CN113637326B - Preparation method of graphene additive for heat-conducting silica gel material - Google Patents
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Abstract
The invention discloses a preparation method of a graphene additive for a heat-conducting silica gel material, wherein the graphene additive is graphene powder obtained by reducing a graphene oxide solution by a special reducing agent, and the preparation method of the graphene additive comprises the following steps: s1: heating the graphene oxide solution to 50-60 ℃; s2: slowly adding a special reducing agent into the graphene oxide solution, and reacting for 23-25 hours under the water bath condition of 65-75 ℃; s3: and after the reaction is finished, carrying out centrifugal separation on the obtained solution, washing the solution to be neutral, and finally carrying out vacuum drying to obtain graphene additive powder. According to the invention, the graphene oxide is reduced by adding the special reducing agent, so that the graphene microchip structure contains functional groups, the phenomena of poor dispersion and serious agglomeration of common graphene in the heat-conducting silica gel are improved, the graphene additive can be well and uniformly dispersed in the silicone oil matrix of the heat-conducting silica gel, and the heat conductivity of the heat-conducting silica gel material is effectively improved.
Description
Technical Field
The invention belongs to the technical field of heat-conducting silica gel, and particularly relates to a preparation method of a graphene additive for a heat-conducting silica gel material.
Background
With the rapid development of semiconductor facilities such as modern electronic equipment and LEDs, the demand and manufacturing difficulty of heat conductive materials are becoming higher and higher. The traditional heat-conducting silicone grease material has the property problem that the heat-conducting property is reduced along with the volatilization of the material, so that the performance of an element is influenced. The heat-conducting silica gel is a thermal interface material compounded by a silica gel matrix and a heat-conducting filler, and is applied to electronic devices including LED lamps by virtue of the advantages of good heat conductivity, flexibility, stability, natural surface adhesion and the like.
As a composite thermal interface material, the thermal conductivity of the silica gel matrix is poor, and therefore, a thermal conductive filler needs to be added to improve the thermal conductivity. Generally, heat-conducting fillers such as copper, aluminum oxide, aluminum nitride and silicon carbide are applied to the market, the heat-conducting silica gel matrix is filled with the heat-conducting fillers according to the same volume fraction or mass fraction, the higher the heat conductivity is, the more excellent the heat-conducting performance of the composite material is, and therefore the composite material with higher heat conductivity can be prepared by selecting the fillers with higher heat conductivity. Graphene is used as a novel heat-conducting filler, has the advantages of ultrahigh carrier mobility, excellent heat conductivity, high specific surface area, high flexibility and the like, so that the graphene is filled in a heat-conducting silica gel matrix, the graphene-based heat-conducting material with high heat conductivity can be prepared, and the heat-conducting property is far superior to that of an interface heat-conducting material prepared by adopting other traditional fillers.
Most of common graphene in the current market can not be well dispersed in a silica gel matrix, so that the heat conduction of the material is uneven, and the graphene and various components of the heat conduction silica gel have mutual repulsion, and the properties of the material, such as curing time, viscosity and the like, are influenced. Therefore, it is necessary to invent a graphene additive suitable for a heat-conducting silica gel material.
Disclosure of Invention
The invention provides a preparation method of a graphene additive for a heat-conducting silica gel material, aiming at overcoming the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a graphene additive for a heat-conducting silica gel material is provided, wherein the graphene additive is graphene powder obtained by reducing a graphene oxide solution by a special reducing agent, and the preparation method of the graphene additive comprises the following steps:
s1: heating the graphene oxide solution to 50-60 ℃;
s2: slowly adding a special reducing agent into the graphene oxide solution, and reacting for 23-25 hours at 65-75 ℃ under the water bath condition;
s3: and after the reaction is finished, carrying out centrifugal separation on the obtained solution, washing the solution to be neutral, and finally carrying out vacuum drying to obtain graphene additive powder.
Optionally, the special reducing agent is an R-based hydrazine, wherein R is an alkyl group of 1 to 8 and an isomer thereof, and the molecular structure thereof is:
optionally, the special reducing agent comprises one or more of tert-butyl hydrazine, methyl hydrazine and octyl hydrazine.
Optionally, the preparation method of the special reducing agent is as follows:
adding concentrated sulfuric acid and urea into a synthesis device, and reacting for 1-3 hours at 15-25 ℃ under an ice bath condition, wherein the molar ratio is 2:1;
II, slowly dropwise adding R alcohol into the synthesis device, wherein the molar ratio of the R alcohol to the urea is 1:1, reacting for 3-5 hours at the temperature of 20-25 ℃, standing for 15-17 hours at room temperature, adding ammonia water to neutralize the pH value to 3-4, filtering and drying to obtain white crystal R-based urea;
III, dissolving R-urea in ethanol, dropwise adding an ethanol solution containing chlorine into the device, and reacting at 14-16 ℃ for 0.2-1 hour after dropwise adding, wherein the molar ratio of the chlorine to the R-urea is 1.05;
and IV, dissolving NaOH in water to prepare an aqueous solution, slowly dropwise adding the aqueous solution into the device, keeping the temperature of 4-6 ℃ for reaction for 0.5-1.5 hours, wherein the molar ratio of the NaOH to the R-based urea is 4.5-5.0, then filtering the reaction solution, and heating the filtrate to obtain a fraction at 100-104 ℃ to obtain the special reducing agent R-based hydrazine.
Optionally, the preparation reaction process of the special reducing agent is as follows:
optionally, in the S1, the temperature of the graphene oxide solution is raised to 55 ℃. After the graphene oxide solution is heated, the next reduction reaction is more facilitated.
Optionally, the volume ratio of the graphene oxide solution to the special reducing agent in S2 is 1.
Optionally, the dropping speed of the special reducing agent in the S2 is 0.1-0.12mL/S.
Optionally, the temperature of vacuum drying in the step S3 is-11 to-9 ℃, and the drying time is 70 to 74 hours.
Optionally, the centrifugal speed of the centrifugal separation in the S3 is 8000-10000r/min.
In conclusion, the beneficial effects of the invention are as follows:
the in-process of special reductant at reduction oxidation graphite alkene for contain the functional group in the graphite alkene microchip structure, this special oxygen-containing functional group can with organic matter long chain better connection such as silica gel, thereby make the two more effectual combinations, the phenomenon that common graphite alkene disperses badly in heat conduction silica gel has been improved, reunion is serious, make good homodisperse of graphite alkene additive in heat conduction silica gel's silicon oil base member, it is more smooth and easy to make the material dispel the heat, the effectual heat conductivity that has improved heat conduction silica gel material, tensile strength, the curing time and the material viscosity of heat conduction silica gel have been optimized, make heat conduction silica gel can regard as thermal interface combined material better.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It is to be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the appended claims.
A preparation method of a graphene additive for a heat-conducting silica gel material comprises the following steps:
s1: heating the graphene oxide solution to 50-60 ℃;
s2: slowly adding a special reducing agent into the graphene oxide solution, and reacting for 20-28 hours under the water bath condition of 65-75 ℃; dropwise adding the graphene oxide solution by using a separating funnel;
s3: and after the reaction is finished, carrying out centrifugal separation on the obtained solution, washing the solution to be neutral, and finally carrying out vacuum drying to obtain graphene additive powder.
The special reducing agent is R-based hydrazine, wherein R is alkyl of 1-8 and isomers thereof, and the special reducing agent comprises one or more of tert-butyl hydrazine, methyl hydrazine and octyl hydrazine.
The preparation method of the special reducing agent comprises the following steps:
adding concentrated sulfuric acid and urea into a synthesis device, and reacting for 1-3 hours at 15-25 ℃ under an ice bath condition, wherein the molar ratio is 2:1;
II, slowly dropwise adding R alcohol into the synthesis device, wherein the molar ratio of the R alcohol to the urea is 1:1, reacting for 2-6 hours at the temperature of 20-25 ℃, standing for 12-20 hours at room temperature, adding ammonia water to neutralize the pH value to 3-4, filtering and drying to obtain white crystal R-based urea;
III, dissolving R-urea in ethanol, dropwise adding an ethanol solution containing chlorine into the device, and reacting at 10-20 ℃ for 0.2-1 hour after dropwise adding, wherein the molar ratio of the chlorine to the R-urea is 1.05;
and IV, dissolving NaOH in water to prepare an aqueous solution, slowly dripping the aqueous solution into the device, keeping the temperature of 2-10 ℃ for reaction for 0.5-2 hours, wherein the molar ratio of NaOH to R-based urea is 4.5-5.0, then filtering the reaction solution, and heating the filtrate to obtain a fraction at 100-104 ℃ to obtain the special reducing agent R-based hydrazine.
The volume ratio of the graphene oxide solution to the special reducing agent in S2 is 1-10.
The dropping speed of the special reducing agent in the S2 is 0.1-0.12mL/S.
And the temperature of vacuum drying in the S3 is-10 ℃, and the drying time is 72 hours.
And the centrifugal speed of the centrifugal separation in the S3 is 8000-10000r/min.
Example 1
The specific reducing agent used in this example was t-butylhydrazine.
1. Manufacturing process
A preparation method of a graphene additive for a heat-conducting silica gel material comprises the following steps:
s1a: heating the graphene oxide solution to 55 ℃;
s2a: slowly adding a special reducing agent into the graphene oxide solution, and reacting for 24 hours at 70 ℃ in a water bath;
s3a: and after the reaction is finished, carrying out centrifugal separation on the obtained solution, washing the solution to be neutral, and finally carrying out vacuum drying to obtain graphene additive powder.
Wherein, the special reducing agent in the step S2a is tert-butylhydrazine, and the specific preparation method is as follows:
(1-1) adding 193g of concentrated sulfuric acid (the mass fraction is 98.5%) and 60g of ground urea into a synthesis device, and reacting for 2 hours at 15 ℃ under an ice bath condition, wherein the molar ratio is 2:1;
(1-2) slowly dropwise adding 74g of tert-butyl alcohol into a synthesis device, wherein the molar ratio of tert-butyl alcohol to urea is 1:1, keeping the temperature at 24 ℃ for reaction for 4 hours, after dropwise adding, standing at room temperature for 16 hours, adding ammonia water for neutralizing the pH value to 3-4, filtering and drying to obtain white crystal tert-butyl urea;
(1-3) dissolving 10g of tert-butyl urea in ethanol, controlling the temperature to be 15 ℃, dropwise adding 19mL of ethanol solution containing 6.4g of chlorine into the device, reacting for half an hour at 15 ℃ after dropwise adding is finished, and controlling the molar ratio of the chlorine to the tert-butyl urea to be 1.05;
(1-4) under the condition of ice bath at 5 ℃, slowly dropwise adding 16.4g of NaOH into the device, dissolving the NaOH in 160mL of water to prepare an aqueous solution, wherein the molar ratio of the NaOH to the tert-butyl urea is 4.6, the reaction solution is continuously stirred for half an hour after dropping for about one hour, then filtering the reaction solution, heating the filtrate, taking a fraction at 100-104 ℃, and obtaining the aqueous solution of tert-butyl hydrazine.
The concentration of the graphene oxide solution in the step S1a is 6g/L.
The volume ratio of the graphene oxide solution to the tert-butylhydrazine in the step S2a is 1.
Slowly adding the special reducing agent in the step S2a, wherein the specific dropping speed is 0.1mL/S.
And (3) performing centrifugal separation in the step (S3 a), wherein the specific centrifugal speed is 10000r/min.
And (3) performing vacuum drying in the step S3a, wherein the drying time is 72 hours under the condition that the temperature is controlled to be-10 ℃.
2. Analysis of results
The obtained graphene additive is added into one of the components of the bi-component addition type heat-conducting silica gel, and can be well dispersed in a system as a filler, and after the obtained heat-conducting silica gel is subjected to mixing and curing of the A, B components, as shown in table 1, the heat conductivity coefficient is improved by 10%, and the tensile strength is improved by 15%.
Example 2
Methyl hydrazine was used as a specific reducing agent in this example.
1. Manufacturing process
A preparation method of a graphene additive for a heat-conducting silica gel material comprises the following steps:
s1b: heating the graphene oxide solution to 58 ℃;
s2b: slowly adding a special reducing agent into the graphene oxide solution, and reacting for 24 hours under the water bath condition of 72 ℃;
s3b: and after the reaction is finished, carrying out centrifugal separation on the obtained solution, washing the solution to be neutral, and finally carrying out vacuum drying to obtain graphene additive powder.
Wherein, the special reducing agent in the step S2b is methylhydrazine, and the specific preparation method is as follows:
(2-1) in a synthesis device, 193g of concentrated sulfuric acid (the mass fraction is 98.5%) and 60g of ground urea are added and reacted for 2 hours under the ice bath condition of 15 ℃, and the molar ratio is 2:1;
(2-2) slowly dropwise adding 32g of methanol into a synthesis device, wherein the molar ratio of the methanol to the urea is 1:1, keeping the temperature at 24 ℃ for reaction for 4 hours, after dropwise adding, standing at room temperature for 16 hours, adding ammonia water for neutralizing the pH value to 3-4, filtering and drying to obtain white crystal methylurea;
(2-3) dissolving 6.4g of methylurea in a synthesis device at 15 ℃, controlling the temperature to be 10 ℃, dropwise adding 19ml of ethanol solution containing 6.4g of chlorine into the device, reacting for half an hour at 10 ℃ after dropwise adding, and controlling the molar ratio of the chlorine to the methylurea to be 1.05;
(2-4) under the ice bath condition of 5 ℃, slowly dripping 16.4g of NaOH dissolved in 160ml of water into the device to prepare an aqueous solution, wherein the molar ratio of the NaOH to the methylurea is 4.3:1, the reaction is continuously stirred for half an hour after about one hour, then filtering the reaction solution, and heating the filtrate to obtain a fraction at 80-90 ℃ to obtain the aqueous solution of the methylhydrazine.
The concentration of the graphene oxide solution in the step S1b is 3g/L.
The volume ratio of the graphene oxide solution to the methylhydrazine in the step S2b is 1.
And (3) slowly adding a special reducing agent in the step S2b, wherein the specific dropping speed is 0.1mL/S.
And (3) performing centrifugal separation in the step S3b, wherein the specific centrifugal speed is 8000r/min.
And (3) performing vacuum drying in the step S3b, wherein the drying time is 72 hours under the condition that the temperature is controlled to be-10 ℃.
2. Analysis of results
The obtained graphene additive is added into one of the components of the bi-component addition type heat-conducting silica gel, and can be well dispersed in a system as a filler, and after the obtained heat-conducting silica gel is subjected to mixing and curing of the A, B components, as shown in table 1, the heat conductivity coefficient is improved by 8.5%, and the tensile strength is improved by 12.8%.
Example 3
Octyl hydrazine was used as the specific reducing agent in this example.
1. Manufacturing process
A preparation method of a graphene additive for a heat-conducting silica gel material comprises the following steps:
s1c: heating the graphene oxide solution to 55 ℃;
s2c: slowly adding a special reducing agent into the graphene oxide solution, and reacting for 24 hours under the water bath condition of 75 ℃;
s3c: and after the reaction is finished, carrying out centrifugal separation on the obtained solution, washing the solution to be neutral, and finally carrying out vacuum drying to obtain graphene additive powder.
Wherein, the special reducing agent in the step S2c is octyl hydrazine, and the specific preparation method is as follows:
(3-1) adding 193g of concentrated sulfuric acid (the mass fraction is 98.5%) and 60g of ground urea into a synthesis device, and reacting for 2 hours at 15 ℃ under an ice bath condition, wherein the molar ratio is 2:1;
(3-2) slowly dripping 130g of octanol into the synthesis device, wherein the molar ratio of octanol to urea is 1:1, carrying out heat preservation reaction at 20 ℃ for 4 hours, finishing dripping, standing at room temperature for 16 hours, adding ammonia water to neutralize the pH value to 3-4, and filtering and drying to obtain white crystals Xin Jiniao;
(3-3) dissolving 14.8g Xin Jiniao in ethanol, controlling the temperature to be 15 ℃, dropwise adding 19mL ethanol solution containing 6.4g of chlorine into the device, reacting for half an hour at 15 ℃ after dropwise adding, and controlling the molar ratio of the chlorine to Xin Jiniao to be 1.05;
(3-4) under the ice bath condition of 5 ℃, slowly dripping 16.4g of NaOH into the device to be dissolved in 160mL of water to prepare an aqueous solution, wherein the molar ratio of the NaOH to the Xin Jiniao is 4.8, the dripping is finished within about one hour, continuing stirring for half an hour, then filtering the reaction solution, and heating the filtrate to obtain a fraction of 100-104 ℃ and an aqueous solution of octylhydrazine.
The concentration of the graphene oxide solution in the step S1c is 8g/L.
The volume ratio of the graphene oxide solution to the octylhydrazine in the step S2c is 1.
And (3) slowly adding the special reducing agent in the step S2c, wherein the specific dropping speed is 0.1ml/S.
And (4) performing centrifugal separation in the step (S3 c), wherein the specific centrifugal speed is 10000r/min.
And (3) performing vacuum drying in the step S3c, wherein the drying time is 72 hours under the condition that the temperature is controlled to be-10 ℃.
2. Analysis of results
The obtained graphene additive is added into one of the components of the bi-component addition type heat-conducting silica gel, can be well dispersed in a system as a filler, and after the obtained heat-conducting silica gel is subjected to mixing and curing of the A, B components, as shown in table 1, the heat conductivity coefficient is improved by 6%, and the tensile strength is improved by 16.9%.
Comparative example 1
No graphene additive is added into the bi-component addition type heat-conducting silica gel, and after the obtained heat-conducting silica gel is subjected to mixing and curing of the A, B component, as shown in Table 1, the heat conductivity coefficient and the tensile strength are not ideal.
Comparative example 2
The graphene 1 purchased from the market, which is a graphene product of Nanjing Xiancheng nanomaterial science and technology Limited, is added as a graphene additive into one of the components of the bi-component addition type heat-conducting silica gel, and cannot be well dispersed in a system as a filler, and the system has obvious agglomerated particles, and after the obtained heat-conducting silica gel is mixed and cured by A, B components, as shown in Table 1, the heat conductivity coefficient is improved by only 0.5%, and the tensile strength is reduced by 23.1%.
Comparative example 3
The graphene 2 purchased from the market, which is a product of XG Sciences company, is added as a graphene additive to one of the components of the bi-component addition type heat-conductive silica gel, and cannot be well dispersed in a system as a filler, and the system has obvious agglomerated particles, and after the obtained heat-conductive silica gel is subjected to mixing and curing of A, B components, as shown in table 1, the heat conductivity coefficient is improved by only 1.5%, and the tensile strength is reduced by 17.3%.
TABLE 1 comparison of the properties of thermally conductive silica gels prepared in examples and comparative examples
Wherein the test of the coefficient of the thermal conductivity meter is to use a DTC-300 thermal conductivity meter under the American TA instruments flag; the tensile strength was measured using a universal electronic tensile tester Z003.
The above-described embodiments do not limit the scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the above-described embodiments should be included in the protection scope of the technical solution.
Claims (9)
1. A preparation method of a graphene additive for a heat-conducting silica gel material is characterized in that the graphene additive is graphene powder obtained by reducing a graphene oxide solution by a special reducing agent, and the preparation method of the graphene additive comprises the following steps:
s1: heating the graphene oxide solution to 50-60 ℃;
s2: slowly adding a special reducing agent into the graphene oxide solution, and reacting for 23-25 hours at 65-75 ℃ under the water bath condition;
s3: after the reaction is finished, carrying out centrifugal separation on the obtained solution, washing the solution to be neutral, and finally carrying out vacuum drying to obtain graphene additive powder;
the special reducing agent is R-based hydrazine, wherein R is alkyl of 1-8 and isomers thereof, and the molecular structure of the special reducing agent is as follows:
2. the method as claimed in claim 1, wherein the specific reducing agent comprises one or more of tert-butyl hydrazine, methyl hydrazine and octyl hydrazine.
3. The method for preparing the graphene additive for the heat-conducting silica gel material according to claim 1, wherein the specific reducing agent is prepared by the following steps:
adding concentrated sulfuric acid and urea into a synthesis device, and reacting for 1-3 hours at 15-25 ℃ under an ice bath condition, wherein the molar ratio is 2:1;
II, slowly dripping R alcohol into the synthesis device, wherein the molar ratio of the R alcohol to the urea is 1:1, reacting for 3-5 hours at the temperature of 20-25 ℃, standing for 15-17 hours at room temperature, adding ammonia water to neutralize the pH value to 3-4, filtering and drying to obtain white crystal R-based urea;
III, dissolving R-urea in ethanol, dropwise adding an ethanol solution containing chlorine into the device, and reacting at 14-16 ℃ for 0.2-1 hour after dropwise adding, wherein the molar ratio of the chlorine to the R-urea is 1.05;
and IV, dissolving NaOH in water to prepare an aqueous solution, slowly dripping the aqueous solution into the device, keeping the temperature of 4-6 ℃ for reaction for 0.5-1.5 hours, wherein the molar ratio of the NaOH to the R-based urea is 4.5-5.0, then filtering the reaction solution, and heating the filtrate to obtain a fraction at the temperature of 80-104 ℃ to obtain the special reducing agent R-based hydrazine.
4. The method for preparing the graphene additive for the heat-conducting silica gel material according to claim 3, wherein the specific reducing agent is prepared by a reaction process comprising:
5. the method as claimed in claim 1, wherein the graphene oxide solution is heated to 55 ℃ in S1.
6. The method for preparing the graphene additive for the heat-conducting silica gel material according to claim 1, wherein the volume ratio of the graphene oxide solution to the specific reducing agent in S2 is 1.
7. The method for preparing the graphene additive for the heat-conducting silica gel material according to claim 1, wherein the dropping speed of the specific reducing agent in the S2 is 0.1-0.12mL/S.
8. The method for preparing a graphene additive for a heat-conductive silicone material according to claim 1, wherein the temperature of vacuum drying in S3 is-11 to-9 ℃, and the drying time is 70 to 74 hours.
9. The method as claimed in claim 1, wherein the centrifugation speed of the centrifugation in S3 is 8000-10000r/min.
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