CN117801520A - Preparation method of high-performance flame-retardant heat-conducting rubber compound in electronic industry - Google Patents
Preparation method of high-performance flame-retardant heat-conducting rubber compound in electronic industry Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-performance flame-retardant heat-conducting rubber compound in the electronic industry, which relates to the technical field of flame-retardant heat-conducting rubber compound preparation, and comprises the following steps of polymer matrix preparation, heat-conducting flame-retardant material preparation and rubber compound preparation: pretreatment, mixing, reaction, solvent removal, refining and cooling. The invention realizes the preparation of the raw materials for improving the mechanical properties of the rubber compound by designing the preparation of the polymer matrix, and solves the problem that the common rubber compound has poor mechanical properties and can not meet the requirements of mechanical stability and mechanical stability of the rubber compound in the electronic industry.
Description
Technical Field
The invention relates to the technical field of preparation of flame-retardant heat-conducting rubber compound, in particular to a preparation method of a high-performance flame-retardant heat-conducting rubber compound in the electronic industry.
Background
With the development of technology, the requirements of the electronic industry on materials are increasingly increased, the heat conducting materials meet the requirements of UL 94V-0, and the thickness of the heat conducting materials meeting the requirements of UL 94V-0 is increasingly thinner.
The flame retardant grade of the filling type flame retardant material is generally improved along with the increase of the filling ratio of the flame retardant filler, and the target flame retardant rubber compound on the market is used for ensuring good operability and mechanical properties of products, generally only has lower filling quantity, and the flame retardance can only achieve the thickness UL94 v-0 of more than 1.5 mm; although the high-efficiency flame retardant filled with a small amount of nitrogen and phosphorus can meet the requirement of UL 94V-0@thickness (0.5-1.5 mm), the high-efficiency flame retardant is easy to cause severe quality problems such as embrittlement, pulverization and the like of products in an aging test at 150 ℃, and the volume resistivity of the products is easy to be reduced due to moisture absorption in the storage or normal use of the products. Although the rubber product made of the methyl vinyl raw rubber is provided with ultralow oil seepage performance due to the molecular structure, the space is limited in the aspect of heat conduction and filling, and more flame retardants can be added to meet the flame retardance and heat conduction requirements on the premise that the liquid silica gel is provided with lower viscosity and the processability is not influenced, but the liquid silica gel product is poor in mechanical strength and cannot meet the requirements of partial application requirements, and the liquid silica gel generally has the defects of oil seepage and the like.
Therefore, the preparation method of the high-performance flame-retardant heat-conductive rubber compound in the electronic industry is very necessary to solve the problems in the prior art.
1. Patent document CN109957251B discloses a method for preparing a rubber compound, and the above patent realizes that the mechanical properties of the prepared rubber compound are more optimized compared with the prior art by optimizing the preparation process of the rubber compound, the tensile strength, the elongation at break and the tearing strength are obviously improved, the application range is wider, but the above patent cannot realize the preparation of raw materials for improving the mechanical properties of the rubber compound.
2. Patent document CN102424724B discloses a preparation method of a silicone rubber compound, the above patent realizes simple process and high product quality, and through the whole nitrogen charging protection rubber mixing process, the concentration of flammable and explosive gas is greatly reduced and extruded out of the kneader, explosion caused by static spark generated by rubber mixing is prevented, but the above patent cannot realize preparation of raw materials for improving the heat conduction and flame retardance of the compound.
3. Patent document CN113248925B discloses an environment-friendly halogen-free flame-retardant silicone rubber for buffering and vibration damping, a preparation method and application, the patent realizes excellent flame retardant property and mechanical property, the vibration damping efficiency is obvious, the requirements of environmental-friendly instructions in the electronic industry are met, the preparation method is easy to realize and convenient to popularize, but the patent cannot realize the treatment of optimizing the comprehensive performance of the rubber compound.
4. Patent document CN105542474B discloses an aluminum silver-plated conductive rubber plate and a preparation method thereof, and the patent realizes low cost, simple process, good processing performance of the rubber compound, bright product appearance, no pattern, softness, stable conductive performance, good electromagnetic shielding effect when being used in communication and electronic industries, but the patent can not realize comprehensive performance test function of the rubber compound.
In summary, the above-mentioned patent cannot realize the preparation of raw materials for improving mechanical properties of the rubber compound, the preparation of raw materials for improving heat conduction and flame retardance of the rubber compound, the treatment for optimizing the comprehensive properties of the rubber compound and the comprehensive performance test function of the rubber compound, so that the rubber compound cannot meet the mechanical strength performance requirements of the electronic industry, the heat conduction and flame retardance high performance requirements cannot be met, and the preparation process cannot be optimized;
therefore, the application provides a preparation method of the high-performance flame-retardant heat-conducting rubber compound in the electronic industry, which can realize the preparation of raw materials for improving the mechanical performance of the rubber compound, the preparation of raw materials for improving the heat-conducting flame-retardant performance of the rubber compound, the treatment for optimizing the comprehensive performance of the rubber compound and the comprehensive performance test function of the rubber compound.
Disclosure of Invention
The invention aims to provide a preparation method of a high-performance flame-retardant heat-conducting rubber compound in the electronic industry, which aims to solve the technical problems that the rubber compound cannot meet the mechanical strength performance requirement of the electronic industry, the heat-conducting flame-retardant high-performance requirement cannot be met and the preparation process cannot be optimized due to the fact that the preparation of raw materials for improving the mechanical performance of the rubber compound, the preparation of raw materials for improving the heat-conducting flame-retardant performance of the rubber compound, the treatment of the comprehensive performance optimization of the rubber compound and the comprehensive performance test function of the rubber compound cannot be realized in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the high-performance flame-retardant heat-conducting rubber compound in the electronic industry comprises the steps of preparing a polymer matrix, preparing a heat-conducting flame-retardant material and preparing the rubber compound, wherein the preparation of the polymer matrix comprises the following steps:
pretreatment: pretreating MDI, PDMS and ODA in a reaction kettle, and removing moisture through a drying agent;
mixing: adding the pretreated raw materials into a reaction kettle according to the molar ratio of 1:1:1, and starting mechanical stirring;
the reaction: heating to a reaction temperature in an inert atmosphere, and continuously stirring and reacting until reactants are completely reacted to form a polyimide solution;
solvent removal: removing residual solvent from the polyimide solution by solvent distillation or volatilization;
refining: further refining the obtained polyimide solution to improve the polymerization degree and remove impurities;
and (3) cooling: and cooling the refined polyimide matrix solution to room temperature to obtain the polyimide matrix with high molecular weight.
Preferably, the preparation of the heat-conducting flame-retardant material comprises the following steps:
step 1: heating methyl vinyl raw rubber and vinyl silicone resin to 120 ℃ by using a kneader to uniformly disperse;
step 2: adding the inorganic flame retardant in batches from small to large according to the particle size, and uniformly mixing;
step 3: adding a coupling agent, stirring uniformly, and vacuumizing and stirring for 30min;
step 4: taking out and placing for 24 hours for cooling;
step 5: placing the rubber compound by using an open mill, and adding a vulcanizing agent into the rubber compound;
step 6: and heating and curing to obtain the product with the determined structural size.
Preferably, the preparation method further comprises the steps of preparing the rubber compound:
the dispersing process comprises the following steps: ball milling and dispersing are carried out by using a high-speed stirrer and a bead mill, so that the heat-conducting flame-retardant material and the flame retardant are ensured to be uniformly dispersed in a polymer matrix, and the speed and the time are continuously adjusted to obtain a uniform dispersion system;
extrusion molding: introducing the dispersion system into a double-screw extrusion molding machine, controlling and adjusting extrusion temperature, and controlling and adjusting molding temperature and pressure by selecting extrusion, injection molding and calendaring molding process parameters meeting production requirements;
curing heat treatment: and introducing the extruded mixed material into a heat curing furnace, controlling and adjusting the temperature and time of curing and heat treatment to promote the cross-linking reaction of the polyimide matrix, and optimizing the crystallization and the heat stability of the material.
Preferably, the preparation of the rubber compound further comprises performance optimization treatment:
interface modification: the silane coupling agent is adopted, and the interface between the heat conduction flame retardant material and the polymer matrix is more compatible through solution mixing and reaction;
filler application: modified zinc oxide, modified aluminum oxide, a plasticizer and a stabilizer are added into the mixed solution, the specific surface area of the modified filler is increased, the mechanical property and the heat conducting property of the material are improved, and the flame-retardant heat conducting rubber compound containing the modified silicon oxide is prepared by a sol-gel method.
Preferably, the preparation method further comprises quantitative performance test, wherein the quantitative performance test takes IPC standard of the electronic industry as a specification;
the quantitative performance test includes: a thermal conductivity test, a flame retardant test and a mechanical property test;
and (3) testing heat conduction performance: carrying out heat conduction performance parameter test on the finished product of the rubber compound by using a laser thermal conductivity meter and a heat conductivity testing instrument;
flame retardant performance test: performing flame retardant performance parameter tests on the finished rubber compound product by using a vertical combustion test and a horizontal combustion test method, and evaluating the flame retardant performance of the rubber compound by adopting a UL94 standard test method;
mechanical property test: the tensile and flexural properties of the compounds, including tensile strength and flexural strength, were tested by a universal tester.
Preferably, the heat-conducting flame-retardant material is used for improving the heat-conducting flame-retardant performance of the rubber compound;
the heat-conducting flame-retardant material comprises: methyl vinyl raw rubber and vinyl silicone resin;
the raw rubber of methyl ethylene has the molecular weight of 20-40 ten thousand, the vinyl content of 0.14-0.22 percent and 95-98 parts, compared with the raw rubber with the conventional 60 molecular weight, the raw rubber is more 'powder-eating', and the hardness of the vulcanized rubber is adjusted by adjusting the raw rubber proportion of different vinyl contents;
the vinyl silicone resin has the viscosity of 6000-20000, the vinyl content of 0.95-1.3%, and 2-5 parts, and is liquid.
Preferably, the rubber compound comprises a polymer matrix, wherein the polymer matrix is used for improving the mechanical property and high-temperature stability of the rubber compound;
the polymer matrix comprises: polyimide matrix and polyether-ether-ketone matrix;
the polyimide matrix is prepared from the following raw materials: the molar ratio of the raw materials of the dimethylbenzene diisocyanate MDI, the polydimethylsiloxane PDMS and the 4, 4-diaminodiphenyl ether ODA to the polyimide matrix is 1:1:1, a step of;
the polyether-ether-ketone group is prepared from the following raw materials: terephthalic acid, terephthalic acid and 4, 4-diaminodiphenyl ether, and the raw material preparation mole ratio of the polyether-ether-ketone matrix is 1:1:1.
preferably, the heat-conducting flame-retardant material is filled with heat-conducting flame-retardant filler, and the heat-conducting flame-retardant filler is used for improving the heat-conducting property and flame-retardant property of the heat-conducting flame-retardant material;
the heat-conducting flame-retardant filler comprises: inorganic flame retardants with different particle sizes, modified zinc oxide and modified aluminum oxide;
the particle size of the inorganic flame retardant with different particle sizes is 8-40um,180-220 parts;
the particle size of the modified zinc oxide is smaller than 1um,20-40 parts, the particle size of the modified aluminum oxide is 2-4um,30-50 parts, and the heat conduction flame retardant filler forms the closest packing.
Preferably, an auxiliary agent is added in the heat-conducting flame-retardant material, and the auxiliary agent is used for enhancing the processability and the material stability of the heat-conducting flame-retardant material;
the auxiliary agent comprises: coupling agents, crosslinking agents, vulcanizing agents, plasticizers, and stabilizers;
0.5 part of coupling agent, 0.5 part of benzoyl peroxide cross-linking agent, 3-5 parts of bi-di-pentaperoxide vulcanizing agent, 1 part of epoxy resin plasticizer and 1 part of stabilizer.
Preferably, the inorganic flame retardant is one or more of aluminum hydroxide and magnesium hydroxide materials with particle sizes, the inorganic flame retardant is spherical and angular in shape, the inorganic flame retardant is non-nitrogen-phosphorus flame retardant, and the thickness of the excellent heat-conducting sheet of the rubber compound is between 0.05 and 1 mm.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the preparation of the polymer matrix is designed, so that the preparation of raw materials for improving the mechanical properties of the rubber compound is realized, and the problem that the mechanical properties of the common rubber compound are poor and the requirements on the mechanical and mechanical stability properties of the rubber compound in the electronic industry cannot be met is solved;
2. according to the invention, the preparation of the heat-conducting flame-retardant material is designed, so that the preparation of raw materials for improving the heat-conducting flame-retardant property of the rubber compound is realized, and the problem that the common rubber compound cannot meet the requirements of ageing procedures in the electronic industry on good heat conductivity and flame retardant coefficient of the rubber compound is solved;
3. according to the invention, the performance optimization treatment is designed, so that the comprehensive performance optimization treatment of the rubber compound is realized, the comprehensive performance of the rubber compound is improved, the rubber compound meets the higher heat conduction and flame retardance requirements, and the mechanical strength of the rubber compound is increased;
4. according to the invention, by designing quantitative performance test, the comprehensive performance test function of the rubber compound is realized, the problem that the process parameter optimization cannot be performed due to the lack of test data support in the rubber compound preparation process is solved, and the preparation process method of the rubber compound is optimized.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
An embodiment of the present invention provides: the preparation method of the high-performance flame-retardant heat-conducting rubber compound in the electronic industry comprises the steps of preparing a polymer matrix, preparing a heat-conducting flame-retardant material and preparing the rubber compound, wherein the preparation of the polymer matrix comprises the following steps:
pretreatment: pretreating MDI, PDMS and ODA in a reaction kettle, and removing moisture through a drying agent;
mixing: adding the pretreated raw materials into a reaction kettle according to the molar ratio of 1:1:1, and starting mechanical stirring;
the reaction: heating to a reaction temperature in an inert atmosphere, and continuously stirring and reacting until reactants are completely reacted to form a polyimide solution;
solvent removal: removing residual solvent from the polyimide solution by solvent distillation or volatilization;
refining: further refining the obtained polyimide solution to improve the polymerization degree and remove impurities;
and (3) cooling: cooling the refined polyimide matrix solution to room temperature to obtain a polyimide matrix with high molecular weight;
furthermore, the polyimide matrix is prepared after pretreatment, mixing, reaction, solvent removal, refining and cooling treatment, the stability problem of the polyimide matrix in a high-temperature environment is solved through a reasonable formula and a reaction process, meanwhile, the problem of chemical stability is solved through selecting a specific monomer, and the flexibility of the material is improved by adding the polydimethylsiloxane in the preparation process, so that the requirements on the flexibility and toughness of the rubber compound in the electronic industry are solved.
Example 2
An embodiment of the present invention provides: the preparation method of the high-performance flame-retardant heat-conducting rubber compound in the electronic industry comprises the following steps of:
step 1: heating methyl vinyl raw rubber and vinyl silicone resin to 120 ℃ by using a kneader to uniformly disperse;
step 2: adding the inorganic flame retardant in batches from small to large according to the particle size, and uniformly mixing;
step 3: adding a coupling agent, stirring uniformly, and vacuumizing and stirring for 30min;
step 4: taking out and placing for 24 hours for cooling;
step 5: placing the rubber compound by using an open mill, and adding a vulcanizing agent into the rubber compound;
step 6: heating and curing to obtain a product with a determined structural size;
further, the use of a relatively low molecular weight methyl vinyl gum mixed with a small amount of liquid vinyl silicone resin improves the "powder-eating" ability and mechanical properties of the resin after vulcanization, and the high molecular weight resin can meet low oil yield; the aluminum hydroxide and other flame-retardant heat-conducting fillers are subjected to surface modification treatment, so that the compatibility with resin is improved, the fillable amount is increased, and the flame-retardant effect and the heat-conducting effect are met; the reasonable particle size matching in the filler can not only improve the filling quantity, but also be helpful for forming a compact ceramic layer for heat insulation and improving the flame retardant effect in the combustion of the material product.
Example 3
An embodiment of the present invention provides: the preparation method of the high-performance flame-retardant heat-conducting rubber compound in the electronic industry further comprises the following steps of:
the dispersing process comprises the following steps: ball milling and dispersing are carried out by using a high-speed stirrer and a bead mill, so that the heat-conducting flame-retardant material and the flame retardant are ensured to be uniformly dispersed in a polymer matrix, and the speed and the time are continuously adjusted to obtain a uniform dispersion system;
extrusion molding: introducing the dispersion system into a double-screw extrusion molding machine, controlling and adjusting extrusion temperature, and controlling and adjusting molding temperature and pressure by selecting extrusion, injection molding and calendaring molding process parameters meeting production requirements;
curing heat treatment: introducing the extruded mixed material into a heat curing furnace, controlling and adjusting the temperature and time of curing and heat treatment to promote the cross-linking reaction of the polyimide matrix, and optimizing the crystallization and the heat stability of the material;
further, stirring and bead grinding are carried out by a high-speed stirrer and a bead mill in a dispersing process, so that the heat-conducting flame-retardant material, the flame retardant and the polymer matrix are fully and uniformly mixed to obtain a uniform dispersion system, then the molding temperature, time and pressure of an extrusion molding machine are regulated to prepare a semi-finished product of the rubber compound meeting the production process requirements, finally the curing and heat treatment temperature and time are regulated by curing heat treatment, the polyimide matrix is subjected to crosslinking reaction under the action of a re-crosslinking agent, and the semi-finished product of the rubber compound is subjected to heat treatment and curing to obtain a finished product of the rubber compound.
Example 4
An embodiment of the present invention provides: a preparation method of a high-performance flame-retardant heat-conducting rubber compound in the electronic industry comprises the following steps:
interface modification: the silane coupling agent is adopted, and the interface between the heat conduction flame retardant material and the polymer matrix is more compatible through solution mixing and reaction;
filler application: adding modified zinc oxide, modified aluminum oxide, a plasticizer and a stabilizer into the mixed solution, improving the specific surface area of modified filler, improving the mechanical property and the heat conducting property of the material, and preparing a flame-retardant heat conducting rubber compound containing modified silicon oxide by a sol-gel method;
further, a surfactant and a silane coupling agent are introduced, and through solution mixing and reaction, the heat-conducting flame-retardant material and the polymer matrix are fused more tightly, and through adding modified zinc oxide, modified aluminum oxide, a plasticizer and a stabilizer, the specific surface area of modified filler is increased, the mechanical property and the heat-conducting property of the rubber compound are enhanced, and the rubber compound meets the strength requirement of the rubber compound in the electronic industry.
Example 5
An embodiment of the present invention provides: the preparation method of the high-performance flame-retardant heat-conducting rubber compound in the electronic industry further comprises quantitative performance test, wherein the quantitative performance test takes the IPC standard in the electronic industry as a specification;
the quantitative performance test includes: a thermal conductivity test, a flame retardant test and a mechanical property test;
and (3) testing heat conduction performance: carrying out heat conduction performance parameter test on the finished product of the rubber compound by using a laser thermal conductivity meter and a heat conductivity testing instrument;
flame retardant performance test: performing flame retardant performance parameter tests on the finished rubber compound product by using a vertical combustion test and a horizontal combustion test method, and evaluating the flame retardant performance of the rubber compound by adopting a UL94 standard test method;
mechanical property test: testing tensile and bending properties of the rubber compound by a universal testing machine, wherein the tensile and bending properties comprise tensile strength and bending strength;
further, a laser thermal conductivity meter and a thermal conductivity testing instrument are used for detecting the thermal conductivity of the finished rubber compound, a vertical combustion test and a horizontal combustion test are used for carrying out combustion test on the finished rubber compound sheet, a UL94 standard test method is adopted for evaluating whether the flame retardant property of the rubber compound meets the flame retardant parameter requirement of the electronic industry, a universal testing machine is used for carrying out tensile and bending property test on the rubber compound, and whether the tensile strength and bending strength of the rubber compound meet the parameter requirement of the electronic industry is evaluated.
Example 6
An embodiment of the present invention provides: a preparation method of a high-performance flame-retardant heat-conductive rubber compound in the electronic industry comprises the steps that a heat-conductive flame-retardant filler is filled in a heat-conductive flame-retardant material, and the heat-conductive flame-retardant filler is used for improving the heat-conductive property and flame-retardant property of the heat-conductive flame-retardant material;
the heat-conducting flame-retardant filler comprises: inorganic flame retardants with different particle sizes, modified zinc oxide and modified aluminum oxide;
the particle size of the inorganic flame retardant with different particle sizes is 8-40um,180-220 parts;
the particle size of the modified zinc oxide is smaller than 1um,20-40 parts, the particle size of the modified aluminum oxide is 2-4um,30-50 parts, and the heat conduction flame retardant filler forms the closest packing;
further, 35um and 190 parts of inorganic flame retardant are selected as particle size, 0.85um and 35 parts of modified zinc oxide are selected as particle size, 2.5um and 38 parts of modified aluminum oxide are added into the mixed solution for fusion reaction, the heat conduction and flame retardance of the rubber compound are improved, the rubber compound is subjected to quantitative performance test and evaluation, the flame retardant addition parameters are continuously adjusted to optimize the performance of the rubber compound, the multi-component rubber compound is designed, more comprehensive performance is formed, and the production requirements and sustainable development of the electronic industry are met.
Example 7
An embodiment of the present invention provides: a preparation method of a high-performance flame-retardant heat-conducting rubber compound in the electronic industry comprises the steps that a polymer matrix is included in the rubber compound, and the polymer matrix is used for improving the mechanical property and the high-temperature stability of the rubber compound;
the polymer matrix comprises: polyimide matrix and polyether-ether-ketone matrix;
the polyimide matrix is prepared from the following raw materials: the molar ratio of the raw materials of the dimethylbenzene diisocyanate MDI, the polydimethylsiloxane PDMS and the 4, 4-diaminodiphenyl ether ODA to the polyimide matrix is 1:1:1, a step of;
the polyether-ether-ketone group is prepared from the following raw materials: terephthalic acid, terephthalic acid and 4, 4-diaminodiphenyl ether, and the raw material preparation mole ratio of the polyether-ether-ketone matrix is 1:1:1, a step of;
further, the polymer matrix can also be a polyether-ether-ketone matrix, and the preparation method of the polyether-ether-ketone matrix is as follows:
pretreatment: pretreating terephthalic acid, terephthalic acid and ODA in a reaction kettle to remove water and impurities;
mixing: adding the pretreated raw materials into a reaction kettle according to the molar ratio of 1:1:1, and starting mechanical stirring;
the reaction: heating to a reaction temperature in an inert atmosphere, and starting a polymerization reaction to generate a polymer chain of polyether-ether-ketone;
solvent removal: removing residual solvent from the polyether-ether-ketone solution obtained by the reaction through a volatilization method or solvent distillation;
precipitation: adding the obtained polyether-ether-ketone solution into a non-solvent to precipitate a polymer;
filtration and washing: filtering and separating the precipitated polyether-ether-ketone, and washing with a proper solvent to remove unreacted monomers and impurities;
and (3) drying: and drying the filtered polyether-ether-ketone, and removing residual solvent to obtain the final high-performance polymer matrix.
The method comprises the following steps of firstly, preparing a polymer matrix as a raw material of a rubber compound, then preparing a heat-conducting flame-retardant material by mixing methyl vinyl raw rubber and liquid vinyl silicone resin, and carrying out surface modification treatment by using modified alumina and modified zinc oxide in the preparation process; meanwhile, inorganic flame retardants and auxiliary agents are filled in the mixed collagen mixture to improve the comprehensive performance of the mixed rubber; then, preparing a finished product of the rubber compound from the mixed collagen through a preparation process and performance optimization treatment; and finally, carrying out quantitative performance test on the finished product of the rubber compound to adjust the parameter design of the preparation process and prepare the finished product of the rubber compound meeting the standard requirements of the electronic industry.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. A preparation method of a high-performance flame-retardant heat-conducting rubber compound in the electronic industry is characterized by comprising the following steps of: the preparation method comprises the steps of preparing a polymer matrix, preparing a heat-conducting flame-retardant material and preparing a rubber compound, wherein the preparation of the polymer matrix comprises the following steps:
pretreatment: pretreating MDI, PDMS and ODA in a reaction kettle, and removing moisture through a drying agent;
mixing: adding the pretreated raw materials into a reaction kettle according to the molar ratio of 1:1:1, and starting mechanical stirring;
the reaction: heating to a reaction temperature in an inert atmosphere, and continuously stirring and reacting until reactants are completely reacted to form a polyimide solution;
solvent removal: removing residual solvent from the polyimide solution by solvent distillation or volatilization;
refining: further refining the obtained polyimide solution to improve the polymerization degree and remove impurities;
and (3) cooling: and cooling the refined polyimide matrix solution to room temperature to obtain the polyimide matrix with high molecular weight.
2. The method for preparing the high-performance flame-retardant heat-conductive rubber compound in the electronic industry, which is characterized by comprising the following steps of: the preparation of the heat-conducting flame-retardant material comprises the following steps:
step 1: heating methyl vinyl raw rubber and vinyl silicone resin to 120 ℃ by using a kneader to uniformly disperse;
step 2: adding the inorganic flame retardant in batches from small to large according to the particle size, and uniformly mixing;
step 3: adding a coupling agent, stirring uniformly, and vacuumizing and stirring for 30min;
step 4: taking out and placing for 24 hours for cooling;
step 5: placing the rubber compound by using an open mill, and adding a vulcanizing agent into the rubber compound;
step 6: and heating and curing to obtain the product with the determined structural size.
3. The method for preparing the high-performance flame-retardant heat-conductive rubber compound in the electronic industry, which is characterized by comprising the following steps of: the preparation method also comprises the steps of preparing the rubber compound:
the dispersing process comprises the following steps: ball milling and dispersing are carried out by using a high-speed stirrer and a bead mill, so that the heat-conducting flame-retardant material and the flame retardant are ensured to be uniformly dispersed in a polymer matrix, and the speed and the time are continuously adjusted to obtain a uniform dispersion system;
extrusion molding: introducing the dispersion system into a double-screw extrusion molding machine, controlling and adjusting extrusion temperature, and controlling and adjusting molding temperature and pressure by selecting extrusion, injection molding and calendaring molding process parameters meeting production requirements;
curing heat treatment: and introducing the extruded mixed material into a heat curing furnace, controlling and adjusting the temperature and time of curing and heat treatment to promote the cross-linking reaction of the polyimide matrix, and optimizing the crystallization and the heat stability of the material.
4. The method for preparing the high-performance flame-retardant and heat-conductive rubber compound in the electronic industry, which is characterized by comprising the following steps of: the preparation of the rubber compound further comprises the performance optimization treatment:
interface modification: the silane coupling agent is adopted, and the interface between the heat conduction flame retardant material and the polymer matrix is more compatible through solution mixing and reaction;
filler application: modified zinc oxide, modified aluminum oxide, a plasticizer and a stabilizer are added into the mixed solution, the specific surface area of the modified filler is increased, the mechanical property and the heat conducting property of the material are improved, and the flame-retardant heat conducting rubber compound containing the modified silicon oxide is prepared by a sol-gel method.
5. The method for preparing the high-performance flame-retardant and heat-conductive rubber compound in the electronic industry, which is characterized by comprising the following steps of: the preparation method further comprises quantitative performance test, wherein the quantitative performance test takes the IPC standard of the electronic industry as a specification;
the quantitative performance test includes: a thermal conductivity test, a flame retardant test and a mechanical property test;
and (3) testing heat conduction performance: carrying out heat conduction performance parameter test on the finished product of the rubber compound by using a laser thermal conductivity meter and a heat conductivity testing instrument;
flame retardant performance test: performing flame retardant performance parameter tests on the finished rubber compound product by using a vertical combustion test and a horizontal combustion test method, and evaluating the flame retardant performance of the rubber compound by adopting a UL94 standard test method;
mechanical property test: the tensile and flexural properties of the compounds, including tensile strength and flexural strength, were tested by a universal tester.
6. A method for preparing a high-performance flame-retardant and heat-conductive rubber compound in the electronic industry, which is applicable to the high-performance flame-retardant and heat-conductive rubber compound in any one of claims 1-5, and is characterized in that: the heat-conducting flame-retardant material is used for improving the heat-conducting flame-retardant performance of the rubber compound;
the heat-conducting flame-retardant material comprises: methyl vinyl raw rubber and vinyl silicone resin;
the raw rubber of methyl ethylene has the molecular weight of 20-40 ten thousand, the vinyl content of 0.14-0.22 percent and 95-98 parts, compared with the raw rubber with the conventional 60 molecular weight, the raw rubber is more 'powder-eating', and the hardness of the vulcanized rubber is adjusted by adjusting the raw rubber proportion of different vinyl contents;
the vinyl silicone resin has the viscosity of 6000-20000, the vinyl content of 0.95-1.3%, and 2-5 parts, and is liquid.
7. The high performance flame retardant and thermally conductive compound for the electronics industry of claim 6, wherein: the rubber compound comprises a polymer matrix, wherein the polymer matrix is used for improving the mechanical property and high-temperature stability of the rubber compound;
the polymer matrix comprises: polyimide matrix and polyether-ether-ketone matrix;
the polyimide matrix is prepared from the following raw materials: the molar ratio of the raw materials of the dimethylbenzene diisocyanate MDI, the polydimethylsiloxane PDMS and the 4, 4-diaminodiphenyl ether ODA to the polyimide matrix is 1:1:1, a step of;
the polyether-ether-ketone group is prepared from the following raw materials: terephthalic acid, terephthalic acid and 4, 4-diaminodiphenyl ether, and the raw material preparation mole ratio of the polyether-ether-ketone matrix is 1:1:1.
8. the high performance flame retardant and thermally conductive compound for the electronics industry of claim 6, wherein: the heat-conducting flame-retardant material is filled with heat-conducting flame-retardant filler, and the heat-conducting flame-retardant filler is used for improving the heat-conducting property and flame-retardant property of the heat-conducting flame-retardant material;
the heat-conducting flame-retardant filler comprises: inorganic flame retardants with different particle sizes, modified zinc oxide and modified aluminum oxide;
the particle size of the inorganic flame retardant with different particle sizes is 8-40um,180-220 parts;
the particle size of the modified zinc oxide is smaller than 1um,20-40 parts, the particle size of the modified aluminum oxide is 2-4um,30-50 parts, and the heat conduction flame retardant filler forms the closest packing.
9. The high performance flame retardant and thermally conductive rubber compound for the electronics industry of claim 8, wherein: an auxiliary agent is added into the heat-conducting flame-retardant material, and the auxiliary agent is used for enhancing the processability and the material stability of the heat-conducting flame-retardant material;
the auxiliary agent comprises: coupling agents, crosslinking agents, vulcanizing agents, plasticizers, and stabilizers;
0.5 part of coupling agent, 0.5 part of benzoyl peroxide cross-linking agent, 3-5 parts of bi-di-pentaperoxide vulcanizing agent, 1 part of epoxy resin plasticizer and 1 part of stabilizer.
10. The high performance flame retardant and thermally conductive rubber compound for the electronics industry of claim 8, wherein: the inorganic flame retardant is one or more of aluminum hydroxide and magnesium hydroxide materials with particle sizes, the inorganic flame retardant is spherical and angular in shape, the inorganic flame retardant is non-nitrogen-phosphorus flame retardant, and the thickness of the excellent heat-conducting sheet of the rubber compound is between 0.05 and 1 mm.
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| CN1640937A (en) * | 2004-12-22 | 2005-07-20 | 华南理工大学 | Fire-retardant silicon rubber and its preparation method |
| CN101735620A (en) * | 2009-12-27 | 2010-06-16 | 周忠坤 | High-temperature resisting methyl vinyl silicone rubber |
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