CN114395368B - Double-component modified thermosetting silica gel and preparation method thereof - Google Patents
Double-component modified thermosetting silica gel and preparation method thereof Download PDFInfo
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- CN114395368B CN114395368B CN202210041529.2A CN202210041529A CN114395368B CN 114395368 B CN114395368 B CN 114395368B CN 202210041529 A CN202210041529 A CN 202210041529A CN 114395368 B CN114395368 B CN 114395368B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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Abstract
The application relates to the field of electrical materials, in particular to a double-component modified thermosetting silica gel and a preparation method thereof; the modified thermosetting silica gel comprises: the silica gel comprises a first component silica gel and a second component silica gel, wherein the raw materials of the first component silica gel comprise: a first vinyl polydimethylsiloxane, a first inorganic powder, a silane coupling agent and a platinum catalyst; the raw materials of the second component silica gel comprise: a second vinyl polydimethylsiloxane, a second inorganic powder, a cross-linking agent and a coupling agent; both the first vinyl dimethicone and the second vinyl dimethicone include a terminal vinyl dimethicone a and a terminal vinyl dimethicone B; the method comprises the following steps: mixing and stirring the first component silica gel raw materials to obtain first component silica gel; mixing and stirring the second component silica gel raw materials to obtain second component silica gel; mixing the first component silica gel and the second component silica gel, and stirring to obtain double-component modified thermosetting silica gel; realizing the preparation of the thermosetting silica gel in a non-vacuum environment.
Description
Technical Field
The application relates to the field of electrical materials, in particular to a double-component modified thermosetting silica gel and a preparation method thereof.
Background
Because of its good thermal stability, silica gel is widely used in the electrical field, wherein, organic silica gel has electrical insulation properties, dielectric loss, voltage resistance, arc resistance, corona resistance, volume resistivity, surface resistivity and the like are all among insulating materials, and the electrical properties are little affected by temperature and frequency, so that the organic silica gel is used as an ideal electrical material; besides excellent heat resistance, the organic silica gel has excellent water repellency, and ensures that electrical equipment is used under wet conditions, so that the organic silica gel is generally used as thermosetting silica gel in the field of electrical materials.
However, current heat seal preparation generally involves two aspects: 1. the organic silicon pouring sealant with low hardness, high elasticity, low migration and high heat conductivity can be prepared by adopting the base material, the unilateral vinyl silicone oil, the silane coupling agent, the heat conducting part, the colorant and the catalyst, but the preparation method is complex, and particularly the operation is complex because of the need of vacuumizing and stirring;
2. by adopting hydroxyl-terminated polydimethylsiloxane, side hydrogen-containing silicone oil crosslinking, a terminal hydrogen-containing silicone oil crosslinking agent, nano calcium carbonate, spherical alumina and angular alumina, the silica gel can be prepared, but vacuum defoaming is required, and the operation is more complicated.
Therefore, how to prepare the thermosetting silica gel without vacuum is a technical problem to be solved at present.
Disclosure of Invention
The application provides a double-component modified thermosetting silica gel and a preparation method thereof, which are used for solving the technical problem that the thermosetting silica gel is difficult to prepare in a non-vacuum environment in the prior art.
In a first aspect, the present application provides a two-component modified thermoset silica gel comprising: the silica gel comprises the following raw materials in parts by weight: first vinyl polydimethylsiloxane: 90-120 parts of first inorganic powder: 80-100 parts of silane coupling agent: 1-5 parts of platinum catalyst: 0.05 to 0.1 part;
the raw materials of the second component silica gel comprise: second vinyl polydimethylsiloxane: 100-120 parts of second inorganic powder: 200-250 parts of cross-linking agent: 5-15 parts of coupling agent: 1-5 parts;
wherein the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane both comprise a terminal vinyl polydimethylsiloxane a and a terminal vinyl polydimethylsiloxane B.
Optionally, the weight ratio of the vinyl-terminated polydimethylsiloxane A to the vinyl-terminated polydimethylsiloxane B is (3.2-5.6): 1.
Alternatively, the viscosity of the vinyl-terminated polydimethylsiloxane A is 1500 Pa.s to 1500 Pa.s at 25 ℃, and the viscosity of the vinyl-terminated polydimethylsiloxane B is 5000 Pa.s to 5500 Pa.s at 25 ℃.
Alternatively, the vinyl content of the terminal vinyl polydimethylsiloxane A is from 0.6mol% to 1mol%.
Optionally, the weight ratio of the first component silica gel to the second component silica gel is (0.7-1.3): 1.
Optionally, the first inorganic powder and the second inorganic powder each comprise one or more of fumed silica, alumina, zinc oxide, and magnesium oxide.
Optionally, the first inorganic powder and the second inorganic powder both comprise fumed silica and alumina, and the weight ratio of the fumed silica to the alumina is (0.3-0.8): 1;
the alumina includes single crystal alumina including spherical or ellipsoidal shape;
the fumed silica comprises fumed silica modified by a nitrogen-containing organosilicon compound, and the particle size of the fumed silica is 1 nm-10 nm.
Optionally, the single crystal alumina comprises a mixture of a first single crystal alumina and a second single crystal alumina, and the weight ratio of the first single crystal alumina to the second single crystal alumina is (12-20): 1;
the particle size of the first single crystal alumina is 1-5 mu m, and the particle size of the second single crystal alumina is 10-40 mu m.
Optionally, the raw materials of the second component further comprise hydrogen-containing silicone oil in parts by weight: 5-10 parts of hydrogen-containing silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.2-0.5%, and the weight ratio of the second inorganic powder to the hydrogen-containing silicone oil is (25-30): 1.
In a second aspect, the present application provides a method for preparing a two-component modified thermoset silica gel, the method for preparing the modified thermoset silica gel of the first aspect, the method comprising:
respectively obtaining first vinyl polydimethylsiloxane, first inorganic powder, a silane coupling agent and a platinum catalyst;
mixing the first vinyl polydimethylsiloxane, the first inorganic powder, the silane coupling agent and the platinum catalyst, and stirring to obtain a first component silica gel;
respectively obtaining second vinyl polydimethylsiloxane, second inorganic powder, a cross-linking agent and a coupling agent;
mixing the second vinyl polydimethylsiloxane, the second inorganic powder, the cross-linking agent and the coupling agent, and stirring to obtain a second component silica gel;
and mixing the first component silica gel and the second component silica gel, and stirring to obtain the double-component modified thermosetting silica gel.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the double-component modified thermosetting silica gel provided by the embodiment of the application, the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane comprising the vinyl-terminated polydimethylsiloxane A and the vinyl-terminated polydimethylsiloxane B are adopted, the first component silica gel and the second component silica gel are mixed, the probability of mutual entanglement of polydimethylsiloxane molecular chains can be reduced in the process of post-stirring, the uneven distribution of inorganic powder molecules with larger specific surface energy due to intermolecular or intramolecular interaction force is avoided, the defects of the inside of molecules of the first component silica gel and the inside of molecules of the second component silica gel are optimized, the gas molecules are prevented from escaping difficultly in the stirring process, and the formation of bubbles inside the first component silica gel, the second component silica gel and the thermosetting silica gel can be effectively avoided, the addition of a defoaming agent or vacuum defoaming can be effectively avoided in the preparation process, and the preparation of the thermosetting silica gel is completed in a non-vacuum environment.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to a person skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic flow chart of a method provided in an embodiment of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
The inventive thinking of this application is: the applicant found in experiments that in order to make the stirring between each raw material uniform during the preparation of the first and second component silica gels, the first and second component silica gels will exhibit more bubbles, and during the later mixing of the first and second component silica gels, probably due to the presence of more bubbles, the bond strength of the thermosetting silica gel decreases after a period of time, in particular the use of the thermosetting silica gel has a density of 2.2g/cm or more 3 After bonding and after a period of 200 ℃ treatment, the bonding strength is rapidly reduced, which greatly affects the use, and the applicant unexpectedly found after a series of experimental researches that when the vinyl polydimethylsiloxane comprises the vinyl-terminated polydimethylsiloxane A and the vinyl-terminated polydimethylsiloxane B, and the weight ratio of the vinyl-terminated polydimethylsiloxane A to the vinyl-terminated polydimethylsiloxane B is (3.2-5.6): 1, the viscosity of the vinyl-terminated polydimethylsiloxane A is 1500 Pa.s to 160 Pa.s at 25 ℃, the vinyl content is 0.6mol% to 1mol%, and the viscosity of the vinyl-terminated polydimethylsiloxane B is 5000 Pa.s to 5500 Pa.s at 25 ℃, the prepared thermosetting silica gel has the specific density of more than 2.2g/cm3After the graphite plates are bonded, even after the graphite plates are treated for a period of time at 200 ℃, the bonding strength of the graphite plates is not obviously reduced, and possible reasons are that in the process of mixing and stirring the first component silica gel and the second component silica gel respectively by utilizing the vinyl-terminated polydimethylsiloxane with specific viscosity and vinyl, the probability of mutual entanglement of the molecular chains of the polydimethylsiloxane is reduced, the uneven distribution of inorganic powder molecules with larger specific surface energy due to intermolecular or intramolecular interaction force is avoided, and the defects inside the molecules of the first component and the molecules of the second component are influenced, so that gas molecules are prevented from escaping very difficultly in the stirring process, and the defoaming treatment is avoided. Furthermore, the suitable crosslinking points, after mixing between the first and second component silica gels obtained by the vinyl terminated polydimethylsiloxane a and vinyl terminated polydimethylsiloxane B in the present application, allow to obtain a suitable crosslinking density sufficient to maintain the molecular attraction between the lamellar graphite molecules at high temperature.
In one embodiment of the present application, there is provided a two-component modified thermoset silica gel comprising: the silica gel comprises the following raw materials in parts by weight: first vinyl polydimethylsiloxane: 90-120 parts of first inorganic powder: 80-100 parts of silane coupling agent: 1-5 parts of platinum catalyst: 0.05 to 0.1 part;
the raw materials of the second component silica gel comprise: second vinyl polydimethylsiloxane: 100-120 parts of second inorganic powder: 200-250 parts of cross-linking agent: 5-15 parts of coupling agent: 1-5 parts;
wherein the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane both comprise a terminal vinyl polydimethylsiloxane a and a terminal vinyl polydimethylsiloxane B;
the silane coupling agent can be gamma-aminopropyl triethoxysilane, and the cross-linking agent can be tetraethoxysilane; the content of effective platinum in the platinum catalyst is 1000 ppm-5000 ppm.
In the application, in the first component silica gel, the weight part of the first vinyl polydimethylsiloxane is 90-120 parts, and the positive effects of ensuring that the terminal vinyl polydimethylsiloxane A and the terminal vinyl polydimethylsiloxane B in the first vinyl polydimethylsiloxane can fully play a role and ensuring that bubbles in the first component silica gel cannot be formed are that the weight part is within the range of the weight part; when the value of the weight portion is larger than the end point maximum value of the range, the adverse effect caused by the excessive first vinyl polydimethylsiloxane is that raw materials are wasted, and when the value of the weight portion is smaller than the end point minimum value of the range, the adverse effect caused by the excessively low first vinyl polydimethylsiloxane is that the content of the terminal vinyl polydimethylsiloxane A and the terminal vinyl polydimethylsiloxane B is insufficient, so that bubbles exist in the first component silica gel, and the performance of the thermosetting silica gel is affected.
The weight part of the first inorganic powder is 80-100 parts, and the positive effect is that in the value range of the weight part, the reduction of the final filling material of the thermosetting silica gel caused by the larger viscosity of the first vinyl polydimethylsiloxane can be prevented, so that the filling rate of the thermosetting silica gel is ensured to be more than 50%; when the value of the weight portion is larger than the end value of the range, the adverse effect caused by excessive inorganic powder is that particles in the heat-seal silica gel are increased to affect the elasticity of the heat-seal silica gel, and when the value of the weight portion is smaller than the end minimum value of the range, the adverse effect caused by the fact that the content of the inorganic powder is too low to ensure that the filling rate of the heat-seal silica gel is more than 50%.
The silane coupling agent has the positive effects that the silane coupling agent can fully bond all raw materials in the first component silica gel and the second component silica gel within the value range of 1-5 parts by weight, and can ensure the high water resistance of the thermosetting silica gel and enhance the adhesiveness of the thermosetting silica gel; when the value of the weight fraction is larger than the end point maximum value of the range, the adverse effect that the excessive silane coupling agent will increase the viscosity of the thermosetting silica gel to cause the reduction of the filling rate of the thermosetting silica gel will result, and when the value of the weight fraction is smaller than the end point minimum value of the range, the adverse effect that the silane coupling agent which is too low will not sufficiently bond the raw materials in the first component silica gel and the second component silica gel, and the water resistance of the thermosetting silica gel and the improvement of the adhesiveness to the thermosetting silica gel cannot be effectively ensured.
The weight part of the platinum catalyst is 0.05-0.1 part, and the positive effects of the platinum catalyst are that in the weight part range, the platinum catalyst can effectively catalyze hydrogen-containing silicone oil, so that the platinum catalyst can react with first vinyl polydimethylsiloxane and second vinyl polydimethylsiloxane to obtain a cross-linked structure with proper cross-linking points and cross-linking density, the hydrogen permeability coefficient of the obtained silica gel molecules is lower, and the first inorganic powder and the second inorganic powder can be bound in the cross-linked structure; when the weight fraction is greater than the end point maximum value of the range, the adverse effect caused by the excessively high platinum catalyst will result in waste of raw materials, and when the weight fraction is less than the end point minimum value of the range, the adverse effect caused by the excessively low platinum catalyst will not provide effective catalytic effect, so that the hydrogen-containing silicone oil cannot react with the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane, and the formation of the cross-linked structure of the thermosetting silicone is affected.
In the second component silica gel, the weight part of the second vinyl polydimethylsiloxane is 100-120 parts, and the positive effects of the weight part range are that the terminal vinyl polydimethylsiloxane A and the terminal vinyl polydimethylsiloxane B in the second vinyl polydimethylsiloxane can be ensured to fully play roles, and the bubbles in the second component silica gel can not be formed; when the value of the weight portion is larger than the end point maximum value of the range, the adverse effect caused by the excessive second vinyl polydimethylsiloxane is that raw materials are wasted, and when the value of the weight portion is smaller than the end point minimum value of the range, the adverse effect caused by the excessively low second vinyl polydimethylsiloxane is that the content of the terminal vinyl polydimethylsiloxane A and the terminal vinyl polydimethylsiloxane B is insufficient, so that bubbles exist in the second component silica gel, and the performance of the thermosetting silica gel is affected.
The weight part of the second inorganic powder is 200-250, the positive effect is in the value range of the weight part, can prevent the final filler of the thermosetting silica gel from being reduced due to the larger viscosity of the second vinyl polydimethylsiloxane, thereby ensuring the filling rate of the thermosetting silica gel to be more than 50%; when the value of the weight portion is larger than the end value of the range, the adverse effect caused by excessive inorganic powder is that particles in the heat-seal silica gel are increased to affect the elasticity of the heat-seal silica gel, and when the value of the weight portion is smaller than the end minimum value of the range, the adverse effect caused by the fact that the content of the inorganic powder is too low to ensure that the filling rate of the heat-seal silica gel is more than 50%.
The cross-linking agent has the positive effects that in the range of 5-15 parts by weight, the cross-linking agent can be ensured to fully react with the second vinyl polydimethylsiloxane, the second inorganic powder and the coupling agent, so that the thermosetting silica gel with uniform performance can be obtained; when the weight fraction is larger than the end point maximum of the range, the adverse effect will be
The coupling agent has the positive effects that the coupling agent can ensure that the coupling agent fully adheres all raw materials in the second component silica gel and enhances the adhesion of the thermosetting silica gel within the value range of 1-5 parts by weight; when the value of the weight portion is larger than the end point maximum value of the range, the adverse effect caused by the excessive coupling agent is that the viscosity of the thermosetting silica gel is increased, so that the filling rate of the thermosetting silica gel is reduced, and when the value of the weight portion is smaller than the end point minimum value of the range, the adverse effect caused by the excessively low coupling agent is that the raw materials in the second component silica gel cannot be sufficiently adhered, and the adhesiveness of the thermosetting silica gel cannot be effectively ensured to be improved.
In some alternative embodiments, the weight ratio of the terminal vinyl dimethicone A to the terminal vinyl dimethicone B is (3.2 to 5.6): 1.
In the application, the weight ratio of the terminal vinyl polydimethylsiloxane A to the terminal vinyl polydimethylsiloxane B is (3.2-5.6), and the positive effect of 1 is that in the weight ratio range, the terminal vinyl polydimethylsiloxane A and the terminal vinyl polydimethylsiloxane B with different viscosities can be ensured to be fully mixed, so that the viscosities of the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane are ensured to be in a proper range, the filling rate of the thermosetting silica gel is ensured to be in a reasonable range, and meanwhile, the first component silica gel, the second component silica gel and bubbles inside the thermosetting silica gel can be effectively avoided; when the weight ratio is greater than or less than the end value of the range, the viscosity of the first and second vinyl polydimethylsiloxanes is not in the proper range, so that the filling rate of the thermosetting silica gel is insufficient, and small bubbles are generated in the first and second component silica gels and the thermosetting silica gel.
In some alternative embodiments, the vinyl-terminated polydimethylsiloxane a has a viscosity of 1500mpa.s to 1500mpa.s at 25 ℃ and the vinyl-terminated polydimethylsiloxane B has a viscosity of 5000mpa.s to 5500 pa.s at 25 ℃.
In the application, the viscosity of the vinyl-terminated polydimethylsiloxane A at 25 ℃ is 1500 to 160 Pa.s, and the viscosity of the vinyl-terminated polydimethylsiloxane B at 25 ℃ is 5000 to 5500 Pa.s, so that the viscosity of the first vinyl polydimethylsiloxane and the viscosity of the second vinyl polydimethylsiloxane are maintained in a proper range, the long-time stability of the bonding degree is ensured, the operation time is prolonged, and the formation of bubbles in the first component silica gel, the second component silica gel and the thermosetting silica gel can be effectively avoided; when the viscosity is greater than or less than the end value of the range, the viscosity of the first and second vinyl polydimethylsiloxanes is unstable, so that the operation time cannot be ensured, and the formation of bubbles inside the first and second component silica gels and the thermosetting silica gel is caused.
In some alternative embodiments, the vinyl-terminated polydimethylsiloxane a has a vinyl content of from 0.6mol% to 1mol%.
In the application, the vinyl content of the vinyl-terminated polydimethylsiloxane A is 0.6 to 1mol percent, and the positive effect is that the probability of mutual entanglement of polydimethylsiloxane molecular chains can be reduced within the content range, so that the formation of bubbles in the first component silica gel, the second component silica gel and the thermosetting silica gel can be effectively avoided; when the value of the content is larger than or smaller than the end value of the range, the mutual entanglement probability of the polydimethylsiloxane molecular chains is influenced, the uneven distribution of inorganic powder molecules with larger specific surface energy due to intermolecular or intramolecular interaction force cannot be avoided, the intramolecular defect of the first component silica gel and the intramolecular defect of the second component silica gel are further influenced, and the gas molecules are difficult to escape in the stirring process, so that the first component silica gel, the second component silica gel and the bubbles inside the thermosetting silica gel are formed.
In some alternative embodiments, the weight ratio of the first component silica gel to the second component silica gel is (0.7 to 1.3): 1.
In the application, the weight ratio of the first component silica gel to the second component silica gel is (0.7-1.3), and the positive effect of 1 is that the mixing of the raw materials of the first component silica gel and the second component silica gel can be ensured within the weight ratio range, and the stirring is sufficient, so that the formation of bubbles in the first component silica gel, the second component silica gel and the thermosetting silica gel can be avoided; when the weight ratio is greater than or less than the end value of the range, the adverse effect will be that the first and second silica gels cannot be sufficiently mixed, resulting in formation of bubbles inside the first and second silica gels and the thermosetting silica gel.
In some alternative embodiments, the first inorganic powder and the second inorganic powder each comprise one or more of fumed silica, alumina, zinc oxide, and magnesium oxide.
In some alternative embodiments, the first inorganic powder and the second inorganic powder each comprise fumed silica and alumina, the weight ratio of fumed silica to alumina being (0.3 to 0.8): 1;
the alumina includes single crystal alumina including spherical or ellipsoidal shape;
the fumed silica comprises fumed silica modified by a nitrogen-containing organosilicon compound, and the particle size of the fumed silica is 1 nm-10 nm.
In the application, the weight ratio of the fumed silica to the alumina is (0.3-0.8): 1 has the positive effects that the particles of the fumed silica and the alumina can be matched and promoted, and the interpenetrating network formed by the silicon hydroxyl groups in the low fumed silica can be maintained at a proper level by utilizing the specific shape of the alumina, so that the filling rate of inorganic powder is ensured, and the filling material of the thermosetting silica gel is ensured to be in a reasonable range; when the weight ratio is larger or smaller than the end value of the range, the balance of the gas phase silicon dioxide and the alumina is caused, so that the filling rate of the inorganic powder is affected, and the filling material of the thermosetting silica gel cannot be ensured to be in a reasonable range.
The particle size of the fumed silica is 1 nm-10 nm, and the fumed silica has the positive effects that a proper interpenetrating network can be formed within the particle size range, and meanwhile, the mutual coordination and promotion between the fumed silica and the alumina particles can be ensured, so that the filling rate of inorganic powder is ensured; when the value of the particle diameter is larger or smaller than the end value of the range, the mutual coordination between the particles of the fumed silica and the alumina is affected, so that the filling rate of the inorganic powder cannot be ensured.
In some alternative embodiments, the single crystal alumina comprises a mixture of a first single crystal alumina and a second single crystal alumina, the ratio by weight of the first single crystal alumina to the second single crystal alumina being (12-20): 1;
the particle size of the first single crystal alumina is 1-5 mu m, and the particle size of the second single crystal alumina is 10-40 mu m.
In the application, the weight ratio of the first single crystal alumina to the second single crystal alumina is (12-20): 1 has the positive effects that in the weight ratio range, a large number of trigonal systems can be ensured to be contained in the alumina, meanwhile, oxygen ions are approximately densely packed in a hexagonal manner, and the symmetry of the crystals is low, so that an interpenetrating network formed by silicon hydroxyl groups in fumed silica can be reduced, the interpenetrating network structure is maintained at a proper level, and the filling rate of thermosetting silica gel is improved; when the weight ratio is larger or smaller than the end value of the range, the trigonal system content in the alumina is unstable, and the stability of the filling rate of the thermosetting silica gel cannot be ensured.
The particle size of the first single crystal alumina is 1-5 mu m, and the particle size of the second single crystal alumina is 10-40 mu m, so that the mutual coordination between the particles of the fumed silica and the alumina can be further promoted by limiting the particle sizes of the two single crystal aluminas, the interpenetrating network formed by the silicon hydroxyl groups in the fumed silica can be effectively reduced, the interpenetrating network structure is maintained at a proper level, and the filling rate of the thermosetting silica gel is further improved; when the value of the particle size is larger or smaller than the end value of the range, the particles of the fumed silica and the alumina are mutually matched, so that the interpenetrating network structure cannot be maintained at a proper level, and the filling rate of the thermosetting silica gel cannot be improved.
In some alternative embodiments, the raw materials of the second component further include hydrogen-containing silicone oil in parts by weight: 5-10 parts of hydrogen-containing silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.2-0.5%, and the weight ratio of the second inorganic powder to the hydrogen-containing silicone oil is (25-30): 1, wherein the hydrogen-containing silicone oil can be side hydrogen-containing silicone oil.
In the application, the hydrogen-containing silicone oil has the positive effects that the hydrogen-containing silicone oil can react with the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane under the catalysis of a platinum catalyst within the range of 5-10 parts by weight, so that a cross-linked structure with proper cross-linking points and cross-linking density is obtained, the hydrogen permeability coefficient of the obtained silica gel molecule is lower, and the first inorganic powder and the second inorganic powder can be bound in the cross-linked structure, so that the filler of the inorganic powder is increased; when the weight fraction of the hydrogen-containing silicone oil is larger or smaller than the end value of the range, the densities of the first component silica gel and the second component silica gel are influenced, so that bubbles in the first component silica gel and the second component silica gel are formed.
The positive effect of the hydrogen content of the hydrogen-containing silicone oil being 0.2-0.5% is that the hydrogen permeability coefficient of the molecules of the obtained thermosetting silicone gel is lower in the value range of the hydrogen content, so that the water resistance of the thermosetting silicone gel can be ensured; when the hydrogen content is larger or smaller than the end value of the range, the hydrogen permeability coefficient of the molecules of the thermosetting adhesive is unstable, and the water resistance of the thermosetting adhesive cannot be effectively ensured.
In one embodiment of the present application, as shown in fig. 1, there is provided a method for preparing a two-component modified thermoset silica gel, the method for preparing the modified thermoset silica gel of the first aspect, the method comprising:
s1, respectively obtaining first vinyl polydimethylsiloxane, first inorganic powder, a silane coupling agent and a platinum catalyst;
s2, mixing the first vinyl polydimethylsiloxane, the first inorganic powder, the silane coupling agent and the platinum catalyst, and stirring to obtain a first component silica gel;
s3, respectively obtaining second vinyl polydimethylsiloxane, second inorganic powder, a cross-linking agent and a coupling agent;
s4, mixing the second vinyl polydimethylsiloxane, the second inorganic powder, the cross-linking agent and the coupling agent, and stirring to obtain a second component silica gel;
s5, mixing the first component silica gel and the second component silica gel, and stirring to obtain the double-component modified thermosetting silica gel.
Example 1
A two-component modified thermoset silica gel comprising: the silica gel comprises the following raw materials in parts by weight: first vinyl polydimethylsiloxane: 90 parts of a first inorganic powder: 80 parts of silane coupling agent: 1 part and platinum catalyst: 0.05 parts;
the raw materials of the second component silica gel comprise: second vinyl polydimethylsiloxane: 100 parts of a second inorganic powder: 250 parts of cross-linking agent: 5 parts of coupling agent: 1 part;
wherein the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane both comprise a terminal vinyl polydimethylsiloxane A and a terminal vinyl polydimethylsiloxane B; the silane coupling agent is gamma-aminopropyl triethoxysilane, and the cross-linking agent is tetraethoxysilane; the platinum catalyst had an effective platinum content of 3000ppm and was purchased from the Dongguan Miteng rubber and plastic materials Co.
The weight ratio of vinyl terminated polydimethylsiloxane A to vinyl terminated polydimethylsiloxane B was 3.2:1.
The viscosity of the terminal vinyl polydimethylsiloxane A at 25 ℃ is 1500mPa.s, and the viscosity of the terminal vinyl polydimethylsiloxane B at 25 ℃ is 5200mPa.s, which are available from Ningbo Ruo He Gao New Material technologies Co., ltd and are available under the trademark RH-Vi1304.
Vinyl-terminated polydimethylsiloxane A had a vinyl content of 0.8mol% and was purchased from Dongguan Huashi technology Co., ltd.
The weight ratio of the first component silica gel to the second component silica gel is 1:1.
The first inorganic powder and the second inorganic powder both comprise fumed silica and alumina, and the weight ratio of the fumed silica to the alumina is 0.3:1;
the alumina comprises single crystal alumina which is ellipsoidal;
the fumed silica comprises fumed silica modified by a nitrogenous organosilicon compound, the particle size of the fumed silica is 7nm, the fumed silica is hexamethyldisilazane modified fumed silica, and the fumed silica is purchased from Guangzhou Jinkai chemical industry Co., ltd and is named Desolid AEROSIL R812S.
The single crystal alumina comprises a mixture of a first single crystal alumina and a second single crystal alumina, available from Guangdong chemical materials science, inc., in a weight ratio of 15:1;
the particle size of the first single crystal alumina was 2.5. Mu.m, and the particle size of the second single crystal alumina was 10. Mu.m.
The raw materials of the second component also comprise hydrogen silicone oil in parts by weight: 10 parts of hydrogen-containing silicone oil with the hydrogen content of 0.35-0.37 percent is purchased from Ningbo Ruo He new material science and technology Co., ltd, and the brand is RH-H536.
As shown in fig. 1, a method for preparing a two-component modified thermosetting silica gel, which is used for preparing the modified thermosetting silica gel, comprises the following steps:
s1, respectively obtaining first vinyl polydimethylsiloxane, first inorganic powder, a silane coupling agent and a platinum catalyst;
s2, mixing the first vinyl polydimethylsiloxane, the first inorganic powder, the silane coupling agent and the platinum catalyst, and stirring to obtain a first component silica gel;
s3, respectively obtaining second vinyl polydimethylsiloxane, second inorganic powder, a cross-linking agent and a coupling agent;
s4, mixing the second vinyl polydimethylsiloxane, the second inorganic powder, the cross-linking agent and the coupling agent, and stirring to obtain a second component silica gel;
s5, mixing the first component silica gel and the second component silica gel, and stirring to obtain the double-component modified thermosetting silica gel.
Example 2
Comparing example 2 with example 1, example 2 differs from example 1 in that:
the silica gel comprises the following raw materials in parts by weight: first vinyl polydimethylsiloxane: 120 parts of first inorganic powder: 100 parts of silane coupling agent: 5 parts of platinum catalyst: 0.1 part;
the raw materials of the second component silica gel comprise: second vinyl polydimethylsiloxane: 120 parts of a second inorganic powder: 250 parts of cross-linking agent: 15 parts of coupling agent: 5 parts;
wherein the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane both comprise a terminal vinyl polydimethylsiloxane A and a terminal vinyl polydimethylsiloxane B;
the weight ratio of vinyl terminated polydimethylsiloxane A to vinyl terminated polydimethylsiloxane B was 5.6:1.
The viscosity of the vinyl-terminated polydimethylsiloxane A was 1550mPa.s at 25℃and the viscosity of the vinyl-terminated polydimethylsiloxane B was 5000mPa.s at 25 ℃.
The weight ratio of the first component silica gel to the second component silica gel is 1:1.
The first inorganic powder and the second inorganic powder each include one or more of fumed silica, alumina, zinc oxide, and magnesium oxide.
The first inorganic powder and the second inorganic powder both comprise fumed silica and alumina, and the weight ratio of the fumed silica to the alumina is 0.8:1;
the single crystal alumina comprises a mixture of a first single crystal alumina and a second single crystal alumina, and the weight ratio of the first single crystal alumina to the second single crystal alumina is 12:1;
the particle size of the first single crystal alumina was 2.5. Mu.m, and the particle size of the second single crystal alumina was 10. Mu.m.
The raw materials of the second component also comprise hydrogen silicone oil in parts by weight: 8.3 parts of hydrogen-containing silicone oil with hydrogen content of 0.2 to 0.5 percent.
Example 3
Comparing example 3 with example 1, example 3 differs from example 1 in that:
the silica gel comprises the following raw materials in parts by weight: first vinyl polydimethylsiloxane: 100 parts of a first inorganic powder: 100 parts of silane coupling agent: 3 parts of platinum catalyst: 0.08 parts;
the raw materials of the second component silica gel comprise: second vinyl polydimethylsiloxane: 110 parts of a second inorganic powder: 220 parts of cross-linking agent: 10 parts of coupling agent: 5 parts;
wherein the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane both comprise a terminal vinyl polydimethylsiloxane A and a terminal vinyl polydimethylsiloxane B.
The weight ratio of vinyl terminated polydimethylsiloxane A to vinyl terminated polydimethylsiloxane B was 4.3:1.
The viscosity of the vinyl-terminated polydimethylsiloxane A was 160 Pa.s at 25℃and the viscosity of the vinyl-terminated polydimethylsiloxane B was 5500 Pa.s at 25 ℃.
The weight ratio of the first component silica gel to the second component silica gel is 1:1.
The first inorganic powder and the second inorganic powder both comprise fumed silica and alumina, and the weight ratio of the fumed silica to the alumina is 0.5:1;
the single crystal alumina comprises a mixture of a first single crystal alumina and a second single crystal alumina, the weight ratio of the first single crystal alumina to the second single crystal alumina being 20:1.
The raw materials of the second component also comprise hydrogen silicone oil in parts by weight: 8 parts.
Comparative example 1
Comparative example 1 and example 3 are compared, and the difference between comparative example 1 and example 3 is that:
the viscosity of the vinyl-terminated polydimethylsiloxane B at 25 ℃ is 475Pa.s to 525Pa.s.
Comparative example 2
Comparative example 2 and example 3 are compared, and the difference between comparative example 2 and example 3 is that:
the inorganic powder is fumed silica.
In practice, it was found that the fumed silica of comparative example 2 was not dispersed in the organic material during the mixing and stirring process, and therefore could not be used.
1. Related experiment 1:
the thermosets obtained in examples 1-3 and comparative examples 1-2 were collected, respectively, while the appearance air bubble properties were recorded, and the results are shown in Table 1.
Test method of related experiment: and respectively observing the first component silica gel, the second component silica gel and the thermosetting silica gel finished product, if no bubble exists in the first component silica gel, marking the first component silica gel, the second component silica gel and the thermosetting silica gel as qualified, and if at least one substance has bubbles, marking the first component silica gel, the second component silica gel and the thermosetting silica gel as unqualified.
TABLE 1
Specific analysis of table 1:
from the data of examples 1-3, it can be seen that:
as can be seen from table 1, when the formulation and the proportion of the thermosetting silica gel as defined in the present application are adopted, the formation of bubbles in each intermediate product and the final product in the preparation stage can be effectively avoided.
From the data of comparative example 1, it can be seen that:
if a lower viscosity terminal vinyl polydimethylsiloxane B is used, i.e., a terminal vinyl polydimethylsiloxane B within the limits of the present application is not used, this will result in the formation of bubbles in each intermediate and final product during the preparation stage.
2. Related experiment 2:
the two-component modified thermosetting silica gel obtained in example 3 was tested for physical properties and the results are shown in Table 2.
Test method of related experiment: detection according to GB/T7123.1-2015
TABLE 2
| Viscosity at 25℃mPas | 45000 |
| The operation time is 25 ℃ and day | 3 |
As can be seen from table 2, the thermosetting silica gel provided in the present application has a high viscosity, but the filling ratio of the first component silica gel and the second component silica gel is 50% or more.
3. Related experiment 3:
the two-component modified thermosetting silica gel obtained in example 3 was used in a density of 2.2g/cm 3 After the graphite sheet was press-molded and cured at 130℃for 100 seconds, the physical properties and chemical properties were measured, respectively, and the measurement results are shown in tables 3 and 4.
TABLE 3 Table 3
TABLE 4 Table 4
As can be seen from tables 3 and 4, the thermosetting silica gel obtained in the present application has moisture resistance at 85 ℃ and 85% humidity, and it also has high strength, low modulus, high rebound resilience and good shock resistance.
One or more technical solutions in the embodiments of the present application at least further have the following technical effects or advantages:
(1) In the modified thermosetting silica gel provided by the application, through using the terminal vinyl polydimethylsiloxane A and the terminal vinyl polydimethylsiloxane B of specific types and proportions, the formation of bubbles inside the first component silica gel, the second component silica gel and the thermosetting silica gel is avoided, the difficult problem that a defoaming agent is required to be added or vacuum defoaming is solved in the prior art, the operation flow is simplified, and the working efficiency is improved.
(2) In the modified thermosetting silica gel provided by the application, the problem of reduced filling rate caused by vinyl polydimethylsiloxane and fumed silica with larger viscosity is solved by adopting the two single crystal alumina with specific particle sizes, so that the filling rate of the first component silica gel and the second component silica gel in the application reaches more than 50%;
(3) In the modified thermosetting silica gel provided by the application, the specific hydrogen-containing silicone oil is adopted to be matched with the platinum catalyst and the first inorganic powder and the second inorganic powder, so that the moisture resistance of the thermosetting silica gel under the conditions of 85 ℃ and 85% humidity is improved;
(4) In the modified thermosetting silica gel provided by the application, the obtained double-component modified thermosetting silica gel has the advantages of high strength, low modulus, high rebound resilience, better shock resistance, long operable time, rapid solidification and no pollution to the use environment.
It should be noted that in this document, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The foregoing is only a specific embodiment of the invention to enable those skilled in the art to understand or practice the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A two-component modified thermoset silica gel, the modified thermoset silica gel comprising: the silica gel comprises the following raw materials in parts by weight: first vinyl polydimethylsiloxane: 90-120 parts of first inorganic powder: 80-100 parts of silane coupling agent: 1-5 parts of platinum catalyst: 0.05 to 0.1 part;
the raw materials of the second component silica gel comprise: second vinyl polydimethylsiloxane: 100-120 parts of second inorganic powder: 200-250 parts of cross-linking agent: 5-15 parts of coupling agent: 1-5 parts;
wherein the first vinyl polydimethylsiloxane and the second vinyl polydimethylsiloxane both comprise a terminal vinyl polydimethylsiloxane a and a terminal vinyl polydimethylsiloxane B; the weight ratio of the vinyl-terminated polydimethylsiloxane A to the vinyl-terminated polydimethylsiloxane B is (3.2-5.6): 1;
the viscosity of the vinyl-terminated polydimethylsiloxane A at 25 ℃ is 1500 Pa.s-160 Pa.s, and the viscosity of the vinyl-terminated polydimethylsiloxane B at 25 ℃ is 5000 Pa.s-5500 Pa.s;
the first inorganic powder and the second inorganic powder both comprise fumed silica and alumina, and the weight ratio of the fumed silica to the alumina is (0.3-0.8): 1.
2. The modified thermoset silica gel of claim 1, wherein the vinyl-terminated polydimethylsiloxane a has a vinyl content of from 0.6mol% to 1mol%.
3. The modified thermoset silica gel of claim 1, wherein the weight ratio of the first component silica gel to the second component silica gel is (0.7 to 1.3): 1.
4. The modified thermoset silica gel of claim 1,
the alumina includes single crystal alumina including spherical or ellipsoidal shape;
the fumed silica comprises fumed silica modified by a nitrogen-containing organosilicon compound, and the particle size of the fumed silica is 1 nm-10 nm.
5. The modified thermoset silica gel of claim 4, wherein the single crystal alumina comprises a mixture of a first single crystal alumina and a second single crystal alumina, the weight ratio of the first single crystal alumina to the second single crystal alumina being (12-20): 1;
the particle size of the first single crystal alumina is 1-5 mu m, and the particle size of the second single crystal alumina is 10-40 mu m.
6. The modified thermoset silica gel of claim 1, wherein the second component further comprises, in parts by weight, a hydrogen containing silicone oil: 5-10 parts of hydrogen-containing silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.2-0.5%, and the weight ratio of the second inorganic powder to the hydrogen-containing silicone oil is (25-30): 1.
7. A process for preparing a two-component modified thermoset silica gel according to any one of claims 1 to 6, comprising:
respectively obtaining first vinyl polydimethylsiloxane, first inorganic powder, a silane coupling agent and a platinum catalyst;
mixing the first vinyl polydimethylsiloxane, the first inorganic powder, the silane coupling agent and the platinum catalyst, and stirring to obtain a first component silica gel;
respectively obtaining second vinyl polydimethylsiloxane, second inorganic powder, a cross-linking agent and a coupling agent;
mixing the second vinyl polydimethylsiloxane, the second inorganic powder, the cross-linking agent and the coupling agent, and stirring to obtain a second component silica gel;
and mixing the first component silica gel and the second component silica gel, and stirring to obtain the double-component modified thermosetting silica gel.
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| US5082886A (en) * | 1989-08-28 | 1992-01-21 | General Electric Company | Low compression set, oil and fuel resistant, liquid injection moldable, silicone rubber |
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