CN103665782A - Manufacture technology for anti-bacterial PET (polybutylene terephthalate) membrane - Google Patents
Manufacture technology for anti-bacterial PET (polybutylene terephthalate) membrane Download PDFInfo
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- CN103665782A CN103665782A CN201310550323.3A CN201310550323A CN103665782A CN 103665782 A CN103665782 A CN 103665782A CN 201310550323 A CN201310550323 A CN 201310550323A CN 103665782 A CN103665782 A CN 103665782A
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Abstract
The invention discloses a manufacture technology for an anti-bacterial PET (polybutylene terephthalate) membrane. The manufacture technology comprises the following steps: (1) preparing raw materials; (2) mixing terephthalic acid prepared in step (1) with ethylene glycol (EG), adding organic filler CaCO3 into the mixed liquid, wherein the mass ratio of terephthalic acid to ethylene glycol (EG) is 1:(1.5-2), the mass content of the filler is 3%-5%; (3) carrying out exchange reaction; (4) carrying out condensation polymerization; (5) reinforcing and modifying; (6) crystallizing and separating. After a series of treatment on the raw material, the PET rubber not only has excellent physical mechanical property, electrical insulating property, creep resistance, fatigue durability, abrasion resistance and dimensional stability in wider temperature range, but also has characteristics of having fast crystallization rate and strong shock resistance, and being easy to mold and process.
Description
Technical field
The manufacture craft of the plastic material the present invention relates to, particularly relates to a kind of manufacture craft of antibacterial PET film.
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 antibacterial PET film.
For realizing object of the present invention, technical scheme of the present invention is as follows:
A manufacture craft for antibacterial PET film, 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, the antibacterial mixture of plant-sourced, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; The antibacterial mixture of described plant-sourced is 10%-15%,
The preparation method of the described antibacterial mixture of plant-sourced is:
Huang Dingju, Herba Eupatorii Odorati, Root or all-grass of Cairo Morningglory, Herba Agerati Conyzoidis, Rhizoma Alpiniae Officinarum, garlic, Sheep's-parsley, water are mixed according to the mass fraction proportioning of 20-25:15-20:10-15: 10-15:8-10:8-10:5-7:10-20, add the cellulase of (unit of activity of 10 parts is 100U) to carry out enzymolysis, enzyme digestion reaction temperature is 30 ℃, the enzyme digestion reaction time is 1 hour, filters and obtains Chinese herbal medicine fluid; After removing slag, adding concentration is 50%～70% aqueous ethanolic solution again, again by solidliquid mixture ultrasonic-assisted extraction, ultrasonic extraction condition: ultrasonic temperature is that 45～56 ℃, ultrasonic frequency are that 20～30kHz, supersound extraction time are 1～2 hour, then by solidliquid mixture suction filtration under 20～30kPa vacuum condition, get filtrate underpressure distillation under 15～25kPa vacuum, 45～50 ℃ of conditions and obtain plant-sourced compound disinfectant.
(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 antibacterial PET film, 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 antibacterial PET film, 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 antibacterial PET film, 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.There is thin-film material, the environmental protection of sterilization effect and there is fungistatic effect; Harmless to people, animal.In addition, the present invention fills a prescription rationally, and preparation method is simple.
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 antibacterial PET film 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, the antibacterial mixture of plant-sourced, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; The antibacterial mixture of described plant-sourced is 10%-15%,
The preparation method of the described antibacterial mixture of plant-sourced is:
Huang Dingju, Herba Eupatorii Odorati, Root or all-grass of Cairo Morningglory, Herba Agerati Conyzoidis, Rhizoma Alpiniae Officinarum, garlic, Sheep's-parsley, water are mixed according to the mass fraction proportioning of 20-25:15-20:10-15: 10-15:8-10:8-10:5-7:10-20, add the cellulase of (unit of activity of 10 parts is 100U) to carry out enzymolysis, enzyme digestion reaction temperature is 30 ℃, the enzyme digestion reaction time is 1 hour, filters and obtains Chinese herbal medicine fluid; After removing slag, adding concentration is 50%～70% aqueous ethanolic solution again, again by solidliquid mixture ultrasonic-assisted extraction, ultrasonic extraction condition: ultrasonic temperature is that 45～56 ℃, ultrasonic frequency are that 20～30kHz, supersound extraction time are 1～2 hour, then by solidliquid mixture suction filtration under 20～30kPa vacuum condition, get filtrate underpressure distillation under 15～25kPa vacuum, 45～50 ℃ of conditions and obtain plant-sourced compound disinfectant.
(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.The thin-film material with sterilization effect, environmental protection prepared by the present invention and there is fungistatic effect; Harmless to people, animal.In addition, the present invention fills a prescription rationally, and preparation method is simple.
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 description 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 antibacterial PET film, 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, the antibacterial mixture of plant-sourced, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; The antibacterial mixture of described plant-sourced is 10%-15%,
The preparation method of the described antibacterial mixture of plant-sourced is:
Huang Dingju, Herba Eupatorii Odorati, Root or all-grass of Cairo Morningglory, Herba Agerati Conyzoidis, Rhizoma Alpiniae Officinarum, garlic, Sheep's-parsley, water are mixed according to the mass fraction proportioning of 20-25:15-20:10-15: 10-15:8-10:8-10:5-7:10-20, add the cellulase of (unit of activity of 10 parts is 100U) to carry out enzymolysis, enzyme digestion reaction temperature is 30 ℃, the enzyme digestion reaction time is 1 hour, filters and obtains Chinese herbal medicine fluid; After removing slag, adding concentration is 50%～70% aqueous ethanolic solution again, again by solidliquid mixture ultrasonic-assisted extraction, ultrasonic extraction condition: ultrasonic temperature is that 45～56 ℃, ultrasonic frequency are that 20～30kHz, supersound extraction time are 1～2 hour, then by solidliquid mixture suction filtration under 20～30kPa vacuum condition, get filtrate underpressure distillation under 15～25kPa vacuum, 45～50 ℃ of conditions and obtain plant-sourced compound disinfectant.
2.(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 antibacterial PET film 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 antibacterial PET film 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 antibacterial PET film 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513464A (en) * | 2014-12-31 | 2015-04-15 | 广西大学 | Production process for PET plastic |
| CN105077898A (en) * | 2015-08-19 | 2015-11-25 | 树业环保科技股份有限公司 | PET non-woven fabric shopping bag and preparation method thereof |
| CN112708162A (en) * | 2020-12-18 | 2021-04-27 | 天津宝兴威科技股份有限公司 | Preparation method of PET film for locally wiping liquid crystal writing board |
| CN114085502A (en) * | 2021-12-02 | 2022-02-25 | 苏州佳尔特新材料科技股份有限公司 | Flame-retardant antibacterial PET film and production process thereof |
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| US20030118817A1 (en) * | 2000-02-19 | 2003-06-26 | Ursula Murschall | Sealable, flame-resistant, co-extruded, biaxially oriented foil that is mat on one side and a method for producing and using same |
| CN101402722A (en) * | 2008-11-26 | 2009-04-08 | 吉林大学 | Method for preparing nano-calcium carbonate/polyester composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513464A (en) * | 2014-12-31 | 2015-04-15 | 广西大学 | Production process for PET plastic |
| CN105077898A (en) * | 2015-08-19 | 2015-11-25 | 树业环保科技股份有限公司 | PET non-woven fabric shopping bag and preparation method thereof |
| CN112708162A (en) * | 2020-12-18 | 2021-04-27 | 天津宝兴威科技股份有限公司 | Preparation method of PET film for locally wiping liquid crystal writing board |
| CN114085502A (en) * | 2021-12-02 | 2022-02-25 | 苏州佳尔特新材料科技股份有限公司 | Flame-retardant antibacterial PET film and production process thereof |
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| CN103665782B (en) | 2015-11-25 |
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