CN104448722A - Preparation technology for PBT plastic - Google Patents
Preparation technology for PBT plastic Download PDFInfo
- Publication number
- CN104448722A CN104448722A CN201310433128.2A CN201310433128A CN104448722A CN 104448722 A CN104448722 A CN 104448722A CN 201310433128 A CN201310433128 A CN 201310433128A CN 104448722 A CN104448722 A CN 104448722A
- Authority
- CN
- China
- Prior art keywords
- terephthalic acid
- reaction
- crystallization
- pbt plastic
- pbt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Polyesters Or Polycarbonates (AREA)
Abstract
A disclosed preparation technology for PBT plastic comprises the technological steps: (1) preparing raw materials; (2) mixing; (3) performing catalytic reaction; (4) forming a material; (5) modifying; and (6) performing crystallization separation. After the raw materials are subjected to a series of processing, the PBT rubber has excellent physical mechanical properties, excellent electric insulating property, creep resistance, fatigue resistance and good friction resistance and dimension stability at a relatively wide temperature scope, also is fast in crystallization speed and easy for forming processing, and has the characteristics of relatively strong impact resistance and the like.
Description
Technical field
The present invention relates to chemical technique, particularly relate to a kind of manufacture craft of PBT plastic.
Background technology
At present, plastics have been widely used in the fields such as construction industry, wrapping material, family daily necessity and automobile.Plastics because of its widely purposes and good use properties and and iron and steel, timber, one of cement four large base mateirals constituting modern industry, PBT plastic is polyethylene terephthalate plastics, be commonly called as polyester resin, it is the polycondensate of terephthalic acid and ethylene glycol, thermoplastic polyester is referred to as together with PET, or saturated polyester, PBT plastic molecular structure high degree of symmetry, there is certain crystalline orientation ability, so there is higher film-forming properties and become second nature, PBT plastic has good optical property and weathering resistance, amorphous PBT plastic has good optical transparence, PBT plastic has bottle that excellent abrasion performance frictional property and dimensional stability and electrical insulating property PBT make to have intensity large in addition, the transparency is good, nontoxic, impermeable, quality is light, high thus the receiving of production efficiency is applied widely, application number is that CN201210048852.9 discloses a kind of high-performance environment-friendly modified PBT, it is prepared from by following material component: component A is PBT raw material, this PBT raw material is original novel material or is obtained by reworked material mixing novel material, component B is subsidiary material, and these subsidiary material at least include halogen-free flame retardants, toughner, compatilizer and glass, during preparation, get by weight percentage the halogen-free flame retardants of 15 ~ 20%, 5 ~ 10% toughner, the compatilizer of 3 ~ 5%, the glass of 25 ~ 35% and surplus be the proportioning of PBT raw material, by granulation after molecular breakdown, restructuring.The present invention take PBT as carrier, add these subsidiary material such as halogen-free flame retardants, toughner, compatilizer, glass and make high-performance environment-friendly modified PBT, its environmental requirement that can improve the fire prevention degree of product and physicals and reach non-halogen non-phosphate, meet industry to utilize, not containing I, Br, the health of environment and people is safe from harm, but this PBT plastics crystallization velocity is slow, shock resistance is poor, not easily processes.
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 PBT plastic.
For realizing object of the present invention, technical scheme of the present invention is as follows:
A manufacture craft for PBT plastic, its processing step is as follows:
(1) raw material prepares; Under temperature of reaction 250 ~ 300 DEG C and reaction pressure 2 ~ 2.5MPa condition, employing zinc oxide is catalyzer, crude terephthalic acid is made high purity terephthalic acid (PTA), and getting its purity is 80%;
(2) mix; Mixed with BDO by terephthalic acid made for step (1), the mass ratio of described terephthalic acid and BDO is 1:1.5 ~ 2, adds precipitated chalk in described mixed solution, and the mass content of described precipitated chalk is 2% ~ 3%;
(3) catalyzed reaction; Catalyzer is added in the mixture of step (2), under the effect of catalyzer, terephthalic acid and BDO generation permutoid reaction, described catalyzer is calcium acetate, and described catalyst levels is 0.01% ~ 0.02% of terephthalic acid quality;
(4) material is become; The reaction product of step (3) is imported polycondensation vessel, and controlling temperature of reaction is 370 DEG C ~ 380 DEG C, carries out under high vacuum and strong mixing, obtains the polyester of high molecular;
(5) modification; In polycondensation vessel, add plastics toughener, stir simultaneously, described plastics toughener is polyurethane propylene vinegar, and its consumption is 5 ~ 6%;
(6) Crystallization Separation; Crystallization operation is carried out to the mixture after step (4), temperature controlled at 300 DEG C ~ 310 DEG C, drop into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 1.0 ~ 1.2% of terephthalic acid quality, obtains PBT plastic after crystallization.
The manufacture craft of above-mentioned a kind of PBT plastic, wherein, in described step (3), described catalyzed reaction is carried out under pH is the acidic conditions of 6 ~ 7.
The manufacture craft of above-mentioned a kind of PBT plastic, wherein, in described step (5), described plastics toughener slowly adds in polycondensation vessel.
The manufacture craft of above-mentioned a kind of PBT plastic, wherein, in described step (5), controlling temperature of reaction is 400 DEG C.
Beneficial effect: make raw material through preparing, mixing, catalyzed reaction, become material, modification, Crystallization Separation six steps, PBT rubber is made not only in wide temperature range, to have excellent physical and mechanical properties, electrical insulating property is excellent, creep resistance, resistance to fatigue, rub resistance, good stability of the dimension, and crystallization rate is fast, forming process is easy, there is the features such as stronger shock resistance, the terephthalic acid of moderate purity produced by raw material in preparing, guarantee the cheap and easy to get of plastics product, enhance productivity, precipitated chalk is added in Blending Processes, plastics are made to be easy to processing, in catalyzed reaction, catalyzer chooses, greatly improve reaction plasticity, the control of temperature of reaction is better ensure that the physical and mechanical properties of the excellence of plastics and the stable of size, under the condition of high vacuum and strong mixing, reaction generates the polyester of high molecular, the plastics toughener added makes plastics possess very strong shock resistance, the crystallization promoter used 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 reactor simultaneously, more accelerate the generation of plastics.
Embodiment
The technique means realized for making the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with embodiment, setting forth the present invention further.
embodiment 1:
The manufacture craft of a kind of PBT plastic of the present embodiment, its processing step is as follows:
(1) raw material prepares; Under temperature of reaction 250 ~ 300 DEG C and reaction pressure 2 ~ 2.5MPa condition, employing zinc oxide is catalyzer, crude terephthalic acid is made high purity terephthalic acid (PTA), and getting its purity is 80%;
(2) mix; Mixed with BDO by terephthalic acid made for step (1), the mass ratio of described terephthalic acid and BDO is 1:1.5 ~ 2, adds precipitated chalk in described mixed solution, and the mass content of described precipitated chalk is 2% ~ 3%;
(3) catalyzed reaction; Catalyzer is added in the mixture of step (2), under the effect of catalyzer, terephthalic acid and 1,4-butyleneglycol generation permutoid reaction, control pH is 6 ~ 7, and described catalyzer is calcium acetate, and described catalyst levels is 0.01% ~ 0.02% of terephthalic acid quality;
(4) material is become; The reaction product of step (3) is imported polycondensation vessel, and controlling temperature of reaction is 370 DEG C ~ 380 DEG C, carries out under high vacuum and strong mixing, obtains the polyester of high molecular;
(5) modification; In polycondensation vessel, slowly add plastics toughener, stir simultaneously, described plastics toughener is polyurethane propylene vinegar, and its consumption is 5 ~ 6%, and controlling temperature of reaction is 400 DEG C.；
(6) Crystallization Separation; Crystallization operation is carried out to the mixture after step (4), temperature is controlled at 300 DEG C ~ 310 DEG C, drop into crystallization promoter, and stir, described crystallization promoter is Sodium Benzoate, and described Sodium Benzoate consumption is 1.0 ~ 1.2% of terephthalic acid quality, obtains PBT plastic after crystallization.
embodiment 2:all the other are identical with described embodiment 1, difference is, in step (2), the mass ratio of terephthalic acid and BDO is 1:1.5, in step (3), catalyst levels is 0.02% of terephthalic acid quality, and in step (6), Sodium Benzoate consumption is 1.2% of terephthalic acid quality.
embodiment 3:all the other are identical with described embodiment 1, difference is, in step (2), the mass ratio of terephthalic acid and BDO is 1:2, in step (3), catalyst levels is 0.01% of terephthalic acid quality, and in step (6), Sodium Benzoate consumption is 1.2% of terephthalic acid quality.
In above-mentioned three kinds of embodiments, polycondensation is there is under the condition of high vacuum and strong mixing, the utilization ratio of reactant terephthaldehyde acid butyl ester reaches more than 85%, catalyzed reaction adds terephthalic acid transformation efficiency and reaches more than 90%, and the use of crystallization promoter makes the crystallization rate of product improve more than 2 times.
Known in practical application, make raw material through preparing, mixing, catalyzed reaction, become material, modification, Crystallization Separation six steps, PBT rubber is made not only in wide temperature range, to have excellent physical and mechanical properties, electrical insulating property is excellent, creep resistance, resistance to fatigue, rub resistance, good stability of the dimension, and crystallization rate is fast, forming process is easy, there is the features such as stronger shock resistance, the terephthalic acid of moderate purity produced by raw material in preparing, guarantee the cheap and easy to get of plastics product, enhance productivity, precipitated chalk is added in Blending Processes, plastics are made to be easy to processing, in catalyzed reaction, catalyzer chooses, greatly improve reaction plasticity, the control of temperature of reaction is better ensure that the physical and mechanical properties of the excellence of plastics and the stable of size, under the condition of high vacuum and strong mixing, reaction generates the polyester of high molecular, the plastics toughener added makes plastics possess very strong shock resistance, the crystallization promoter used 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 reactor simultaneously, more accelerate the generation of plastics.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention to do equivalent structure or the conversion of equivalent flow process, 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 (4)
1. a manufacture craft for PBT plastic, is characterized in that, its processing step is as follows:
(1) raw material prepares; Under temperature of reaction 250 ~ 300 DEG C and reaction pressure 2 ~ 2.5MPa condition, employing zinc oxide is catalyzer, crude terephthalic acid is made high purity terephthalic acid (PTA), and getting its purity is 80%;
(2) mix; Mixed with BDO by terephthalic acid made for step (1), the mass ratio of described terephthalic acid and BDO is 1:1.5 ~ 2, adds precipitated chalk in described mixed solution, and the mass content of described precipitated chalk is 2% ~ 3%;
(3) catalyzed reaction; Catalyzer is added in the mixture of step (2), under the effect of catalyzer, terephthalic acid and BDO generation permutoid reaction, described catalyzer is calcium acetate, and described catalyst levels is 0.01% ~ 0.02% of terephthalic acid quality;
(4) material is become; The reaction product of step (3) is imported polycondensation vessel, and controlling temperature of reaction is 370 DEG C ~ 380 DEG C, carries out under high vacuum and strong mixing, obtains the polyester of high molecular;
(5) modification; In polycondensation vessel, add plastics toughener, stir simultaneously, described plastics toughener is polyurethane propylene vinegar, and its consumption is 5 ~ 6%;
(6) Crystallization Separation; Crystallization operation is carried out to the mixture after step (4), temperature controlled at 300 DEG C ~ 310 DEG C, drop into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 1.0 ~ 1.2% of terephthalic acid quality, obtains PBT plastic after crystallization.
2. the manufacture craft of PBT plastic according to claim 1, is characterized in that, in described step (3), described catalyzed reaction is carried out under pH is the acidic conditions of 6 ~ 7.
3. the manufacture craft of PBT plastic according to claim 1, is characterized in that, in described step (5), described plastics toughener slowly adds in polycondensation vessel.
4. the manufacture craft of PBT plastic according to claim 1, is characterized in that, in described step (5), controlling temperature of reaction is 400 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310433128.2A CN104448722A (en) | 2013-09-23 | 2013-09-23 | Preparation technology for PBT plastic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310433128.2A CN104448722A (en) | 2013-09-23 | 2013-09-23 | Preparation technology for PBT plastic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104448722A true CN104448722A (en) | 2015-03-25 |
Family
ID=52895511
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310433128.2A Pending CN104448722A (en) | 2013-09-23 | 2013-09-23 | Preparation technology for PBT plastic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104448722A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369024A (en) * | 2021-12-31 | 2022-04-19 | 河南金丹乳酸科技股份有限公司 | PTA and BDO esterification process for PBAT production |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093543A (en) * | 2009-12-14 | 2011-06-15 | 上海杰事杰新材料(集团)股份有限公司 | Method for preparing 2,3-polybutylece terephthalate and copolyester thereof |
| CN102964579A (en) * | 2012-12-06 | 2013-03-13 | 盘锦科隆精细化工有限公司 | Reinforced thermoplastic polyester elastomer and preparation method thereof |
| CN103304788A (en) * | 2013-06-06 | 2013-09-18 | 张家港市宝田新型材料科技有限公司 | Preparation method of polybutylene terephthalate polyester resin |
-
2013
- 2013-09-23 CN CN201310433128.2A patent/CN104448722A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093543A (en) * | 2009-12-14 | 2011-06-15 | 上海杰事杰新材料(集团)股份有限公司 | Method for preparing 2,3-polybutylece terephthalate and copolyester thereof |
| CN102964579A (en) * | 2012-12-06 | 2013-03-13 | 盘锦科隆精细化工有限公司 | Reinforced thermoplastic polyester elastomer and preparation method thereof |
| CN103304788A (en) * | 2013-06-06 | 2013-09-18 | 张家港市宝田新型材料科技有限公司 | Preparation method of polybutylene terephthalate polyester resin |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369024A (en) * | 2021-12-31 | 2022-04-19 | 河南金丹乳酸科技股份有限公司 | PTA and BDO esterification process for PBAT production |
| CN114369024B (en) * | 2021-12-31 | 2024-01-30 | 河南金丹乳酸科技股份有限公司 | PTA and BDO esterification process for PBAT production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR20160011705A (en) | New biodegradable masterbatch and preparation method thereof | |
| CN103709383B (en) | Titanium series polyester catalyst and its preparation method and application | |
| CN101691524A (en) | Method for preparing epoxidized soybean oil with high epoxy value by fractional step method | |
| WO2012032876A1 (en) | Method for producing polyester compositions | |
| CN102731755A (en) | Method for preparing plasticizer | |
| CN101891884A (en) | Polyester polycondensation catalyst and preparation method and application thereof | |
| CN102634174A (en) | Preparation method of flame-retardant copolyester film of phosphorus, silicon and fluorine | |
| EP3875514B1 (en) | Copolymerized polyester resin, molded product, and heat-shrinkable film | |
| CN107955142B (en) | Process for preparing isosorbide-containing polyesters | |
| CN102660009B (en) | Preparation method of flame-retardant linear copolyester resin | |
| CN103665782B (en) | A kind of manufacture craft of antibacterial PET film | |
| KR20170082565A (en) | Concentrate composition for polymeric chain extension | |
| CN109517148B (en) | Environment-friendly bottle polyester and preparation method thereof | |
| CN103665781B (en) | The manufacture craft of the PET that a kind of crystallization is easily processed soon | |
| CN103951815A (en) | Preparation method of polyester for highlight flame-retardant polyester thin film | |
| CN104448722A (en) | Preparation technology for PBT plastic | |
| CN104284917A (en) | Method for manufacturing ester composition, and resin composition | |
| EP4137528A1 (en) | Copolyester resin, molded article, heat-shrinkable film, and fiber | |
| CN104292773A (en) | Process for preparing PBT plastic | |
| CN101234355A (en) | High-efficiency catalyst for synthesizing di(2-ethylhexyl) terephthalate | |
| CN106046622B (en) | It is a kind of to be used to manufacture material of cable insulation and preparation method thereof | |
| CN103540108B (en) | A kind of manufacture craft of crystallization nanometer PET | |
| CN104017348A (en) | Polypropylene carbonate modified composite material and preparation method thereof | |
| KR20090068771A (en) | A thermoplastic polyester resin and a mothod for preparing the same | |
| CN108659210B (en) | Heterogeneous catalyst and application thereof in polyester preparation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150325 |
|
| WD01 | Invention patent application deemed withdrawn after publication |