CN104356614A - Preparation method of PET polyester based on emulsion polymerization process - Google Patents
Preparation method of PET polyester based on emulsion polymerization process Download PDFInfo
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- CN104356614A CN104356614A CN201410644528.2A CN201410644528A CN104356614A CN 104356614 A CN104356614 A CN 104356614A CN 201410644528 A CN201410644528 A CN 201410644528A CN 104356614 A CN104356614 A CN 104356614A
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Abstract
The invention relates to a preparation method of PET polyester based on an emulsion polymerization process, belonging to the technical field of high polymer materials. The preparation method comprises the following steps: adding water and an emulsifier into a reactor, uniformly stirring, then, adding acrylic acid, hydroxyethyl acrylate and methyl methacrylate, uniformly stirring, then, adding an initiator, heating to perform polymerization reaction, adding ferric oxide, glass fiber and silicon oxide powder, uniformly stirring, carrying out suction filtration to obtain a polymer, washing a filter cake by using alcohol, and drying the filter cake to obtain a prepolymer; uniformly mixing the prepolymer, polyethylene glycol terephthalate, butanediol diacrylate, a nucleating agent, an antioxidant, a silane coupling agent and a lubricant to obtain a mixture; and feeding the mixture into a twin-screw extruder, and extruding and pelletizing. According to the polyester material provided by the invention, the glass fiber is prepared into the prepolymer by virtue of an emulsion coating manner, and the prepolymer and the polyester are extruded to obtain the polymer material, so that the glass transition temperature of the polyester is lowered and the mechanical strength of the polyester is improved.
Description
Technical field
The present invention relates to a kind of preparation method of the PET polyester based on emulsion polymerization, belong to technical field of polymer materials.
Background technology
Polyester is the abbreviation of poly terephthalic acid and second diester, is commonly called as terylene, and being called for short PET, is high polymers, by ethylene glycol terephthalate generation dehydration condensation.Ethylene glycol terephthalate is by terephthalic acid and ethylene glycol generation esterification gained.PET is oyster white or polymkeric substance that is light yellow, highly crystalline, and surface smoothing is glossy.In wide temperature range, have excellent physical and mechanical properties, life-time service temperature can reach 120 DEG C, and electrical insulating property is excellent, even under high-temperature high-frequency, its electrical property is still better, but corona resistance is poor, creep resistance, resistance to fatigue, rub resistance, dimensional stability are all fine.
Its advantage shows: 1. have good mechanical property, and shock strength is 3 ~ 5 times of other films, and folding resistance is good.2. oil resistant, resistance to fat, resistance to diluted acid, diluted alkaline, resistance to most of solvent.3. there is excellent high-and low-temperature resistance performance, can in 120 DEG C of temperature ranges life-time service, short-period used can resistance to 150 DEG C of high temperature, can resistance to-70 DEG C of low temperature, and very little to its mechanical impact during high and low temperature.4. gas and vapor permeability low, namely have excellent choke, water, oil and peculiar smell performance.5. transparency is high, can shielding of ultraviolet, and glossiness is good.6. nontoxic, tasteless, wholesomeness is good, can be directly used in food product pack.
But PET polyester also exists the not high problem of physical strength, and the second-order transition temperature of PET product compared with high, crystallization velocity is slow, molding cycle is long, molding shrinkage is large, poor dimensional stability, crystallization shaping in fragility, thermotolerance low etc. shortcoming.
Summary of the invention
The object of the invention is: solve the problem that second-order transition temperature is higher, physical strength is bad that PET polyester exists.A kind of preparation method of the PET polyester based on emulsion polymerization is proposed.
Based on a preparation method for the PET polyester of emulsion polymerization, comprise the steps:
1st step, emulsion polymerizing preparation compound: by weight, add 90 ~ 110 parts, water, emulsifying agent 2 ~ 4 parts in the reactor, stir, add 4 ~ 6 parts, vinylformic acid, Hydroxyethyl acrylate 4 ~ 7 parts, methyl methacrylate 5 ~ 9 parts again, after stirring, add initiator 0.2 ~ 0.4 part again, polyreaction is carried out in heating, add Indian red 1 ~ 2 part again, 10 ~ 20 parts, glass fibre, silica powder 4 ~ 8 parts stir, polymkeric substance is obtained after suction filtration, use washing with alcohol filter cake again, after being dried by filter cake, obtain performed polymer;
2nd step, by performed polymer, polyethylene terephthalate 40 ~ 60 parts, butyleneglycol double methacrylate 3 ~ 5 parts, 0.5 ~ 1 part, oxidation inhibitor, silane coupling agent 0.5 ~ 1 part, lubricant 0.5 ~ 1 part, mix, obtain mixture;
3rd step, mixture is sent into extruding pelletization in twin screw extruder.
In the 1st described step, the temperature of polyreaction is 70 ~ 80 DEG C, and polymerization reaction time is 1 ~ 2 hour.
Described initiator is selected from hydrogen peroxide, Potassium Persulphate, isopropyl benzene hydroperoxide, diisopropylbenzenehydroperoxide, p-propyl-toluene hydrogen peroxide.
Described emulsifying agent is selected from Sodium dodecylbenzene sulfonate, hydroxy alkyl sulfonic acid sodium, diisooctyl succinate sodium sulfonate, polyacrylamide.
Described silane coupling agent is the one in KH-550, KH-560, KH-570.
Described oxidation inhibitor is antioxidant 1010 or irgasfos 168.
The length of described glass fibre is 10 ~ 500 microns.
Twin screw extruder extrusion temperature one district temperature 190 ~ 200 DEG C, two district's temperature 200 ~ 210 DEG C, three district's temperature 220 ~ 230 DEG C, four district's temperature 210 ~ 230 DEG C, five district's temperature 230 ~ 240 DEG C, screw speed is 180 ~ 220 rpm.
beneficial effect
Polyester material provided by the invention, by glass fibre is made performed polymer by the mode that emulsion is coated, then is extruded by performed polymer and polyester, reduces the second-order transition temperature of polyester, improve physical strength.
Embodiment
embodiment 1
Based on the preparation method of the PET polyester of emulsion polymerization, comprise the steps:
1st step, emulsion polymerizing preparation compound: add water 90Kg in the reactor, emulsifying agent 2Kg, stir, add vinylformic acid 4Kg again, Hydroxyethyl acrylate 4Kg, methyl methacrylate 5Kg, after stirring, add initiator 0.2Kg again, polyreaction is carried out in heating, add Indian red 1Kg again, glass fibre 10Kg, silica powder 4Kg stirs, polymkeric substance is obtained after suction filtration, use washing with alcohol filter cake again, after filter cake is dried, obtain performed polymer, the temperature of polyreaction is 70 DEG C, polymerization reaction time is 1 hour, initiator is Potassium Persulphate, emulsifying agent is Sodium dodecylbenzene sulfonate, the length of described glass fibre is 10 ~ 500 microns,
2nd step, by performed polymer, polyethylene terephthalate 40Kg, butyleneglycol double methacrylate 3Kg, oxidation inhibitor 0.5Kg, Silane coupling reagent KH-570 0.5Kg, lubricant 0.5Kg, mix, obtain mixture; Described oxidation inhibitor is antioxidant 1010;
3rd step, mixture is sent into extruding pelletization in twin screw extruder,, twin screw extruder extrusion temperature one district temperature 190 DEG C, two district's temperature 200 DEG C, three district's temperature 220 DEG C, four district's temperature 210 DEG C, five district's temperature 230 DEG C, screw speed is 180 rpm.
embodiment 2
Based on the preparation method of the PET polyester of emulsion polymerization, comprise the steps:
1st step, emulsion polymerizing preparation compound: add water 110Kg in the reactor, emulsifying agent 4Kg, stir, add vinylformic acid 6Kg again, Hydroxyethyl acrylate 7Kg, methyl methacrylate 9Kg, after stirring, add initiator 0.4Kg again, polyreaction is carried out in heating, add Indian red 2Kg again, glass fibre 20Kg, silica powder 8Kg stirs, polymkeric substance is obtained after suction filtration, use washing with alcohol filter cake again, after filter cake is dried, obtain performed polymer, the temperature of polyreaction is 80 DEG C, polymerization reaction time is 2 hours, initiator is Potassium Persulphate, emulsifying agent is Sodium dodecylbenzene sulfonate, the length of described glass fibre is 10 ~ 500 microns,
2nd step, by performed polymer, polyethylene terephthalate 60Kg, butyleneglycol double methacrylate 5Kg, oxidation inhibitor 1Kg, Silane coupling reagent KH-570 1Kg, lubricant 1Kg, mix, obtain mixture; Described oxidation inhibitor is antioxidant 1010;
3rd step, mixture is sent into extruding pelletization in twin screw extruder,, twin screw extruder extrusion temperature one district temperature 190 DEG C, two district's temperature 200 DEG C, three district's temperature 220 DEG C, four district's temperature 210 DEG C, five district's temperature 230 DEG C, screw speed is 180 rpm.
embodiment 3
Based on the preparation method of the PET polyester of emulsion polymerization, comprise the steps:
1st step, emulsion polymerizing preparation compound: add water 100Kg in the reactor, emulsifying agent 3Kg, stir, add vinylformic acid 5Kg again, Hydroxyethyl acrylate 6Kg, methyl methacrylate 8Kg, after stirring, add initiator 0.3Kg again, polyreaction is carried out in heating, add Indian red 2Kg again, glass fibre 15Kg, silica powder 6Kg stirs, polymkeric substance is obtained after suction filtration, use washing with alcohol filter cake again, after filter cake is dried, obtain performed polymer, the temperature of polyreaction is 75 DEG C, polymerization reaction time is 2 hours, initiator is Potassium Persulphate, emulsifying agent is Sodium dodecylbenzene sulfonate, the length of described glass fibre is 10 ~ 500 microns,
2nd step, by performed polymer, polyethylene terephthalate 50Kg, butyleneglycol double methacrylate 4Kg, oxidation inhibitor 0.6Kg, Silane coupling reagent KH-570 0.8Kg, lubricant 0.6Kg, mix, obtain mixture; Described oxidation inhibitor is antioxidant 1010;
3rd step, mixture is sent into extruding pelletization in twin screw extruder,, twin screw extruder extrusion temperature one district temperature 195 DEG C, two district's temperature 205 DEG C, three district's temperature 225 DEG C, four district's temperature 220 DEG C, five district's temperature 235 DEG C, screw speed is 200 rpm.
reference examples 1
Be with the difference of embodiment 3: the preparation not carrying out performed polymer, glass fibre adds in the 2nd step.
Based on the preparation method of the PET polyester of emulsion polymerization, comprise the steps:
1st step, by polyethylene terephthalate 50Kg, butyleneglycol double methacrylate 4Kg, oxidation inhibitor 0.6Kg, Silane coupling reagent KH-570 0.8Kg, lubricant 0.6Kg, glass fibre 15Kg, mix, obtain mixture; Described oxidation inhibitor is antioxidant 1010, and the length of described glass fibre is 10 ~ 500 microns;
2nd step, mixture is sent into extruding pelletization in twin screw extruder,, twin screw extruder extrusion temperature one district temperature 195 DEG C, two district's temperature 205 DEG C, three district's temperature 225 DEG C, four district's temperature 220 DEG C, five district's temperature 235 DEG C, screw speed is 200 rpm.
reference examples 2
Be with the difference of embodiment 3: glass fibre adds in the 2nd step.
Based on the preparation method of the PET polyester of emulsion polymerization, comprise the steps:
1st step, emulsion polymerizing preparation compound: add water 100Kg in the reactor, emulsifying agent 3Kg, stir, add vinylformic acid 5Kg again, Hydroxyethyl acrylate 6Kg, methyl methacrylate 8Kg, after stirring, add initiator 0.3Kg again, polyreaction is carried out in heating, add Indian red 2Kg again, silica powder 6Kg stirs, polymkeric substance is obtained after suction filtration, use washing with alcohol filter cake again, after filter cake is dried, obtain performed polymer, the temperature of polyreaction is 75 DEG C, polymerization reaction time is 2 hours, initiator is Potassium Persulphate, emulsifying agent is Sodium dodecylbenzene sulfonate,
2nd step, by performed polymer, polyethylene terephthalate 50Kg, butyleneglycol double methacrylate 4Kg, oxidation inhibitor 0.6Kg, Silane coupling reagent KH-570 0.8Kg, lubricant 0.6Kg, glass fibre 15Kg, mix, obtain mixture; Described oxidation inhibitor is antioxidant 1010, and the length of described glass fibre is 10 ~ 500 microns;
3rd step, mixture is sent into extruding pelletization in twin screw extruder,, twin screw extruder extrusion temperature one district temperature 195 DEG C, two district's temperature 205 DEG C, three district's temperature 225 DEG C, four district's temperature 220 DEG C, five district's temperature 235 DEG C, screw speed is 200 rpm.
reference examples 3
Be with the difference of embodiment 3: in the 1st step, do not add Hydroxyethyl acrylate.
Based on the preparation method of the PET polyester of emulsion polymerization, comprise the steps:
1st step, emulsion polymerizing preparation compound: add water 100Kg, emulsifying agent 3Kg in the reactor, stir, add vinylformic acid 5Kg, methyl methacrylate 8Kg again, after stirring, add initiator 0.3Kg again, polyreaction is carried out in heating, add Indian red 2Kg again, silica powder 6Kg stirs, after suction filtration, obtain polymkeric substance, then use washing with alcohol filter cake, after filter cake is dried, obtain performed polymer, the temperature of polyreaction is 75 DEG C, and polymerization reaction time is 2 hours, initiator is Potassium Persulphate, and emulsifying agent is Sodium dodecylbenzene sulfonate;
2nd step, by performed polymer, polyethylene terephthalate 50Kg, butyleneglycol double methacrylate 4Kg, oxidation inhibitor 0.6Kg, Silane coupling reagent KH-570 0.8Kg, lubricant 0.6Kg, glass fibre 15Kg, mix, obtain mixture; Described oxidation inhibitor is antioxidant 1010, and the length of described glass fibre is 10 ~ 500 microns;
3rd step, mixture is sent into extruding pelletization in twin screw extruder,, twin screw extruder extrusion temperature one district temperature 195 DEG C, two district's temperature 205 DEG C, three district's temperature 225 DEG C, four district's temperature 220 DEG C, five district's temperature 235 DEG C, screw speed is 200 rpm.
performance test
As can be seen from the table, polyester provided by the present invention has good physical strength and lower second-order transition temperature.Contrasting can find out by embodiment and reference examples 1, mechanical property can be improved significantly by introducing performed polymer; Can be found out by embodiment and reference examples 2, by glass fibre being prepared in the physical strength can improving polyester in performed polymer preferably.Can being found out by embodiment and reference examples 3, can second-order transition temperature be reduced by introducing Hydroxyethyl acrylate in performed polymer.
Claims (7)
1., based on a preparation method for the PET polyester of emulsion polymerization, it is characterized in that, comprise the steps:
1st step, emulsion polymerizing preparation compound: by weight, add 90 ~ 110 parts, water, emulsifying agent 2 ~ 4 parts in the reactor, stir, add 4 ~ 6 parts, vinylformic acid, Hydroxyethyl acrylate 4 ~ 7 parts, methyl methacrylate 5 ~ 9 parts again, after stirring, add initiator 0.2 ~ 0.4 part again, polyreaction is carried out in heating, add Indian red 1 ~ 2 part again, 10 ~ 20 parts, glass fibre, silica powder 4 ~ 8 parts stir, polymkeric substance is obtained after suction filtration, use washing with alcohol filter cake again, after being dried by filter cake, obtain performed polymer;
2nd step, by performed polymer, polyethylene terephthalate 40 ~ 60 parts, butyleneglycol double methacrylate 3 ~ 5 parts, nucleator 0.5 ~ 1 part, 0.5 ~ 1 part, oxidation inhibitor, silane coupling agent 0.5 ~ 1 part, lubricant 0.5 ~ 1 part, mix, obtain mixture;
3rd step, mixture is sent into extruding pelletization in twin screw extruder.
2. the preparation method of the PET polyester based on emulsion polymerization according to claim 1, is characterized in that: described initiator is selected from hydrogen peroxide, Potassium Persulphate, isopropyl benzene hydroperoxide, diisopropylbenzenehydroperoxide, p-propyl-toluene hydrogen peroxide.
3. the preparation method of the PET polyester based on emulsion polymerization according to claim 1, is characterized in that: described emulsifying agent is selected from Sodium dodecylbenzene sulfonate, hydroxy alkyl sulfonic acid sodium, diisooctyl succinate sodium sulfonate, polyacrylamide.
4. the preparation method of the PET polyester based on emulsion polymerization according to claim 1, is characterized in that: described silane coupling agent is the one in KH-550, KH-560 or KH-570.
5. the preparation method of the PET polyester based on emulsion polymerization according to claim 1, is characterized in that: described oxidation inhibitor is antioxidant 1010 or irgasfos 168.
6. the preparation method of the PET polyester based on emulsion polymerization according to claim 1, is characterized in that: the length of described glass fibre is preferably 10 ~ 500 microns.
7. the preparation method of the PET polyester based on emulsion polymerization according to claim 1, it is characterized in that: twin screw extruder extrusion temperature one district temperature 190 ~ 200 DEG C, two district's temperature 200 ~ 210 DEG C, three district's temperature 220 ~ 230 DEG C, four district's temperature 210 ~ 230 DEG C, five district's temperature 230 ~ 240 DEG C, screw speed is 180 ~ 220 rpm.
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| CN201410644528.2A CN104356614B (en) | 2014-11-14 | 2014-11-14 | A kind of preparation method of the PET polyester based on emulsion polymerization |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629235A (en) * | 2015-02-21 | 2015-05-20 | 刘平 | Method for preparing elastomer sheath material for wind energy cable |
| CN106328745A (en) * | 2016-08-27 | 2017-01-11 | 无锡中洁能源技术有限公司 | Solar back plate with high mechanical strength |
| CN107383802A (en) * | 2017-08-09 | 2017-11-24 | 张家港市六福新材料科技有限公司 | A kind of preparation method based on PET polyester composites |
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| WO2009112515A1 (en) * | 2008-03-11 | 2009-09-17 | Dsm Ip Assets B.V. | Fibre coated with a sizing composition |
| CN102675835A (en) * | 2012-04-17 | 2012-09-19 | 中山赛特工程塑料有限公司 | PET (Poly Ethylene Terephthalate) compound |
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Patent Citations (2)
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| WO2009112515A1 (en) * | 2008-03-11 | 2009-09-17 | Dsm Ip Assets B.V. | Fibre coated with a sizing composition |
| CN102675835A (en) * | 2012-04-17 | 2012-09-19 | 中山赛特工程塑料有限公司 | PET (Poly Ethylene Terephthalate) compound |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629235A (en) * | 2015-02-21 | 2015-05-20 | 刘平 | Method for preparing elastomer sheath material for wind energy cable |
| CN104629235B (en) * | 2015-02-21 | 2016-08-24 | 国家电网公司 | A kind of preparation method of wind energy cable elastic body jacket material |
| CN106328745A (en) * | 2016-08-27 | 2017-01-11 | 无锡中洁能源技术有限公司 | Solar back plate with high mechanical strength |
| CN107383802A (en) * | 2017-08-09 | 2017-11-24 | 张家港市六福新材料科技有限公司 | A kind of preparation method based on PET polyester composites |
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