CN113416391A - Modified PBT polymer with improved shrinkage performance and preparation process thereof - Google Patents
Modified PBT polymer with improved shrinkage performance and preparation process thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of PBT modification, and particularly relates to a modified PBT polymer with improved shrinkage performance and a preparation process thereof. The modified PBT polymer comprises the following raw materials: polybutylene terephthalate, polypropylene copolymer, metallic lead, glass fiber, nano-cellulose, chalcopyrite, other mineral substances, organic nano-montmorillonite, nano-zinc nitride, active silicon micro-powder, a curing agent, an activating agent and a cross-linking agent. The modified polymer of the invention adopts the copolymerized polypropylene, the metallic lead, the ore and the nano material to modify and strengthen the PBT in the prior art of adopting the glass fiber, improves the rigidity, the impact resistance and the dimensional stability of the PBT, comprehensively improves the mechanical property and the chemical resistance of the PBT, obtains the PBT injection molding resin with excellent thermal property and low shrinkage, enlarges the application field of the PBT, and is suitable for the application of household appliance parts such as electric heating equipment, oven grills and the like.
Description
Technical Field
The invention belongs to the technical field of PBT modification, and particularly relates to a modified PBT polymer with improved shrinkage performance and a preparation process thereof.
Background
Polybutylene terephthalate PBT, also known as polytetramethylene terephthalate, or polybutylene terephthalate resin, is made by transesterification of 1, 4-butanediol with dimethyl terephthalate or by direct esterification with purified terephthalic acid, followed by polycondensation. PBT is the latest and fastest-developing variety found in five engineering plastics, has excellent mechanical properties, self-lubricating property and wear resistance, and is low in friction coefficient, large in notch sensitivity, low in impact resistance and large in molding shrinkage.
In the prior art, more than 80 percent of PBT products are modified products, and the advantages of performance enhancement, functional improvement and the like can be realized through material modification. In the prior art, glass fiber or other materials are mostly adopted to modify and reinforce PBT, and the PBT modified by the glass fiber has improved tensile strength, bending strength and thermal denaturation temperature, and when the PBT works at high temperature for a long time, the longitudinal shrinkage and the transverse shrinkage of the PBT product modified by the glass fiber are inconsistent and warping is easy to occur. Therefore, the invention provides a PBT modification process aiming at the problems of poor formability, unstable size, shrinkage and the like of the existing PBT modified product.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a modified PBT polymer with improved shrinkage performance and a preparation process thereof, wherein the internal crystal grain distribution stability of PBT resin is improved by using polypropylene copolymer, metallic lead, mineral substances and nano materials, so as to form a polymer with excellent mechanical properties, friction resistance and impact resistance, and the polymer has the characteristics of low shrinkage and enhanced thermal properties.
The technical content of the invention is as follows:
the invention provides a modified PBT polymer with improved shrinkage performance, which comprises the following raw materials: polybutylene terephthalate, polypropylene copolymer, metallic lead, glass fiber, nanocellulose, chalcopyrite, other ore substances, organic nano montmorillonite, nano zinc nitride, active silicon micro powder, a curing agent, an activating agent and a cross-linking agent;
in the preparation raw materials of the modified PBT polymer, 52-55 wt% of polybutylene terephthalate, 6-9 wt% of co-polypropylene, 0.03-0.05 wt% of metallic lead, 7-11 wt% of glass fiber, 7-11 wt% of nano-cellulose, 1-4 wt% of chalcopyrite, 3-6 wt% of other minerals, 4-8 wt% of organic nano-montmorillonite, 3-5 wt% of nano-zinc nitride, 3-6 wt% of active silicon micropowder, 1-2 wt% of curing agent, 1-2 wt% of activating agent and 1-2 wt% of cross-linking agent are used;
the particle diameter of the metal lead is 2-5 mu m;
the other ore substances comprise one or more of kaolin, mica powder, gypsum powder, calcium carbonate, aluminum hydroxide, quartz powder and marble powder, and the particle diameters of the chalcopyrite and the other ore substances are 10-15 mu m;
the curing agent comprises one or more than one of m-phenylenediamine, N-dimethylaminopropylamine and N, N-diethylaminopropylamine;
the activating agent comprises one or more than one of N-caproyl caprolactam, N-benzoyl caprolactam, ethylene diamine phosphate and propylene diamine phosphate;
the cross-linking agent comprises one or more of 1, 4-butanediol diacrylate, ethylene glycol dimethacrylate, divinyl benzene and diallyl maleate;
the invention also provides a preparation process of the modified PBT polymer with improved shrinkage performance, which comprises the following steps:
1) mixing polybutylene terephthalate, polypropylene copolymer, metallic lead, active silicon micro powder and an activator, smelting in vacuum, stirring at a constant speed, keeping the temperature to 215-235 ℃ at a heating rate of 50-70 ℃/min, stirring for 30-40 min, cooling to 220-245 ℃, stirring for 20-30 min, cooling at a constant speed, and performing injection molding to obtain a mixed melt A;
2) mixing the residual polybutylene terephthalate, glass fiber, nano-cellulose, chalcopyrite, organic nano-montmorillonite, nano-zinc nitride and a cross-linking agent, putting the mixture into vacuum for smelting, keeping the temperature to 250-280 ℃ at a heating rate of 50-70 ℃/min under uniform stirring, stirring for 30-40 min, then cooling at a uniform speed, and carrying out injection molding to obtain a mixed melt B;
3) mixing and melting the mixed melt A, the mixed melt B, other ore substances and a curing agent, uniformly stirring, and then extruding and molding through a double-screw extruder to obtain a modified PBT polymer;
the pressure of the vacuum in the step 1) and the step 2) is 10-1～10-4Pa, adopting vacuum can reduce the melting point of the material, reduce the cost and prevent the material from being oxidized;
after the temperature is reduced to 130-150 ℃ at a constant speed, carrying out injection molding and cutting into particles;
the temperature of the mixed melt in the step 3) is 175-200 ℃, and the stirring speed is 120-200 r/min;
the extrusion temperature of the double-screw extruder is 90-110 ℃, and the speed is 180-250 r/min;
the chalcopyrite and other ore materials are ground to a particle diameter of 10-15 mu m before use.
The invention has the following beneficial effects:
according to the modified PBT polymer, based on the existing technology of adopting glass fiber, the PBT is modified and enhanced by adopting the polypropylene copolymer, the metallic lead, the ore and the nano material, so that the rigidity, the impact resistance and the dimensional stability of the PBT are improved, the mechanical property and the chemical resistance of the PBT are comprehensively improved, the PBT injection molding resin with excellent thermal property and low shrinkage is obtained, the application field of the PBT is expanded, and the modified PBT polymer is suitable for application of household appliance parts such as electric heating equipment, a grill and the like;
the preparation process of the modified PBT polymer adopts the PBT to be respectively melted and modified with different materials to obtain different mixed melts, and finally fuses into a whole with the aim of improving chemical resistance, size stability and mechanical property, and utilizes the polypropylene copolymer, the metallic lead, the ore substance and the nano material to improve the stable distribution state of internal crystal grains of the PBT resin to form the polymer with excellent mechanical property, friction resistance and impact resistance, and the polymer has the characteristics of low shrinkage and enhanced thermal property, thereby comprehensively improving the performance of the modified PBT polymer.
Detailed Description
The present invention is described in further detail in the following detailed description with reference to specific embodiments, which are intended to be illustrative only and not to be limiting of the scope of the invention, as various equivalent modifications of the invention will become apparent to those skilled in the art after reading the present invention and are intended to be included within the scope of the appended claims.
All the raw materials and reagents of the invention are conventional market raw materials and reagents unless otherwise specified.
Example 1
Preparation of a modified PBT polymer with improved shrink properties:
1) mixing 32 wt% of polybutylene terephthalate, 8 wt% of polypropylene copolymer, 0.03 wt% of metallic lead, 3 wt% of active silicon micropowder and 1 wt% of activating agent, and placing the mixture in a container of 10 wt%-2Pa, smelting under vacuum, keeping the temperature to 225 ℃ at a heating rate of 60 ℃/min while stirring at a constant speed, stirring for 35min, cooling to 235 ℃, stirring for 20-30 min, cooling to 140 ℃ at a constant speed, performing injection molding, and cutting into particles to obtain a mixed melt A;
the particle diameter of the metal lead is 2-5 mu m;
the activating agent is a mixture of N-caproyl caprolactam and N-benzoyl caprolactam in a ratio of 1: 1;
2) mixing the rest 20 wt% of polybutylene terephthalate, 11 wt% of glass fiber, 5 wt% of nano-cellulose, 3.97 wt% of chalcopyrite, 4 wt% of organic nano-montmorillonite, 5 wt% of nano-zinc nitride and 1 wt% of cross-linking agent, and placing the mixture in a container of 10- 2Pa vacuum smelting, stirring at a constant speed, keeping the temperature to 265 ℃ at a heating rate of 60 ℃/min, stirring for 35min, then cooling at a constant speed to 140 ℃, performing injection molding, and cutting into particles to obtain a mixed melt B;
the cross-linking agent is diallyl maleate;
3) mixing and melting the mixed melt A, the mixed melt B, 4 wt% of other ore substances and 2 wt% of curing agent at 185 ℃, stirring at 155r/min, uniformly stirring, and extruding and molding by using a double-screw extruder at 100 ℃ and 210r/min to obtain a modified PBT polymer;
the other ore materials are mixed by 1:1:1 of mica powder, gypsum powder and marble powder, and are ground until the particle diameter is 10-15 mu m before use;
the curing agent is a mixture of m-phenylenediamine and N, N-dimethylaminopropylamine in a ratio of 1: 1.
Example 2
Preparation of a modified PBT polymer with improved shrink properties:
1) mixing 33 wt% of polybutylene terephthalate, 8 wt% of polypropylene copolymer, 0.05 wt% of metallic lead, 5 wt% of active silicon micropowder and 2 wt% of activating agent, and placing the mixture in a container of 10 wt%-4Pa vacuum smelting, stirring at a constant speed, keeping the temperature to 215 ℃ at a heating rate of 50 ℃/min, stirring for 40min, cooling to 220 ℃ and stirring for 30min, then cooling to 130 ℃ at a constant speed, injection molding, and cutting into particles to obtain a mixed melt A;
the particle diameter of the metal lead is 2-5 mu m;
the activating agent is a mixture of N-caproyl caprolactam and phosphoric acid propane diamine in a ratio of 1: 1;
2) mixing the rest 20 wt% of polybutylene terephthalate, 9 wt% of glass fiber, 6 wt% of nano-cellulose, 2.95 wt% of chalcopyrite, 5 wt% of organic nano-montmorillonite, 3 wt% of nano-zinc nitride and 2 wt% of cross-linking agent, and placing the mixture in a container of 10- 4Pa, smelting under vacuum, keeping the temperature to 250 ℃ at a heating rate of 50 ℃/min while stirring at a constant speed, stirring for 40min, then cooling to 130 ℃ at a constant speed, carrying out injection molding, and cutting into particles to obtain a mixed melt B;
the cross-linking agent is 1, 4-butanediol diacrylate;
3) mixing and melting the mixed melt A, the mixed melt B, 3 wt% of other ore substances and 1 wt% of curing agent at 175 ℃, stirring at 120r/min, uniformly stirring, and extruding and molding by using a double-screw extruder at 90 ℃ and 250r/min to obtain a modified PBT polymer;
the other ore substances are kaolin, gypsum powder and quartz powder which are mixed in a ratio of 1:1:1, and are ground until the particle diameter is 10-15 mu m before use;
the curing agent is m-phenylenediamine.
Example 3
Preparation of a modified PBT polymer with improved shrink properties:
1) 31 wt% of polybutylene terephthalate, 7 wt% of polypropylene copolymer, 0.03 wt% of metallic lead, 4 wt% of active silicon micropowder and 1 wt% of activating agent are mixed and placed at 10-1Pa vacuum smelting, stirring at a constant speed, keeping the temperature to 235 ℃ at a heating rate of 70 ℃/min, stirring for 30min, cooling to 245 ℃ and stirring for 20min, then cooling to 150 ℃ at a constant speed, injection molding, and cutting into particles to obtain a mixed melt A;
the particle diameter of the metal lead is 2-5 mu m;
the activating agent is N-benzoyl caprolactam;
2) mixing the rest 22 wt% of polybutylene terephthalate, 10 wt% of glass fiber, 4 wt% of nano-cellulose, 1.97 wt% of chalcopyrite, 6 wt% of organic nano-montmorillonite, 4 wt% of nano-zinc nitride and 2 wt% of cross-linking agent, and placing the mixture in a container of 10 wt%- 1Pa vacuum smelting, stirring at a constant speed, keeping the temperature to 280 ℃ at a heating rate of 70 ℃/min, stirring for 30min, then cooling at a constant speed to 150 ℃, performing injection molding, and cutting into particles to obtain a mixed melt B;
the cross-linking agent is a mixture of divinylbenzene and diallyl maleate in a ratio of 1: 1;
3) mixing and melting the mixed melt A, the mixed melt B, 6 wt% of other ore substances and 1 wt% of curing agent at the temperature of 200 ℃, stirring at the speed of 200r/min, uniformly stirring, and then extruding and molding by using a double-screw extruder at the extrusion temperature of 110 ℃ and the speed of 180r/min to obtain a modified PBT polymer;
the other ore materials are kaolin and calcium carbonate which are mixed in a ratio of 1:1, and are ground until the particle diameter is 10-15 mu m before use;
the curing agent is N, N-diethylaminopropylamine.
Example 4
Preparation of a modified PBT polymer with improved shrink properties:
1) mixing 33 wt% of polybutylene terephthalate, 6 wt% of polypropylene copolymer, 0.04 wt% of metallic lead, 6 wt% of active silicon micropowder and 2 wt% of activating agent, placing the mixture in a container of 10 wt%-3Pa vacuum smelting, stirring at a constant speed, keeping the temperature to 220 ℃ at a heating rate of 56 ℃/min, stirring for 36min, cooling to 232 ℃ and stirring for 28min, then cooling to 144 ℃ at a constant speed, injection molding, and cutting into particles to obtain a mixed melt A;
the particle diameter of the metal lead is 2-5 mu m;
the activating agent is a mixture of N-benzoyl caprolactam and ethylene diamine phosphate in a ratio of 1: 1;
2) mixing the rest 22 wt% of polybutylene terephthalate, 7 wt% of glass fiber, 4 wt% of nano-cellulose, 2.96 wt% of chalcopyrite, 8 wt% of organic nano-montmorillonite, 3 wt% of nano-zinc nitride and 1 wt% of cross-linking agent, and placing the mixture in a container 10- 3Smelting under Pa vacuum, stirring at a constant speed, keeping the temperature to 260 ℃ at a heating rate of 58 ℃/min, stirring for 38min, then cooling at a constant speed to 139 ℃, performing injection molding, and cutting into particles to obtain a mixed melt B;
the cross-linking agent is a mixture of ethylene glycol dimethacrylate and divinylbenzene 1: 1;
3) mixing and melting the mixed melt A, the mixed melt B, 3 wt% of other ore substances and 2 wt% of curing agent at 190 ℃, stirring at 180r/min, uniformly stirring, and extruding and molding by using a double-screw extruder at 100 ℃ and 230r/min to obtain a modified PBT polymer;
the other ore materials are kaolin and marble powder which are mixed in a ratio of 1:1, and are ground until the particle diameter is 10-15 mu m before use;
the curing agent is a mixture of N, N-dimethylaminopropylamine and N, N-diethylaminopropylamine in a ratio of 1: 1.
Comparative example 1
The control of example 1, the modified polymer of comparative example 1, was prepared without using metallic lead, and the other conditions were unchanged.
Comparative example 2
The control of example 1, the modified polymer of comparative example 2 was prepared without chalcopyrite and other mineral constituents, and other conditions were unchanged.
The examples of the invention and the comparative modified PBT polymer are subjected to related performance detection, and the detection method and the result are shown as follows.
TABLE 1 physical Properties and impact Properties measurements
TABLE 2 thermal Performance testing
TABLE 3 mechanical Strength test
As can be seen from the data, the modified PBT polymer obtained by the invention still retains more excellent mechanical properties after being modified, and simultaneously has improved and enhanced impact resistance, shrinkage and thermal properties, compared with the comparative example 1 and the comparative example 2, the metallic lead and the ore lamp component adopted by the modified polymer prepared by the invention have promotion effects on the mechanical properties, the thermal properties, the impact resistance and the physical properties of the modified PBT. The modified PBT polymer has the characteristics of low shrinkage and enhanced thermal property, the performance of the modified PBT polymer is comprehensively improved, the application field of the PBT is expanded, and the modified PBT polymer is suitable for application of household electrical appliance parts such as electric heating equipment, oven grills and the like.
Claims (10)
1. A modified PBT polymer with improved shrinkage performance is characterized in that the modified PBT polymer is prepared from the following raw materials: polybutylene terephthalate, polypropylene copolymer, metallic lead, glass fiber, nano-cellulose, chalcopyrite, other mineral substances, organic nano-montmorillonite, nano-zinc nitride, active silicon micro-powder, a curing agent, an activating agent and a cross-linking agent.
2. The modified PBT polymer of claim 1, wherein the modified PBT polymer comprises, as raw materials, 52 to 55 wt% of polybutylene terephthalate, 6 to 9 wt% of co-polypropylene, 0.03 to 0.05 wt% of metallic lead, 7 to 11 wt% of glass fiber, 7 to 11 wt% of nanocellulose, 1 to 4 wt% of chalcopyrite, 3 to 6 wt% of other minerals, 4 to 8 wt% of organic nano-montmorillonite, 3 to 5 wt% of nano-zinc nitride, 3 to 6 wt% of active silica micropowder, 1 to 2 wt% of curing agent, 1 to 2 wt% of activating agent, and 1 to 2 wt% of crosslinking agent.
3. The modified PBT polymer of claim 1 or 2, wherein the metallic lead has a particle diameter of 2 to 5 μm.
4. The modified PBT polymer of claim 1 or 2, wherein the activator comprises one or more of N-hexanoylcaprolactam, N-benzoylcaprolactam, ethylenediamine phosphate, and propylenediamine phosphate.
5. The modified PBT polymer of claim 1 or 2, wherein the crosslinking agent comprises one or more of 1, 4-butanediol diacrylate, ethylene glycol dimethacrylate, divinylbenzene, and diallyl maleate.
6. A preparation process of a modified PBT polymer with improved shrinkage performance is characterized by comprising the following steps:
1) mixing polybutylene terephthalate, polypropylene copolymer, metallic lead, active silicon micro powder and an activator, smelting in vacuum, stirring at a constant speed, keeping the temperature to 215-235 ℃ at a heating rate of 50-70 ℃/min, stirring for 30-40 min, cooling to 220-245 ℃, stirring for 20-30 min, cooling at a constant speed, and performing injection molding to obtain a mixed melt A;
2) mixing the residual polybutylene terephthalate, glass fiber, nano-cellulose, chalcopyrite, organic nano-montmorillonite, nano-zinc nitride and a cross-linking agent, putting the mixture into vacuum for smelting, keeping the temperature to 225-250 ℃ at a heating rate of 50-70 ℃/min under uniform stirring, stirring for 30-40 min, then cooling at a uniform speed, and performing injection molding to obtain a mixed melt B;
3) and mixing and melting the mixed melt A, the mixed melt B, other ore substances and a curing agent, uniformly stirring, and then extruding and molding through a double-screw extruder to obtain the modified PBT polymer.
7. The process for preparing the modified PBT polymer according to claim 6, wherein the vacuum in the step 1) or 2) has a pressure of 10-1～10-4Pa。
8. The preparation process of the modified PBT polymer of claim 6, wherein the temperature is reduced to 130-150 ℃ at a constant speed in step 1) and step 2), and then the mixture is subjected to injection molding and is cut into particles.
9. The process for preparing the modified PBT polymer of claim 6, wherein the other minerals comprise one or more of kaolin, mica powder, gypsum powder, calcium carbonate, aluminum hydroxide, quartz powder and marble powder;
the chalcopyrite and other ore materials are ground to a particle diameter of 10-15 mu m before use.
10. The process for preparing the modified PBT polymer according to claim 6, wherein the temperature of the mixing and melting in the step 3) is 175-200 ℃, and the stirring speed is 120-200 r/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114479389A (en) * | 2022-03-28 | 2022-05-13 | 金发科技股份有限公司 | Nanofiber modified PBT (polybutylene terephthalate) composite material as well as preparation method and application thereof |
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| CN103254587A (en) * | 2013-05-10 | 2013-08-21 | 常熟市协新冶金材料有限公司 | Toughened polybutylene terephthalate alloy composite material |
| CN104177787A (en) * | 2013-05-24 | 2014-12-03 | 上海杰事杰新材料(集团)股份有限公司 | Low shrinkage and high strength modified PET (polyethylene terephthalate) material and preparation method thereof |
| CN105001661A (en) * | 2006-02-09 | 2015-10-28 | 瓦尔德瑞沃咨询集团公司 | Metal polymer composite material with enhanced viscoelasticity and thermal performance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105001661A (en) * | 2006-02-09 | 2015-10-28 | 瓦尔德瑞沃咨询集团公司 | Metal polymer composite material with enhanced viscoelasticity and thermal performance |
| CN103254587A (en) * | 2013-05-10 | 2013-08-21 | 常熟市协新冶金材料有限公司 | Toughened polybutylene terephthalate alloy composite material |
| CN104177787A (en) * | 2013-05-24 | 2014-12-03 | 上海杰事杰新材料(集团)股份有限公司 | Low shrinkage and high strength modified PET (polyethylene terephthalate) material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114479389A (en) * | 2022-03-28 | 2022-05-13 | 金发科技股份有限公司 | Nanofiber modified PBT (polybutylene terephthalate) composite material as well as preparation method and application thereof |
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