CN108530859B - Preparation method of particle reinforced rubber reinforced composite material - Google Patents
Preparation method of particle reinforced rubber reinforced composite material Download PDFInfo
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- CN108530859B CN108530859B CN201810152826.8A CN201810152826A CN108530859B CN 108530859 B CN108530859 B CN 108530859B CN 201810152826 A CN201810152826 A CN 201810152826A CN 108530859 B CN108530859 B CN 108530859B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention provides a preparation method of a particle reinforced rubber reinforced composite material, which comprises the following steps: preparing particle reinforced rubber: mixing methyl phenyl vinyl silicone rubber, a vulcanizing agent, silicon carbide powder, silicon dioxide powder and low-melting-point glass powder to obtain a first mixture; vulcanizing the first mixture to obtain a first vulcanized product; putting the first vulcanized product into an oven for drying to obtain a first dried product; calcining the first dried product at high temperature to obtain particle reinforced rubber; preparing reinforced particles: providing niobium powder and aluminum nitride powder, and carrying out ball milling on the niobium powder and the aluminum nitride powder to obtain a second mixture; sintering the second mixture to obtain a reinforced particle block; crushing the reinforced particle block to obtain reinforced particles; crushing the particle-reinforced rubber to obtain particle-reinforced rubber granules; putting polycarbonate, PET, particle reinforced rubber granules, reinforced particles and a processing aid into a double-screw extruder, and extruding the particle reinforced rubber composite material.
Description
Technical Field
The invention relates to the field of polymer matrix composite materials, in particular to a preparation method of a particle reinforced rubber reinforced composite material.
Background
The polymer materials with wide application range mainly comprise four general plastics and five engineering plastics, wherein the four general plastics comprise PC and PET resin. The PC resin has high impact strength, but is sensitive to gaps, easy to generate stress cracking, poor in flowability during processing, poor in chemical resistance and the like, and the application of the PC resin is limited to a certain extent; the PET resin also has very good performances, such as good fluidity, good chemical resistance and the like, and is widely applied to the fields of electronic appliances, automobiles and the like, but the PET resin has low notch impact strength and insufficient toughness. Therefore, the blend of PC and PET is prepared by blending modification, so that the blend has the advantages of PC and PET resin, the defects of PC and PET when used alone can be overcome, the PC/PET blend material with excellent performance can be obtained, and the application field of the PC and PET resin is widened.
The prior art already has a method for preparing PC/PET blending material, but the common PC/PET blending material has at least the following defects: 1. although the PC/PET blending material has the advantages of both PC and PET materials, the conventional PC/PET blending material cannot meet the actual requirement with the continuous improvement of the performance requirement of the industry on the high polymer material; 2. there have been some prior arts which propose the idea of adding reinforcing particles to a blend system to improve the strength of a material, but since there are almost infinite kinds of reinforcing particles, there has been no suggestion in the prior arts which specific reinforcing particles are effective; 3. the prior art also lacks an efficient manufacturing process without the ability to identify reinforcing particles.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a particle reinforced rubber reinforced composite material, thereby overcoming the defects of the prior art.
The invention provides a preparation method of a particle reinforced rubber reinforced composite material, which is characterized by comprising the following steps: the method comprises the following steps: preparing particle reinforced rubber: putting methyl phenyl vinyl silicone rubber, a vulcanizing agent, silicon carbide powder, silicon dioxide powder and low-melting-point glass powder into an open mill for mixing to obtain a first mixture; vulcanizing the first mixture to obtain a first vulcanized product, wherein the vulcanization temperature is 150 ℃ and 160 ℃, and the vulcanization time is 10-20 min; drying the first vulcanized product in an oven at the drying temperature of 200 ℃ and the drying time of 210 ℃ for 5-6h to obtain a first dried product; calcining the first dried product at high temperature to obtain particle reinforced rubber; preparing reinforced particles: providing niobium powder and aluminum nitride powder, and carrying out ball milling on the niobium powder and the aluminum nitride powder to obtain a second mixture; sintering the second mixture by using a spark plasma sintering method to obtain a reinforced particle block; crushing the reinforced particle block to obtain reinforced particles; crushing the particle-reinforced rubber to obtain particle-reinforced rubber granules; putting polycarbonate, PET, particle reinforced rubber granules, reinforced particles and a processing aid into a double-screw extruder, and extruding the particle reinforced rubber reinforced composite material by using the double-screw extruder.
Preferably, in the above technical scheme, the high-temperature calcination process is as follows: the calcination temperature is 800-1000 ℃, and the calcination time is 1-2 h.
Preferably, in the above technical scheme, the volume ratio of the niobium powder to the aluminum nitride powder is 1: 1-1: 2.
preferably, in the above technical scheme, the ball milling process is: the rotating speed of the ball mill is 500-.
Preferably, in the above technical solution, the process of sintering the second mixture by using the spark plasma sintering method specifically includes: the sintering temperature is 1800-1900 ℃, the sintering pressure is 50-100MPa, and the sintering time is 10-30 min.
Preferably, in the technical scheme, by weight, the polycarbonate accounts for 100 parts, the PET accounts for 80-120 parts, the particle reinforced rubber granules accounts for 20-30 parts, and the reinforcing particles account for 5-10 parts.
Preferably, in the above technical solution, the processing temperature of the twin-screw extruder is: the first zone temperature is 220-230 ℃, the second zone temperature is 230-240 ℃, the third zone temperature is 240-250 ℃, the fourth zone temperature is 250-260 ℃ and the die head temperature is 240-250 ℃.
Preferably, in the technical scheme, the screw rotating speed of the double-screw extruder is 50-70 r/min.
The invention also provides a particle reinforced rubber reinforced composite material, which is prepared by the method.
Compared with the prior art, the invention has the following beneficial effects: 1. according to the invention, the reinforced rubber and the reinforced particles are added into the PC/PET blending system, so that the comprehensive mechanical property of the PC/PET blending system is improved; 2. the reinforced particles which can actually improve the mechanical property of the PC/PET blending system are provided, and the defects of the prior art are made up; 3. aiming at a new reinforced particle type, a new manufacturing process is provided, and the high-performance particle reinforced rubber reinforced composite material is successfully prepared.
Detailed Description
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component. The chemical agents of the present invention may be purchased from chemical stores or from a network. The relevant experimental equipment is well known in the art.
Example 1
A particle reinforced rubber reinforced composite is prepared by the following method: preparing particle reinforced rubber: putting methyl phenyl vinyl silicone rubber, a vulcanizing agent, silicon carbide powder, silicon dioxide powder and low-melting-point glass powder into an open mill for mixing to obtain a first mixture; vulcanizing the first mixture to obtain a first vulcanized product, wherein the vulcanization temperature is 150 ℃, and the vulcanization time is 20 min; putting the first vulcanized product into an oven for drying at the drying temperature of 200 ℃ for 6 hours to obtain a first dried product; calcining the first dried product at high temperature to obtain particle reinforced rubber; preparing reinforced particles: providing niobium powder and aluminum nitride powder, and carrying out ball milling on the niobium powder and the aluminum nitride powder to obtain a second mixture; sintering the second mixture by using a spark plasma sintering method to obtain a reinforced particle block; crushing the reinforced particle block to obtain reinforced particles; crushing the particle-reinforced rubber to obtain particle-reinforced rubber granules; putting polycarbonate, PET, particle reinforced rubber granules, reinforced particles and a processing aid into a double-screw extruder, and extruding the particle reinforced rubber reinforced composite material by using the double-screw extruder. The high-temperature calcination process comprises the following steps: the calcining temperature is 800 ℃, and the calcining time is 2 h. The volume ratio of niobium powder to aluminum nitride powder is 1: 1. the ball milling process comprises the following steps: the rotating speed of the ball mill is 500r/min, and the ball milling time is 4 h. The process for sintering the second mixture by spark plasma sintering comprises: the sintering temperature is 1800 ℃, the sintering pressure is 100MPa, and the sintering time is 30 min. The polycarbonate accounts for 100 parts, the PET accounts for 80 parts, the particle reinforced rubber granules accounts for 20 parts, and the reinforcing particles account for 5 parts by weight. The processing temperature of the double-screw extruder is as follows: the first zone temperature was 220 deg.C, the second zone temperature was 230 deg.C, the third zone temperature was 240 deg.C, the fourth zone temperature was 250 deg.C, and the die temperature was 240 deg.C. The screw speed of the twin-screw extruder was 70 r/min.
Example 2
A particle reinforced rubber reinforced composite is prepared by the following method: preparing particle reinforced rubber: putting methyl phenyl vinyl silicone rubber, a vulcanizing agent, silicon carbide powder, silicon dioxide powder and low-melting-point glass powder into an open mill for mixing to obtain a first mixture; vulcanizing the first mixture to obtain a first vulcanized product, wherein the vulcanization temperature is 160 ℃, and the vulcanization time is 10 min; putting the first vulcanized product into an oven for drying at the drying temperature of 210 ℃ for 5 hours to obtain a first dried product; calcining the first dried product at high temperature to obtain particle reinforced rubber; preparing reinforced particles: providing niobium powder and aluminum nitride powder, and carrying out ball milling on the niobium powder and the aluminum nitride powder to obtain a second mixture; sintering the second mixture by using a spark plasma sintering method to obtain a reinforced particle block; crushing the reinforced particle block to obtain reinforced particles; crushing the particle-reinforced rubber to obtain particle-reinforced rubber granules; putting polycarbonate, PET, particle reinforced rubber granules, reinforced particles and a processing aid into a double-screw extruder, and extruding the particle reinforced rubber reinforced composite material by using the double-screw extruder. The high-temperature calcination process comprises the following steps: the calcining temperature is 1000 ℃, and the calcining time is 1 h. The volume ratio of niobium powder to aluminum nitride powder is 1: 2. the ball milling process comprises the following steps: the rotating speed of the ball mill is 600r/min, and the ball milling time is 3 h. The process for sintering the second mixture by spark plasma sintering comprises: the sintering temperature is 1900 ℃, the sintering pressure is 50MPa, and the sintering time is 10 min. The polycarbonate accounts for 100 parts, the PET accounts for 120 parts, the particle reinforced rubber granules account for 30 parts, and the reinforcing particles account for 10 parts by weight. The processing temperature of the double-screw extruder is as follows: the first zone temperature was 230 deg.C, the second zone temperature was 240 deg.C, the third zone temperature was 250 deg.C, the fourth zone temperature was 260 deg.C, and the die temperature was 250 deg.C. The screw rotating speed of the double-screw extruder is 50 r/min.
Example 3
A particle reinforced rubber reinforced composite is prepared by the following method: preparing particle reinforced rubber: putting methyl phenyl vinyl silicone rubber, a vulcanizing agent, silicon carbide powder, silicon dioxide powder and low-melting-point glass powder into an open mill for mixing to obtain a first mixture; vulcanizing the first mixture to obtain a first vulcanized product, wherein the vulcanization temperature is 150 ℃ and 160 ℃, and the vulcanization time is 10-20 min; drying the first vulcanized product in an oven at the drying temperature of 200 ℃ and the drying time of 210 ℃ for 5-6h to obtain a first dried product; calcining the first dried product at high temperature to obtain particle reinforced rubber; preparing reinforced particles: providing niobium powder and aluminum nitride powder, and carrying out ball milling on the niobium powder and the aluminum nitride powder to obtain a second mixture; sintering the second mixture by using a spark plasma sintering method to obtain a reinforced particle block; crushing the reinforced particle block to obtain reinforced particles; crushing the particle-reinforced rubber to obtain particle-reinforced rubber granules; putting polycarbonate, PET, particle reinforced rubber granules, reinforced particles and a processing aid into a double-screw extruder, and extruding the particle reinforced rubber reinforced composite material by using the double-screw extruder. The high-temperature calcination process comprises the following steps: the calcination temperature is 800-1000 ℃, and the calcination time is 1-2 h. The volume ratio of niobium powder to aluminum nitride powder is 1: 1-1: 2. the ball milling process comprises the following steps: the rotating speed of the ball mill is 500-. The process for sintering the second mixture by spark plasma sintering comprises: the sintering temperature is 1800-1900 ℃, the sintering pressure is 50-100MPa, and the sintering time is 10-30 min. The weight portion of the polycarbonate is 100 portions, the PET is 80-120 portions, the particle reinforced rubber granules are 20-30 portions, and the reinforced particles are 5-10 portions. The processing temperature of the double-screw extruder is as follows: the first zone temperature is 220-230 ℃, the second zone temperature is 230-240 ℃, the third zone temperature is 240-250 ℃, the fourth zone temperature is 250-260 ℃ and the die head temperature is 240-250 ℃. The screw rotating speed of the double-screw extruder is 50-70 r/min.
Example 4
In the preparation of the particle-reinforced rubber, the raw materials did not include silica powder, and the remaining parameters, steps, and components were the same as in example 3.
Example 5
In the preparation of the particle-reinforced rubber, the raw materials do not contain the low-melting glass powder, and the other parameters, steps and components are the same as those in example 3.
Example 6
Vulcanizing the first mixture to obtain a first vulcanized product, wherein the vulcanization temperature is 140 ℃, the vulcanization time is 30min, and the other parameters, steps and components are the same as those in example 3.
Example 7
Vulcanizing the first mixture to obtain a first vulcanized product, wherein the vulcanization temperature is 170 ℃, the vulcanization time is 5min, and the other parameters, steps and components are the same as those in example 3.
Example 8
The drying temperature is 220 ℃, the drying time is 4h, and the rest parameters, steps and components are the same as those in the embodiment 3.
Example 9
The high-temperature calcination process comprises the following steps: the calcining temperature is 700 ℃, and the calcining time is 4 h. The remaining parameters, steps and components were the same as in example 3.
Example 10
The high-temperature calcination process comprises the following steps: the calcining temperature is 1100 ℃, and the calcining time is 0.5 h. The remaining parameters, steps and components were the same as in example 3.
Example 11
The volume ratio of niobium powder to aluminum nitride powder was 2:1, and the remaining parameters, steps, and components were the same as in example 3.
Example 12
The volume ratio of niobium powder to aluminum nitride powder was 1:3, and the remaining parameters, steps and components were the same as in example 3.
Example 13
The ball milling process comprises the following steps: the rotating speed of the ball mill is 700r/min, the ball milling time is 2h, and the rest parameters, steps and components are the same as those in the embodiment 3.
Example 14
The process for sintering the second mixture by spark plasma sintering comprises: the sintering temperature is 2000 ℃, the sintering pressure is 80MPa, and the sintering time is 20 min. The remaining parameters, steps and components were the same as in example 3.
Example 15
The process for sintering the second mixture by spark plasma sintering comprises: the sintering temperature is 1700 ℃, the sintering pressure is 80MPa, and the sintering time is 20 min. The remaining parameters, steps and components were the same as in example 3.
Example 16
The process for sintering the second mixture by spark plasma sintering comprises: the sintering temperature is 1700 ℃, the sintering pressure is 120MPa, and the sintering time is 50 min. The remaining parameters, steps and components were the same as in example 3.
Example 17
The process for sintering the second mixture by spark plasma sintering comprises: the sintering temperature is 2000 ℃, the sintering pressure is 80MPa, and the sintering time is 5 min. The remaining parameters, steps and components were the same as in example 3.
Example 18
The polycarbonate, the PET, the particle-reinforced rubber granules and the reinforcing particles were added in amounts of 100 parts, 40 parts and 8 parts, respectively, and the parameters, steps and components were the same as in example 3.
Example 19
The polycarbonate, PET, reinforcing rubber granules and reinforcing particles were added in amounts of 100 parts, 25 parts and 12 parts, respectively, based on 100 parts by weight of polycarbonate, 100 parts of PET, and the other parameters, steps and components were the same as in example 3.
Example 20
The processing temperature of the double-screw extruder is as follows: the first zone temperature was 210 ℃, the second zone temperature was 245 ℃, the third zone temperature was 245 ℃, the fourth zone temperature was 255 ℃, the die temperature was 245 ℃, and the remaining parameters, steps, and components were the same as in example 3.
Example 21
The processing temperature of the double-screw extruder is as follows: the first zone temperature was 235 deg.C, the second zone temperature was 240 deg.C, the third zone temperature was 245 deg.C, the fourth zone temperature was 255 deg.C, the die temperature was 245 deg.C, and the remaining parameters, steps, and components were the same as in example 3.
Example 22
The processing temperature of the double-screw extruder is as follows: the first zone temperature was 225 deg.C, the second zone temperature was 235 deg.C, the third zone temperature was 235 deg.C, the fourth zone temperature was 265 deg.C, the die temperature was 255 deg.C, and the remaining parameters, steps, and components were the same as in example 3.
Example 23
The screw rotation speed of the twin-screw extruder is 80 r/min. The remaining parameters, steps and components were the same as in example 3.
Tensile strength, stiffness and notched impact strength tests were performed on examples 1-23, all according to relevant national standards, and for comparison, the test results were normalized based on example 1, and the final test results are shown in table 1.
TABLE 1
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (1)
1. A preparation method of a particle reinforced rubber reinforced composite material is characterized by comprising the following steps: the method comprises the following steps: preparing particle reinforced rubber: putting methyl phenyl vinyl silicone rubber, a vulcanizing agent, silicon carbide powder, silicon dioxide powder and low-melting-point glass powder into an open mill for mixing to obtain a first mixture; vulcanizing the first mixture to obtain a first vulcanized product, wherein the vulcanization temperature is 160 ℃, and the vulcanization time is 10 min; putting the first vulcanized product into an oven for drying at the drying temperature of 210 ℃ for 5 hours to obtain a first dried product; calcining the first dried product at high temperature to obtain particle reinforced rubber; preparing reinforced particles: providing niobium powder and aluminum nitride powder, and carrying out ball milling on the niobium powder and the aluminum nitride powder to obtain a second mixture; sintering the second mixture by using a spark plasma sintering method to obtain a reinforced particle block; crushing the reinforced particle block to obtain reinforced particles; crushing the particle-reinforced rubber to obtain particle-reinforced rubber granules; putting polycarbonate, PET, particle reinforced rubber granules, reinforced particles and a processing aid into a double-screw extruder, and extruding a particle reinforced rubber reinforced composite material by using the double-screw extruder, wherein the high-temperature calcination process comprises the following steps: the calcining temperature is 1000 ℃, the calcining time is 1h, and the volume ratio of the niobium powder to the aluminum nitride powder is 1: 2, the ball milling process comprises the following steps: the rotating speed of the ball mill is 600r/min, the ball milling time is 3h, and the process for sintering the second mixture by using the spark plasma sintering method specifically comprises the following steps: the sintering temperature is 1900 ℃, the sintering pressure is 50MPa, the sintering time is 10min, in parts by weight, 100 parts of polycarbonate, 120 parts of PET, 30 parts of particle reinforced rubber granules and 10 parts of reinforcing particles are counted, and the processing temperature of a double-screw extruder is as follows: the temperature of the first zone is 230 ℃, the temperature of the second zone is 240 ℃, the temperature of the third zone is 250 ℃, the temperature of the fourth zone is 260 ℃, the temperature of the die head is 250 ℃, and the screw rotating speed of the double-screw extruder is 50 r/min.
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| CN101541872A (en) * | 2006-11-24 | 2009-09-23 | 拜尔材料科学股份公司 | Impact-modified filled polycarbonate compositions |
| WO2011073290A1 (en) * | 2009-12-18 | 2011-06-23 | Bayer Materialscience Ag | Scratch-resistant, impact-resistant polycarbonate moulding compositions having good mechanical properties ii |
| CN104870562A (en) * | 2012-12-20 | 2015-08-26 | 沙特基础全球技术有限公司 | Thermoplastic compositions, methods of manufacture, and articles thereof |
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