CN103540108A - Production process for crystallized nano PET (Polythylene Terephthalate) plastic - Google Patents
Production process for crystallized nano PET (Polythylene Terephthalate) plastic Download PDFInfo
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- CN103540108A CN103540108A CN201310430786.6A CN201310430786A CN103540108A CN 103540108 A CN103540108 A CN 103540108A CN 201310430786 A CN201310430786 A CN 201310430786A CN 103540108 A CN103540108 A CN 103540108A
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Abstract
The invention discloses a production process for crystallized nano PET (Polythylene Terephthalate) plastic. The production process comprises the following steps: (1) preparing raw materials; (2) blending: mixing terephthalic acid prepared in the step (1) with ethylene glycol (EG), wherein the mass ratio of the terephthalic acid to the ethylene glycol (EG) is 1 to (1.5-2), adding a CaCO2 organic filling agent into a mixed solution, wherein the mass content of the filling agent is 3%-5% (3) carrying out an exchange reaction; (4) carrying out a condensation polymerization reaction; (5) enhancing and modifying; and (6) crystallizing and separating. According to the production process, after the raw materials are subjected to a series of treatment, PET rubber not only has a good physical and mechanical performance, good electrical insulating property, good creep resistance, good fatigue resistance, good wear resistance and good size stability in a wide temperature range, but also has a rapid crystallization rate and is easy to mold and process; the PET rubber has the characteristics of strong shock resistance and the like.
Description
Technical field
The manufacture craft of the plastic material the present invention relates to, particularly relates to a kind of manufacture craft of crystallization nanometer PET plastics.
Background technology
At present, plastics have been widely used in the fields such as construction industry, wrapping material, family daily necessity and automobile.Plastics are because of its purposes and good use properties and iron and steel widely, timber, cement has formed one of four large base mateirals of modern industry, PET plastics are polyethylene terephthalate plastics, be commonly called as polyester resin, it is the polycondensate of terephthalic acid and ethylene glycol, be referred to as thermoplastic polyester together with PBT, or saturated polyester, PET plastic molecules structure height is symmetrical, there is certain crystalline orientation ability, so there is higher film-forming properties and become second nature, PET plastics have good optical property and weathering resistance, amorphous PET plastics have good optical transparence, PET plastics have bottle that good abrasion performance frictional property and dimensional stability and electrical insulating property PET make to have intensity large in addition, the transparency is good, nontoxic, impermeable, quality is light, production efficiency is high thereby be subject to widely application, but PET plastics crystallization velocity is slow, shock resistance is poor, be difficult for processing.
Summary of the invention
For overcoming the deficiency in prior art, the object of the invention is to provide a kind of manufacture craft of crystallization nanometer PET plastics.
For realizing object of the present invention, technical scheme of the present invention is as follows:
A manufacture craft for crystallization nanometer PET plastics, its processing step is as follows:
(1) raw material is prepared; Under 250～300 ℃ of temperature of reaction and reaction pressure 2～2.5MPa condition, employing Zinc compounds is catalyzer, and crude terephthalic acid is made to high purity terephthalic acid (PTA), and getting its purity is 98%;
(2) blend; The terephthalic acid that step (1) is made mixes with ethylene glycol (EG), and the mass ratio of described terephthalic acid and ethylene glycol (EG) is 1:1.5 ~ 2, and in described mixed solution, adding CaCO3 organic filler, the mass content of described weighting agent is 3% ~ 5%;
(3) permutoid reaction; In the mixture of step (2), add catalyzer, under the effect of catalyzer, terephthalic acid and ethylene glycol generation permutoid reaction, described catalyzer is the acetate of zinc, cobalt, manganese and the mixture of antimonous oxide, described catalyst levels is 0.01% ~ 0.05% of terephthalic acid quality;
(4) polycondensation; The reaction product of step (3) is imported to polycondensation vessel, and controlling temperature of reaction is 270 ℃ ~ 280 ℃, under high vacuum and strong mixing, carries out, and obtains the polyester of high molecular;
(5) enhancing modified; In polycondensation vessel, add plastics toughener, nano flame retardant mixture, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; Described nano flame retardant mixture is 10%-15%,
The preparation method of described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, 60 ℃ of temperature, be dried 24 hours, grinding is sieved, and obtains modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.Filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at 600W power ultrasonic, with constant temperature heating device, be heated to 90 ℃, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain nano flame retardant mixture;
(6) Crystallization Separation; Mixture after step (4) is carried out to crystallization operation, temperature is controlled to 200 ℃ ~ 210 ℃, drops into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 0.9 ~ 1.5% of terephthalic acid quality, obtains PET plastics after crystallization.
The manufacture craft of above-mentioned a kind of crystallization nanometer PET plastics, wherein, in described step (3), carries out under the acidic conditions that described permutoid reaction is 5 ~ 6 at pH.
The manufacture craft of above-mentioned a kind of crystallization nanometer PET plastics, wherein, in described step (4), described polyester is along with reaction migrates out polycondensation vessel gradually.
The manufacture craft of above-mentioned a kind of crystallization nanometer PET plastics, wherein, in described step (6), the dry the finished product that obtain of described PET plastic warp washing.
Beneficial effect: make raw material through preparing, blend, permutoid reaction, polycondensation, enhancing modified, six steps of Crystallization Separation, make PET rubber not only in wide temperature range, there is good physical and mechanical properties, electrical insulating property is good, creep resistance, resistance to fatigue, rub resistance, good stability of the dimension, and crystallization rate is fast, forming process is easy, there is the stronger features such as shock resistance, the terephthalic acid of high-purity in raw material preparation, guarantee the high purity of plastics product, enhance productivity, in Blending Processes, added organic filler, make plastics be easy to processing, in permutoid reaction, catalyzer chooses, reaction plastics have greatly been improved, the control of temperature of reaction is better has guaranteed the stable of the excellent physical and mechanical properties of plastics and size, under the condition of high vacuum and strong mixing, reaction generates the polyester of high molecular, the plastics toughener adding makes plastics possess very strong shock resistance, the crystallization promoter using in Crystallization Separation operation, make the crystallization velocity of plastics fast, raise the efficiency, be convenient to collect, acid condition has katalysis to permutoid reaction, product is shifted out to reactor simultaneously, more accelerated the generation of plastics.Fire retardant prepared by the present invention is not halogen-containing, organism, and asepsis environment-protecting, has a extensive future; The present invention carries out twice-modified, such benefit: increase reactive behavior point, improve modified effect; In the time of modification, can steam again except the moisture in system, dry and modification is carried out simultaneously, has improved working efficiency; In nano silicone hydroxyapatite, Attapulgite, polynite, kaolin etc. self micropore, have a large amount of physics and chemistry planar water, at high temperature produce water vapor, blocking-up oxygen, absorbs heat, reaches multiple fire-retardant effect; Powerful absorption property can effectively improve the synergy of several fire retardants, stops and is raise by fire retardant matter temperature, has improved flame retarding efficiency; The aboundresources such as silicon hydroxyapatite, Attapulgite, polynite, kaolin, greatly reduce the industrial cost of fire retardant, and also the Application and Development for attapulgite provides a new way; The present invention adopts solution method ultrasonic wave to disperse and mechanical high-speed agitator stirs, make fire retardant separately component in solution, reached nano level dispersion, effectively avoided the natural oxidation to matrix material, thereby made matrix material there is better mechanical property.The oxygen index of matrix material is 41.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with embodiment, further set forth the present invention.
Embodiment 1:
The manufacture craft of a kind of crystallization nanometer PET plastics of the present embodiment, its processing step is as follows:
(1) raw material is prepared; Under 250～300 ℃ of temperature of reaction and reaction pressure 2～2.5MPa condition, employing Zinc compounds is catalyzer, and crude terephthalic acid is made to high purity terephthalic acid (PTA), and getting its purity is 98%;
(2) blend; The terephthalic acid that step (1) is made mixes with ethylene glycol (EG), and the mass ratio of described terephthalic acid and ethylene glycol (EG) is 1:1.5 ~ 2, and in described mixed solution, adding CaCO3 organic filler, the mass content of described weighting agent is 3% ~ 5%;
(3) permutoid reaction; In the mixture of step (2), add catalyzer, under the effect of catalyzer, terephthalic acid and ethylene glycol generation permutoid reaction, described catalyzer is the acetate of zinc, cobalt, manganese and the mixture of antimonous oxide, described catalyst levels is 0.01% ~ 0.05% of terephthalic acid quality;
(4) polycondensation; The reaction product of step (3) is imported to polycondensation vessel, and controlling temperature of reaction is 270 ℃ ~ 280 ℃, under high vacuum and strong mixing, carries out, and obtains the polyester of high molecular;
(5) enhancing modified; In polycondensation vessel, add plastics toughener, nano flame retardant mixture, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; Described nano flame retardant mixture is 10%-15%,
The preparation method of described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, 60 ℃ of temperature, be dried 24 hours, grinding is sieved, and obtains modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.Filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at 600W power ultrasonic, with constant temperature heating device, be heated to 90 ℃, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain nano flame retardant mixture;
(6) Crystallization Separation; Mixture after step (4) is carried out to crystallization operation, temperature is controlled to 200 ℃ ~ 210 ℃, drops into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 0.9 ~ 1.5% of terephthalic acid quality, obtains PET plastics after crystallization.
Wherein, in described step (3), under the acidic conditions that described permutoid reaction is 5 ~ 6 at pH, carry out,
Crucial, in described step (4), described polyester is along with reaction migrates out polycondensation vessel gradually, and in described step (6), described PET plastic warp washing is dried and obtains the finished product.
Embodiment 2: all the other are identical with described embodiment 1, and difference is, the terephthalic acid purity of preparing in step (1) is medium, and in the present embodiment, cost is relatively low, but it is slow to make the speed of reaction of plastics, and efficiency is low, and plastics physicals reduces.
Embodiment 3: all the other are identical with described embodiment 1, and difference is, changes crystallization promoter: changing Sodium Benzoate is organic montmorillonoid in step (6), and in this enforcement, corresponding temperature of reaction increases, and crystallization effect is poorer than embodiment 1.
Known in practical application, make raw material through preparing, blend, permutoid reaction, polycondensation, enhancing modified, six steps of Crystallization Separation, make PET rubber not only in wide temperature range, there is good physical and mechanical properties, electrical insulating property is good, creep resistance, resistance to fatigue, rub resistance, good stability of the dimension, and crystallization rate is fast, forming process is easy, there is the stronger features such as shock resistance, the terephthalic acid of high-purity in raw material preparation, guarantee the high purity of plastics product, enhance productivity, in Blending Processes, added organic filler, make plastics be easy to processing, in permutoid reaction, catalyzer chooses, reaction plastics have greatly been improved, the control of temperature of reaction is better has guaranteed the stable of the excellent physical and mechanical properties of plastics and size, under the condition of high vacuum and strong mixing, reaction generates the polyester of high molecular, the plastics toughener adding makes plastics possess very strong shock resistance, the crystallization promoter using in Crystallization Separation operation, make the crystallization velocity of plastics fast, raise the efficiency, be convenient to collect, acid condition has katalysis to permutoid reaction, product is shifted out to reactor simultaneously, more accelerated the generation of plastics.Fire retardant prepared by the present invention is not halogen-containing, organism, and asepsis environment-protecting, has a extensive future; The present invention carries out twice-modified, such benefit: increase reactive behavior point, improve modified effect; In the time of modification, can steam again except the moisture in system, dry and modification is carried out simultaneously, has improved working efficiency; In nano silicone hydroxyapatite, Attapulgite, polynite, kaolin etc. self micropore, have a large amount of physics and chemistry planar water, at high temperature produce water vapor, blocking-up oxygen, absorbs heat, reaches multiple fire-retardant effect; Powerful absorption property can effectively improve the synergy of several fire retardants, stops and is raise by fire retardant matter temperature, has improved flame retarding efficiency; The aboundresources such as silicon hydroxyapatite, Attapulgite, polynite, kaolin, greatly reduce the industrial cost of fire retardant, and also the Application and Development for attapulgite provides a new way; The present invention adopts solution method ultrasonic wave to disperse and mechanical high-speed agitator stirs, make fire retardant separately component in solution, reached nano level dispersion, effectively avoided the natural oxidation to matrix material, thereby made matrix material there is better mechanical property.The oxygen index of matrix material is 41.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes content of the present invention to do, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (5)
1. a manufacture craft for crystallization nanometer PET plastics, is characterized in that, its processing step is as follows:
(1) raw material is prepared; Under 250～300 ℃ of temperature of reaction and reaction pressure 2～2.5MPa condition, employing Zinc compounds is catalyzer, and crude terephthalic acid is made to high purity terephthalic acid (PTA), and getting its purity is 98%;
(2) blend; The terephthalic acid that step (1) is made mixes with ethylene glycol (EG), and the mass ratio of described terephthalic acid and ethylene glycol (EG) is 1:1.5 ~ 2, and in described mixed solution, adding CaCO3 organic filler, the mass content of described weighting agent is 3% ~ 5%;
(3) permutoid reaction; In the mixture of step (2), add catalyzer, under the effect of catalyzer, terephthalic acid and ethylene glycol generation permutoid reaction, described catalyzer is the acetate of zinc, cobalt, manganese and the mixture of antimonous oxide, described catalyst levels is 0.01% ~ 0.05% of terephthalic acid quality;
(4) polycondensation; The reaction product of step (3) is imported to polycondensation vessel, and controlling temperature of reaction is 270 ℃ ~ 280 ℃, under high vacuum and strong mixing, carries out, and obtains the polyester of high molecular;
(5) enhancing modified; In polycondensation vessel, add plastics toughener, nano flame retardant mixture, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; Described nano flame retardant mixture is 10%-15%,
The preparation method of described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, 60 ℃ of temperature, be dried 24 hours, grinding is sieved, and obtains modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.
2. filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at 600W power ultrasonic, with constant temperature heating device, be heated to 90 ℃, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain nano flame retardant mixture;
(6) Crystallization Separation; Mixture after step (4) is carried out to crystallization operation, temperature is controlled to 200 ℃ ~ 210 ℃, drops into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 0.9 ~ 1.5% of terephthalic acid quality, obtains PET plastics after crystallization.
3. the manufacture craft of crystallization nanometer PET plastics according to claim 1, is characterized in that, in described step (3), under the acidic conditions that described permutoid reaction is 5 ~ 6 at pH, carries out.
4. the manufacture craft of crystallization nanometer PET plastics according to claim 1, is characterized in that, in described step (4), described polyester is along with reaction migrates out polycondensation vessel gradually.
5. the manufacture craft of crystallization nanometer PET plastics according to claim 1, is characterized in that, in described step (6), and the dry the finished product that obtain of described PET plastic warp washing.
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Cited By (2)
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| CN104513464A (en) * | 2014-12-31 | 2015-04-15 | 广西大学 | Production process for PET plastic |
| CN104861185A (en) * | 2015-04-28 | 2015-08-26 | 安徽美翔塑业有限公司 | Thin film production process |
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| CN104513464A (en) * | 2014-12-31 | 2015-04-15 | 广西大学 | Production process for PET plastic |
| CN104861185A (en) * | 2015-04-28 | 2015-08-26 | 安徽美翔塑业有限公司 | Thin film production process |
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