CN109796739B - Elastomer polyester material and preparation method thereof - Google Patents
Elastomer polyester material and preparation method thereof Download PDFInfo
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- CN109796739B CN109796739B CN201811616358.1A CN201811616358A CN109796739B CN 109796739 B CN109796739 B CN 109796739B CN 201811616358 A CN201811616358 A CN 201811616358A CN 109796739 B CN109796739 B CN 109796739B
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Abstract
The invention discloses an elastomer polyester material, which is prepared from the following raw materials in parts by weight: 0.1-0.2 part of triethylamine, 40-50 parts of rubber powder dispersion liquid, 200 parts of polycarbonate 170-one-wall resin, 20-30 parts of lignin, 10-16 parts of montmorillonite powder, 4-7 parts of epoxy octyl stearate, 5-7 parts of phosphorous acid, 4-6 parts of ethylene glycol, 2-3 parts of bisphenol A and 0.01-0.02 part of p-toluenesulfonic acid.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to an elastomer polyester material and a preparation method thereof.
Background
Polycarbonate is a thermoplastic engineering plastic with excellent comprehensive performance developed in the early 60 s of the 20 th century, and has the advantages of outstanding impact toughness, transparency, dimensional stability, excellent mechanical strength, electric insulation, wide range of use temperature, and good creep resistance, weather resistance and self-extinguishing property. However, the polycarbonate is also sensitive to gaps, easy to generate stress cracking, high in melt viscosity and poor in fluidity, and therefore, the polycarbonate needs to be modified, such as development of new polycarbonate products, reinforcement modification, toughening modification and the like. At present, polycarbonate is widely used in the fields of electronics, electrical appliances, automobiles, optical materials and the like, and because of good dimensional stability and good toughness, polycarbonate is very common as an outer sheath material, however, polycarbonate has poor resilience and is sensitive to notches, and when bending and other processing are realized, breakage and the like are easy to occur, so how to further improve the elasticity of polycarbonate is the focus of current research.
Disclosure of Invention
The invention aims to provide an elastomer polyester material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
an elastomer polyester material is composed of the following raw materials in parts by weight:
0.1-0.2 part of triethylamine, 40-50 parts of rubber powder dispersion liquid, 200 parts of polycarbonate 170-containing material, 20-30 parts of lignin, 10-16 parts of montmorillonite powder, 4-7 parts of epoxy octyl stearate, 5-7 parts of phosphorous acid, 4-6 parts of ethylene glycol, 2-3 parts of bisphenol A and 0.01-0.02 part of p-toluenesulfonic acid.
The rubber powder dispersion liquid is prepared from the following raw materials in parts by weight:
50-70 parts of silicone rubber powder, 24-30 parts of thionyl chloride, 4-6 parts of stearic acid, 0.8-1 part of tert-butyl p-diphenol, 30-40 parts of methyl methacrylate and 0.8-1 part of initiator.
The initiator is dicumyl peroxide.
The preparation method of the rubber powder dispersion comprises the following steps:
(1) adding an initiator into isopropanol of which the weight is 10-14 times that of the initiator, and uniformly stirring to obtain an initiator solution;
(2) mixing tert-butyl p-diphenol and silicon rubber powder, stirring for 10-20 minutes, adding the mixture into isopropanol with the weight 5-7 times of that of the mixture, uniformly stirring, adding methyl methacrylate, feeding the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-65 ℃, adding the initiator solution, keeping the temperature and stirring for 3-5 hours, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain polyester modified rubber powder;
(3) mixing stearic acid with the polyester modified rubber powder, preserving heat for 3-4 minutes at the temperature of 110-120 ℃, cooling to normal temperature, adding into thionyl chloride, sending into a thermostatic water bath at the temperature of 60-65 ℃, preserving heat and stirring for 15-20 hours to obtain the rubber powder dispersion.
A method of preparing an elastomeric polyester material comprising the steps of:
(1) adding bisphenol A into thionyl chloride with the weight 10-20 times of that of the bisphenol A, and uniformly stirring to obtain bisphenol A dispersion liquid;
(2) mixing phosphorous acid and montmorillonite powder, stirring for 1-2 hours at the temperature of 120-140 ℃, mixing with ethylene glycol, stirring uniformly, feeding into a reaction kettle, adding p-toluenesulfonic acid, stirring for 2-3 hours at the temperature of 90-95 ℃, discharging and cooling to obtain pretreated soil powder;
(3) adding the pretreated soil powder into the bisphenol A dispersion liquid, and stirring for 70-80 minutes at the temperature of 50-55 ℃ to obtain a soil powder dispersion liquid;
(4) mixing the soil powder dispersion liquid with the rubber powder dispersion liquid, uniformly stirring, adding lignin, uniformly stirring, sending into an ice water bath, adding triethylamine, stirring for reacting for 6-7 hours, and distilling to remove thionyl chloride to obtain montmorillonite modified rubber powder;
(5) and (3) uniformly stirring the montmorillonite modified rubber powder, polycarbonate and epoxy octyl stearate, feeding the mixture into an extruder, performing melt extrusion, and cooling to obtain the elastomer polyester material.
The invention has the advantages that:
according to the invention, silicon rubber powder is used as an elastomer, bisphenol is treated by tert-butyl to carry out diphenol treatment and then is blended with methyl acrylate monomer, polymerization is carried out under the action of an initiator to obtain polyester modified rubber powder, then thionyl chloride solution of stearic acid is adopted for carrying out acyl chlorination modification, montmorillonite powder participates in esterification reaction of phosphorous acid and ethylene glycol, bisphenol A modification is adopted, the heat resistance is effectively improved through bisphenol a ester modification, and then lignin modified rubber powder is obtained through the blending reaction of phenolic hydroxyl and acyl chloride in lignin.
Detailed Description
Example 1
An elastomer polyester material is composed of the following raw materials in parts by weight:
triethylamine 0.2, rubber powder dispersion liquid 50, polycarbonate 200, lignin 30, montmorillonite powder 16, epoxy octyl stearate 7, phosphorous acid 7, ethylene glycol 6, bisphenol A3 and p-toluenesulfonic acid 0.02.
The rubber powder dispersion liquid is prepared from the following raw materials in parts by weight:
70 parts of silicone rubber powder, 30 parts of thionyl chloride, 6 parts of stearic acid, 1 part of tert-butyl-p-diphenol, 40 parts of methyl methacrylate and 1 part of initiator.
The initiator is dicumyl peroxide.
The preparation method of the rubber powder dispersion comprises the following steps:
(1) adding an initiator into isopropanol with the weight 14 times that of the initiator, and uniformly stirring to obtain an initiator solution;
(2) mixing tert-butyl p-diphenol and silicon rubber powder, stirring for 20 minutes, adding the mixture into isopropanol with the weight being 7 times that of the mixture, uniformly stirring, adding methyl methacrylate, feeding the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65 ℃, adding the initiator solution, keeping the temperature, stirring for 5 hours, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain polyester modified rubber powder;
(3) mixing stearic acid with the polyester modified rubber powder, keeping the temperature at 120 ℃ for 4 minutes, cooling to normal temperature, adding the mixture into thionyl chloride, sending the mixture into a thermostatic water bath at 65 ℃, and keeping the temperature and stirring for 15 to 20 hours to obtain the rubber powder dispersion.
A method of preparing an elastomeric polyester material comprising the steps of:
(1) adding bisphenol A into thionyl chloride with the weight 20 times that of the bisphenol A, and uniformly stirring to obtain bisphenol A dispersion liquid;
(2) mixing phosphorous acid and montmorillonite powder, stirring for 2 hours at 140 ℃, mixing with ethylene glycol, stirring uniformly, feeding into a reaction kettle, adding p-toluenesulfonic acid, stirring for 3 hours at 95 ℃, discharging and cooling to obtain pretreated soil powder;
(3) adding the pretreated soil powder into the bisphenol A dispersion liquid, and stirring for 80 minutes at 55 ℃ to obtain a soil powder dispersion liquid;
(4) mixing the soil powder dispersion liquid with the rubber powder dispersion liquid, uniformly stirring, adding lignin, uniformly stirring, feeding into an ice water bath, adding triethylamine, stirring for reaction for 7 hours, and distilling to remove thionyl chloride to obtain montmorillonite modified rubber powder;
(5) and (3) uniformly stirring the montmorillonite modified rubber powder, polycarbonate and epoxy octyl stearate, feeding the mixture into an extruder, performing melt extrusion, and cooling to obtain the elastomer polyester material.
Example 2
An elastomer polyester material is composed of the following raw materials in parts by weight:
triethylamine 0.1, rubber powder dispersion liquid 40, polycarbonate 170, lignin 20, montmorillonite powder 10, epoxy octyl stearate 4, phosphorous acid 5, ethylene glycol 4, bisphenol A2 and p-toluenesulfonic acid 0.01.
The rubber powder dispersion liquid is prepared from the following raw materials in parts by weight:
50 parts of silicone rubber powder, 24 parts of thionyl chloride, 4 parts of stearic acid, 0.8 part of tert-butyl p-diphenol, 30 parts of methyl methacrylate and 0.8 part of initiator.
The initiator is dicumyl peroxide.
The preparation method of the rubber powder dispersion comprises the following steps:
(1) adding an initiator into isopropanol with the weight being 10 times of that of the initiator, and uniformly stirring to obtain an initiator solution;
(2) mixing tert-butyl p-diphenol and silicon rubber powder, stirring for 10 minutes, adding the mixture into isopropanol with the weight 5 times that of the mixture, uniformly stirring, adding methyl methacrylate, feeding the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60 ℃, adding the initiator solution, keeping the temperature and stirring for 3 hours, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain polyester modified rubber powder;
(3) mixing stearic acid with the polyester modified rubber powder, keeping the temperature at 110 ℃ for 3 minutes, cooling to normal temperature, adding the mixture into thionyl chloride, sending the mixture into a thermostatic water bath at 60 ℃, and keeping the temperature and stirring for 15 hours to obtain the rubber powder dispersion.
A method of preparing an elastomeric polyester material comprising the steps of:
(1) adding bisphenol A into thionyl chloride with the weight 10 times that of the bisphenol A, and uniformly stirring to obtain bisphenol A dispersion liquid;
(2) mixing phosphorous acid and montmorillonite powder, stirring for 1 hour at 120 ℃, mixing with ethylene glycol, stirring uniformly, feeding into a reaction kettle, adding p-toluenesulfonic acid, stirring for 2 hours at 90 ℃, discharging and cooling to obtain pretreated soil powder;
(3) adding the pretreated soil powder into the bisphenol A dispersion liquid, and stirring for 70 minutes at the temperature of 50 ℃ to obtain a soil powder dispersion liquid;
(4) mixing the soil powder dispersion liquid with the rubber powder dispersion liquid, uniformly stirring, adding lignin, uniformly stirring, sending into an ice water bath, adding triethylamine, stirring for reacting for 6 hours, and distilling to remove thionyl chloride to obtain montmorillonite modified rubber powder;
(5) and (3) uniformly stirring the montmorillonite modified rubber powder, polycarbonate and epoxy octyl stearate, feeding the mixture into an extruder, performing melt extrusion, and cooling to obtain the elastomer polyester material.
And (3) performance testing:
elastomeric polyester material of example 1:
tensile strength testing was performed according to ASTM D638/ISO 527:
the result was 94 MPa;
elongation at break test:
the result was 148%; tensile modulus testing was performed:
the result was 2481 MPa;
flexural strength testing was performed according to ASTM D790/ISO 178:
the result was 125 MPa.
Elastomeric polyester material of example 2:
tensile strength testing was performed according to ASTM D638/ISO 527:
the result was 101 MPa;
elongation at break test:
the result was 153%; tensile modulus testing was performed:
the result was 2489 MPa;
flexural strength testing was performed according to ASTM D790/ISO 178:
as a result, 127MPa was obtained.
Claims (2)
1. An elastomer polyester material is characterized by being prepared from the following raw materials in parts by weight:
0.1-0.2 part of triethylamine, 40-50 parts of rubber powder dispersion liquid, 200 parts of polycarbonate 170-ion resin, 20-30 parts of lignin, 10-16 parts of montmorillonite powder, 4-7 parts of epoxy octyl stearate, 5-7 parts of phosphorous acid, 4-6 parts of ethylene glycol, 2-3 parts of bisphenol A and 0.01-0.02 part of p-toluenesulfonic acid;
the rubber powder dispersion is prepared from the following raw materials in parts by weight: 50-70 parts of silicone rubber powder, 24-30 parts of thionyl chloride, 4-6 parts of stearic acid, 0.8-1 part of tert-butyl p-diphenol, 30-40 parts of methyl methacrylate and 0.8-1 part of initiator;
the preparation method of the rubber powder dispersion comprises the following steps:
(1) adding an initiator into isopropanol of which the weight is 10-14 times that of the initiator, and uniformly stirring to obtain an initiator solution;
(2) mixing tert-butyl p-diphenol and silicon rubber powder, stirring for 10-20 minutes, adding the mixture into isopropanol with the weight 5-7 times of that of the mixture, uniformly stirring, adding methyl methacrylate, feeding the mixture into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-65 ℃, adding the initiator solution, keeping the temperature and stirring for 3-5 hours, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain polyester modified rubber powder;
(3) mixing stearic acid with the polyester modified rubber powder, preserving heat for 3-4 minutes at the temperature of 110-120 ℃, cooling to normal temperature, adding into thionyl chloride, sending into a constant-temperature water bath at the temperature of 60-65 ℃, preserving heat and stirring for 15-20 hours to obtain the rubber powder dispersion;
the preparation method of the elastomer polyester material comprises the following steps:
(1) adding bisphenol A into thionyl chloride with the weight 10-20 times of that of the bisphenol A, and uniformly stirring to obtain bisphenol A dispersion liquid;
(2) mixing phosphorous acid and montmorillonite powder, stirring for 1-2 hours at the temperature of 120-140 ℃, mixing with ethylene glycol, stirring uniformly, feeding into a reaction kettle, adding p-toluenesulfonic acid, stirring for 2-3 hours at the temperature of 90-95 ℃, discharging and cooling to obtain pretreated soil powder;
(3) adding the pretreated soil powder into the bisphenol A dispersion liquid, and stirring for 70-80 minutes at the temperature of 50-55 ℃ to obtain a soil powder dispersion liquid;
(4) mixing the soil powder dispersion liquid with the rubber powder dispersion liquid, uniformly stirring, adding lignin, uniformly stirring, sending into an ice water bath, adding triethylamine, stirring for reacting for 6-7 hours, and distilling to remove thionyl chloride to obtain montmorillonite modified rubber powder;
(5) and (3) uniformly stirring the montmorillonite modified rubber powder, polycarbonate and epoxy octyl stearate, feeding the mixture into an extruder, performing melt extrusion, and cooling to obtain the elastomer polyester material.
2. An elastomeric polyester material according to claim 1, wherein said initiator is dicumyl peroxide.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101130624A (en) * | 2006-08-22 | 2008-02-27 | 东丽纤维研究所（中国）有限公司 | Method for producing poly-p-benzene dicarboxylic acid trimethylene glycol ester phyllosilicate nano material |
| CN106633692A (en) * | 2016-12-05 | 2017-05-10 | 芜湖天鸿汽车零部件有限公司 | Mold material for injection molding of automobile bumper and preparation method of mold material |
| CN108976787A (en) * | 2018-08-06 | 2018-12-11 | 合肥滴答科技有限公司 | A kind of carbon nanotube fire proofing material and preparation method thereof |
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| ES2667328T3 (en) * | 2012-12-07 | 2018-05-10 | Covestro Deutschland Ag | Flame retardant polycarbonate molding compositions VI |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101130624A (en) * | 2006-08-22 | 2008-02-27 | 东丽纤维研究所（中国）有限公司 | Method for producing poly-p-benzene dicarboxylic acid trimethylene glycol ester phyllosilicate nano material |
| CN106633692A (en) * | 2016-12-05 | 2017-05-10 | 芜湖天鸿汽车零部件有限公司 | Mold material for injection molding of automobile bumper and preparation method of mold material |
| CN108976787A (en) * | 2018-08-06 | 2018-12-11 | 合肥滴答科技有限公司 | A kind of carbon nanotube fire proofing material and preparation method thereof |
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Effective date of registration: 20210831 Address after: 315800 first floor, South Building 1, building 1, No. 86, cishanhe Road, Chunxiao, Beilun District, Ningbo City, Zhejiang Province Patentee after: Ningbo Xingli New Material Co.,Ltd. Address before: 325802 No.315, fangbei village, Longgang Town, Cangnan County, Wenzhou City, Zhejiang Province Patentee before: Fang Wanpiao |