Technical field
The present invention relates to field of compound material, particularly relate to the production method that a kind of film-covered iron polyester film is toughness reinforcing.
Background technology
Metal sheet film coating technique is plastic film and metal sheet by high temperature hot pressing, film is pasted processing technology on a metal plate.Film coating technique was born in Japan in 1977, at first for tank processed, can replace interior painting, outer painting technology, develop into the multiple fields such as building materials internal and external ornament finishing, household electrical appliances, automobile till now.The features such as biaxially oriented polyester film physical strength is high, good in optical property, use temperature are wide, barrier is excellent, oil resistant, corrosion-resistant, cost is low, and be applied in widely in film-covered iron matrix material.
The detailed physicals of biaxially oriented polyester film is in table 1.
Table 1: the performance of biaxial stretching polyester film
But biaxially oriented polyester film is because the strict molecular chain structure of itself, be difficult to when non-processor directly bonding with tinplate.Prior art has the Third monomer containing active group by interpolation to improve the surface energy of polyester material for bonding, but due to adding of the 3rd reactive monomer, the kindliness of polyester material, mechanical property has and declines significantly, is difficult to realize through engineering approaches application.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of kindliness that can improve polyester film, with the production method that the film-covered iron polyester film rushing shape and deep processing application being suitable for the film-covered iron material later stage is toughness reinforcing.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide the production method that a kind of film-covered iron polyester film is toughness reinforcing, comprise the following steps:
1), after terephthalic acid, ethylene glycol, toughness reinforcing monomer and catalyzer proportionally being weighed, homophase mixes; Add successively in reactor according to the order of solid after first liquid, making beating 10-20 minute; Then heat and carry out esterification, when aquifer yield is more than or equal to 90%, completes esterification and continue again to heat, carry out vacuum polycondensation;
2) ionic comonomer containing active group, stablizer and opening agent are added in the performed polymer after esterification carry out mixing vacuum polycondensation, then obtain the toughness reinforcing polyester of film-covered iron through water-cooled pelletizing;
3) obtained polyester drawn is obtained film-covered iron toughened polymer ester film;
4) polyester film of gained and tinplate compound are obtained matrix material.
In a preferred embodiment of the present invention, in step 1), toughness reinforcing monomer is the polycondensate containing the long chain diol or straight dihydric alcohol being more than or equal to 3 carbon atoms.
In a preferred embodiment of the present invention, the ratio in step 1) between each reactant is acid, alcohol mole total amount compares between 1 ~ 2, and wherein, toughness reinforcing monomer content is less than or equal to 40% of alcohol total mass.
In a preferred embodiment of the present invention, in step 1), esterification reaction temperature is between 230 ~ 270 DEG C.
In a preferred embodiment of the present invention, in step 1), catalyzer is antimony-based catalyst, germanium series catalysts or Titanium series catalyst, this catalyst content be reactant total mass ten thousand/to 6/10000ths.
In a preferred embodiment of the present invention, step 2) in, ionic comonomer is that described ionic comonomer content is that one of percentage of sour molar content is to 5 percent containing sulfonic sodium salt ester or containing the one in sulfonic sylvite ester or two kinds of mixtures.
In a preferred embodiment of the present invention, step 2) in, stablizer is PET polyester synthesis stablizer phosphoric acid ester, content be reactant total mass ten thousand/.
In a preferred embodiment of the present invention, step 2) in, described opening agent is one or several in particle diameter 2 μm ~ 6 μm barium sulfate, calcium carbonate or silicon-dioxide, and the content of opening agent is 7/30000 to ten thousand/10000ths of total mass.
In a preferred embodiment of the present invention, described condensation temperature is 250 ~ 280 DEG C, and described polycondensation reaction time is 2 ~ 4 hours.
In a preferred embodiment of the present invention, the complex method of polyester film and tinplate is hot pressing complex method.
The invention has the beneficial effects as follows: the present invention is in polyester synthesis by adding the monomer containing active group, to improve the adhesiveproperties of polyester film surface and metal sheet surface, add toughness reinforcing monomer, by the snappiness regulating the content of toughness reinforcing monomer to control film simultaneously; Just well can fit with tinplate surface without the need to sizing agent.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
The embodiment of the present invention comprises:
The production method that film-covered iron polyester film is toughness reinforcing, it comprises the following steps:
1), after terephthalic acid, ethylene glycol, toughness reinforcing monomer and catalyzer being weighed according to a certain percentage, liquid and liquid, add in reactor successively according to the order of solid after first liquid after solid mixes with solid-phase, wherein toughness reinforcing monomer is that carbon atom is more than or equal to the straight dihydric alcohol of three atoms, the polycondensate of straight dihydric alcohol, as 1,3-PD, BDO, 1,6-hexylene glycol, heptanediol, certain herbaceous plants with big flowers glycol, Diethylene Glycol, one contracting propylene glycol, the polyoxyethylene glycol of different molecular weight.Multiple-CH2-from molecular structure in the middle of long chain diol can increase intermolecular kindliness, wherein alkyd mole total amount than 1 ~ 2 between; Toughness reinforcing monomer content more high tenacity is larger, but content is no more than 40% of alcohol total amount; Catalyzer is antimony-based catalyst, germanium series catalysts, Titanium series catalyst such as, catalyst content be reactant total mass ten thousand/to 6/10000ths.
After reactant adds, making beating 10 ~ 20 minutes in still, 150Kp in inflated with nitrogen to still for the first time, aeration speed is 4Kp/min, then slowly gas is released, venting speed is 4Kp/min, with air in nitrogen replacement still, when pressure in still is normal pressure, continue with identical speed to inflated with nitrogen in still, be charged to pressure 120Kp in still, carry out nitrogen protection, then carry out intensification and be raised to 200 DEG C for the first time, keep 15min, now reach the boiling point of alcohol, object is in order to alcohol and acid fully contact at interface under stress, so that solid acid and liquid alcohol carry out surface reaction.
Then be warmed up between 230 ~ 270 DEG C and carry out esterification, period observes the pressure change in still at any time, the pressure in still is kept to be no more than 320Kp, water outlet is started when reacting condensing tower temperature more than 138 DEG C, reaction is when aquifer yield reaches more than 90%, go out water speed obviously to decline, now complete esterification.
2) ionic comonomer containing active group, stablizer, opening agent are added in the performed polymer after esterification mix vacuum polycondensation, ionic comonomer is containing sulfonic sodium salt ester or containing the one in sulfonic sylvite ester or two kinds of mixtures, content is 1% ~ 5% of the molar content of acid, stablizer is phosphoric acid ester, content be reactant total mass ten thousand/.Opening agent is one or several in particle diameter 2 μm ~ 6 μm barium sulfate, calcium carbonate and silicon-dioxide.The content of opening agent is 7/30000 to ten thousand/10000ths of total mass.Stir fully mixing in 20 minutes after material adds, vacuumize gradually, temperature facility is 250 ~ 280 DEG C, vacuum polycondensation 2-4 hour.Stop stirring, to reaction system inflated with nitrogen, material is discharged to tank, obtain the toughness reinforcing polyester of film-covered iron through water-cooled pelletizing.
3) obtained polyester is obtained film-covered iron toughened polymer ester film through stretch processes.
4) polyester film of gained and the hot compound of tinplate are obtained the good matrix material of hot plyability.
Embodiment 1: the production method that a kind of film-covered iron polyester film is toughness reinforcing, it comprises the following steps:
1) terephthalic acid, ethylene glycol, 1, 4-butyleneglycol compares 1:1.4 according to acid alcohol amount, catalyst oxidation antimony content is 2/10000ths of total mass, liquid and liquid, add successively in reactor according to the order of solid after first liquid after solid mixes with solid-phase, after reactant adds, making beating 10 minutes in still, 150Kp in inflated with nitrogen to still for the first time, aeration speed is 4Kp/min, then slowly gas is released, venting speed is 4Kp/min, with air in nitrogen replacement still, when pressure in still is normal pressure, continue with identical speed to inflated with nitrogen in still, be charged to pressure 120Kp in still, carry out nitrogen protection, then carry out intensification and be raised to 200 DEG C for the first time, keep 15min, then be warmed up between 250 DEG C and carry out esterification, period observes the pressure change in still at any time, the pressure in still is kept to be no more than 320Kp, water outlet is started when reacting condensing tower temperature more than 138 DEG C, reaction is when aquifer yield reaches more than 90%, go out water speed obviously to decline, now complete esterification.
2) by two for 5-sodium sulfo isophthalate hydroxyl ethyl ester, addition is the molar content 3% of acid, triphenyl addition be reactant total mass ten thousand/, the silicon-dioxide of particle diameter 3 microns, addition is 3/10000ths of total mass, adds in the performed polymer after esterification and mixes vacuum polycondensation, stirs fully mixing in 20 minutes after material adds, vacuumize gradually, the speed vacuumized is 2Kp/min, and temperature facility is 260 DEG C, vacuum polycondensation 3 hours.Stop stirring, to reaction system inflated with nitrogen, material is discharged to tank, obtain the toughness reinforcing polyester of film-covered iron through water-cooled pelletizing.
3) obtained polyester is obtained film-covered iron toughened polymer ester film through stretch processes.
4) polyester film of gained and the hot compound of tinplate are obtained the good matrix material of hot plyability.
The quantitative measurement result of the film obtained by the method for embodiment 1 is as shown in the table:
Through the film iron composite material of hot compound according to ASTM B 533-85 standard testing stripping performance, film is peeled off not get off, last body fracture.
Embodiment 2: the production method that a kind of film-covered iron polyester film is toughness reinforcing, it comprises the following steps:
1) terephthalic acid, ethylene glycol, poly(oxyethylene glycol) 400 compares 1:1.4 according to acid alcohol amount, catalyst oxidation antimony content is 2/10000ths of total mass, liquid and liquid, add successively in reactor according to the order of solid after first liquid after solid mixes with solid-phase, after reactant adds, making beating 15 minutes in still, 150Kp in inflated with nitrogen to still for the first time, aeration speed is 4Kp/min, then slowly gas is released, venting speed is 4Kp/min, with air in nitrogen replacement still, when pressure in still is normal pressure, continue with identical speed to inflated with nitrogen in still, be charged to pressure 120Kp in still, carry out nitrogen protection, then carry out intensification and be raised to 200 DEG C for the first time, keep 15min, then be warmed up between 260 DEG C and carry out esterification, period observes the pressure change in still at any time, the pressure in still is kept to be no more than 320Kp, water outlet is started when reacting condensing tower temperature more than 138 DEG C, reaction is when aquifer yield reaches more than 90%, go out water speed obviously to decline, now complete esterification.
2) by two for m-phthalic acid-5-potassium sulfonate hydroxyl ethyl ester, addition is the molar content 3% of acid, triphenyl addition be reactant total mass ten thousand/, the silicon-dioxide of particle diameter 5 microns, addition is 3/10000ths of total mass, adds in the performed polymer after esterification and mixes vacuum polycondensation, stirs fully mixing in 20 minutes after material adds, vacuumize gradually, the speed vacuumized is 2Kp/min, and temperature facility is 270 DEG C, vacuum polycondensation 3 hours.Stop stirring, to reaction system inflated with nitrogen, material is discharged to tank, obtain the toughness reinforcing polyester of film-covered iron through water-cooled pelletizing.
3) obtained polyester is obtained film-covered iron toughened polymer ester film through stretch processes.
4) polyester film of gained and the hot compound of tinplate are obtained the good matrix material of hot plyability.
The quantitative measurement result of the film obtained by the method for embodiment 2 is as shown in the table:
Wherein, through the film iron composite material of hot compound according to ASTM B 533-85 standard testing stripping performance, film is peeled off not get off, last body fracture.
Embodiment 3: the production method that a kind of film-covered iron polyester film is toughness reinforcing, it comprises the following steps:
1) terephthalic acid, ethylene glycol, 1.6-heptanediol, 1:1.5 is compared according to acid alcohol amount, catalyst oxidation titanium content is 2/10000ths of total mass, liquid and liquid, add successively in reactor according to the order of solid after first liquid after solid mixes with solid-phase, after reactant adds, making beating 20 minutes in still, 150Kp in inflated with nitrogen to still for the first time, aeration speed is 4Kp/min, then slowly gas is released, venting speed is 4Kp/min, with air in nitrogen replacement still, when pressure in still is normal pressure, continue with identical speed to inflated with nitrogen in still, be charged to pressure 120Kp in still, carry out nitrogen protection, then carry out intensification and be raised to 200 DEG C for the first time, keep 15min, then be warmed up between 240 DEG C and carry out esterification, period observes the pressure change in still at any time, the pressure in still is kept to be no more than 320Kp, water outlet is started when reacting condensing tower temperature more than 130 DEG C, reaction is when aquifer yield reaches more than 90%, go out water speed obviously to decline, now complete esterification.
2) by two for terephthalic acid-5-sodium sulfonate hydroxyl ethyl ester, addition is the molar content 4% of acid, trimethyl phosphate addition be reactant total mass ten thousand/, the calcium carbonate of particle diameter 3 microns, addition is 3/10000ths of total mass, adds in the performed polymer after esterification and mixes vacuum polycondensation, stirs fully mixing in 20 minutes after material adds, vacuumize gradually, the speed vacuumized is 2Kp/min, and temperature facility is 265 DEG C, vacuum polycondensation 3 hours.Stop stirring, to reaction system inflated with nitrogen, material is discharged to tank, obtain the toughness reinforcing polyester of film-covered iron through water-cooled pelletizing.
3) obtained polyester is obtained film-covered iron toughened polymer ester film through stretch processes.
4) polyester film of gained and the hot compound of tinplate are obtained the good matrix material of hot plyability.
The quantitative measurement result of the film obtained by the method for embodiment 3 is as shown in the table:
Wherein, through the film iron composite material of hot compound according to ASTM B 533-85 standard testing stripping performance, film is peeled off not get off, last body fracture.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. the production method that film-covered iron polyester film is toughness reinforcing, is characterized in that, comprises the following steps:
1), after terephthalic acid, ethylene glycol, toughness reinforcing monomer and catalyzer proportionally being weighed, homophase mixes; Add successively in reactor according to the order of solid after first liquid, making beating 10-20 minute; Then heat and carry out esterification, when aquifer yield is more than or equal to 90%, completes esterification and continue again to heat, carry out vacuum polycondensation;
2) ionic comonomer containing active group, stablizer and opening agent are added in the performed polymer after esterification carry out mixing vacuum polycondensation, then obtain the toughness reinforcing polyester of film-covered iron through water-cooled pelletizing;
3) obtained polyester drawn is obtained film-covered iron toughened polymer ester film;
4) polyester film of gained and tinplate compound are obtained matrix material.
2. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, is characterized in that, in step 1), toughness reinforcing monomer is the polycondensate containing the long chain diol or straight dihydric alcohol being more than or equal to 3 carbon atoms.
3. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, is characterized in that, the ratio in step 1) between each reactant is alcohol, acid mole total amount compares between 1 ~ 2, and wherein, toughness reinforcing monomer content is less than or equal to 40% of alcohol total mass.
4. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, is characterized in that, in step 1), esterification reaction temperature is between 230 ~ 270 DEG C.
5. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, it is characterized in that, in step 1), catalyzer is antimony-based catalyst, germanium series catalysts or Titanium series catalyst, this catalyst content be reactant total mass ten thousand/to 6/10000ths.
6. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, it is characterized in that, step 2) in, ionic comonomer is that described ionic comonomer content is that one of percentage of sour molar content is to 5 percent containing sulfonic sodium salt ester or containing the one in sulfonic sylvite ester or two kinds of mixtures.
7. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, is characterized in that, step 2) in, stablizer is PET polyester synthesis stablizer phosphoric acid ester, content be reactant total mass ten thousand/.
8. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, it is characterized in that, step 2) in, described opening agent is one or several in particle diameter 2 μm ~ 6 μm barium sulfate, calcium carbonate or silicon-dioxide, and the content of opening agent is 7/30000 to ten thousand/10000ths of total mass.
9. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, is characterized in that, described condensation temperature is 250 ~ 280 DEG C, and described polycondensation reaction time is 2 ~ 4 hours.
10. the production method that film-covered iron polyester film according to claim 1 is toughness reinforcing, is characterized in that, the complex method of polyester film and tinplate is hot pressing complex method.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109910402A (en) * | 2017-12-13 | 2019-06-21 | 宝山钢铁股份有限公司 | A kind of film-covered iron that interfacial bubbles rate is extremely low and its manufacturing method |
| CN112111052A (en) * | 2019-06-20 | 2020-12-22 | 中国石油化工股份有限公司 | Raw material formula of PET flat filament and preparation method thereof |
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| CN101544750A (en) * | 2009-04-22 | 2009-09-30 | 无锡国能新材料科技有限公司 | Method for preparing polyethylene glycol terephthalate by adopting anchoring agent |
| CN103753932A (en) * | 2013-12-27 | 2014-04-30 | 天津万华股份有限公司 | Directly-compoundable low-melting-point polyester thin film preparation method for laminated steel |
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2014
- 2014-11-10 CN CN201410627394.3A patent/CN104448726B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544750A (en) * | 2009-04-22 | 2009-09-30 | 无锡国能新材料科技有限公司 | Method for preparing polyethylene glycol terephthalate by adopting anchoring agent |
| CN103753932A (en) * | 2013-12-27 | 2014-04-30 | 天津万华股份有限公司 | Directly-compoundable low-melting-point polyester thin film preparation method for laminated steel |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109910402A (en) * | 2017-12-13 | 2019-06-21 | 宝山钢铁股份有限公司 | A kind of film-covered iron that interfacial bubbles rate is extremely low and its manufacturing method |
| CN112111052A (en) * | 2019-06-20 | 2020-12-22 | 中国石油化工股份有限公司 | Raw material formula of PET flat filament and preparation method thereof |
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Effective date of registration: 20211216 Address after: 611730 No. 249 binqing Road, south area of Chengdu modern industrial port, Pidu District, Chengdu, Sichuan Patentee after: Chengdu Fuquan New Material Co.,Ltd. Address before: 214000 63 East Ring Road, Yuqi street, Huishan District, Wuxi, Jiangsu Patentee before: HARBIN INSTITUTE OF TECHNOLOGY WUXI Research Institute OF NEW MATERIALS Patentee before: Wuxi Haite New Material Research Institute Co., Ltd |