CN113308021B - Preparation method of silicon micro powder for epoxy resin system - Google Patents
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Abstract
The invention relates to a preparation method for silicon powder in an epoxy resin system, which adopts a silane coupling agent for two-step modification, namely, firstly adopting gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane to carry out dry modification on the silicon powder to obtain primary modified silicon powder, and then adopting N-phenyl-gamma-aminopropyl trimethoxy silane to carry out wet modification on the primary modified silicon powder to obtain the modified silicon powder. The method has simple process, and the prepared modified silica powder has high activation degree, good hydrophobicity and low surface hydroxyl, makes up the characteristic of poor hydrophobicity of the single modified silica powder of the epoxy coupling agent, greatly reduces the viscosity when being applied to an epoxy resin system, and greatly improves the dispersibility in resin.
Description
Technical Field
The invention belongs to the field of composite material preparation, and relates to a preparation method of silica powder for an epoxy resin system.
Background
Compared with other common inorganic fillers such as attapulgite and the like, the silicon micropowder has better mechanical properties, heat resistance, dispersibility, electrical properties and the like. However, when the silica powder is directly used as an organic phase filler, the material performance is not ideal in many cases, mainly because the existence of the surface silicon hydroxyl groups causes poor affinity with a high molecular organic material, and the silica powder is dispersed unevenly or even agglomerated when used as the filler, so that the material performance is greatly influenced, and therefore, the silica powder needs to be subjected to surface modification.
Disclosure of Invention
The invention aims to provide a method for modifying silicon micropowder of an epoxy resin system. The method combines dry modification and wet modification to obtain the product with good modification effect.
The technical scheme for realizing the purpose of the invention is as follows: a preparation method of silicon micropowder for an epoxy resin system comprises the following steps: adopting silane coupling agent to modify in two steps, namely adopting prehydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane to modify by a mixer dry method at a proper temperature to obtain primary modified silicon micropowder; and then carrying out wet modification on the prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane by using a stirrer at a proper temperature to obtain secondary modified silicon micropowder.
Preferably, the technical scheme of the preparation method for the epoxy resin system silicon micropowder comprises the following steps: the method for hydrolyzing the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane comprises the following steps: mixing a silane coupling agent gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, ethanol and water for hydrolysis reaction, wherein the mass ratio of the silane coupling agent to the isopropanol to the water is 1:0.8-1.2:1.8 to 2.2, the hydrolysis time is 20 to 30min, and the hydrolysis pH is 4.0 to 5.0. Further preferably, the hydrolysis time is 20min and the hydrolysis pH is 4.0; the mass ratio of the silane coupling agent to the isopropyl alcohol to the water is 1.
Preferably, the technical scheme of the preparation method for the epoxy resin system silicon micropowder comprises the following steps: the method for hydrolyzing the N-phenyl-gamma-aminopropyl trimethoxy silane comprises the following steps: mixing N-phenyl-gamma-aminopropyltrimethoxysilane, isopropanol and water for hydrolysis reaction, wherein the mass ratio of the N-phenyl-gamma-aminopropyltrimethoxysilane to the isopropanol to the water is 1:0.8-1.2:1.8-2.2, wherein the hydrolysis time is 20-30min, and the pH value of the hydrolysis is 7.5-8.5. Further preferably: the mass ratio of the N-phenyl-gamma-aminopropyltrimethoxysilane to the isopropanol to the water is 1.
Preferably, the technical scheme of the preparation method for the epoxy resin system silicon micropowder comprises the following steps: the dry modification temperature is 140 to 150 ℃, and the modification time is 15 to 25min; the wet modification temperature is 80-90 ℃, and the modification time is 55-65min. Further preferably: the dry modification temperature is 150 ℃, and the modification time is 20min; the wet modification temperature is 90 ℃, and the modification time is 60min.
Preferably, the technical scheme of the preparation method for the epoxy resin system silicon micropowder comprises the following steps: in the dry modification and the wet modification, the addition amount of the silane coupling agent is 4-6 per mill, preferably 5 per mill of the mass of the silicon micropowder respectively.
Preferably, the technical scheme of the preparation method for the epoxy resin system silicon micropowder comprises the following steps: the method comprises the following specific steps:
(1) And (3) hydrolysis reaction: mixing a silane coupling agent gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, ethanol and water for hydrolysis reaction to obtain silane coupling agent hydrolysate, and adjusting the pH of the hydrolysate to be 4.0 to 5.0;
mixing a silane coupling agent N-phenyl-gamma-aminopropyltrimethoxysilane, isopropanol and water for hydrolysis reaction to obtain a silane coupling agent hydrolysate, and adjusting the pH of the hydrolysate to 7.5 to 8.5;
(2) Modification reaction: mixing the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane hydrolysate with silicon micropowder, and performing dry modification at the temperature of 140-150 ℃ by using a high-speed mixer to obtain primary modified silicon micropowder; and carrying out wet modification on the N-phenyl-gamma-aminopropyltrimethoxysilane hydrolysate and the primary modified silicon micro powder at the temperature of between 80 and 90 ℃ by using a high-speed mixer to obtain secondary modified silicon micro powder.
Compared with the prior art, the invention has the following advantages:
according to the method, the surface hydroxyl number of the silicon micropowder and the viscosity of the epoxy resin can be reduced through modification, the phenylamino group in the silane coupling agent is grafted on the surface of the silicon micropowder to promote the silicon micropowder to be changed from hydrophilicity to hydrophobicity, meanwhile, the epoxy group in the silane coupling agent obviously improves the dispersibility of the silicon micropowder in the epoxy resin, and the problem of poor compatibility of the silicon micropowder and the epoxy resin is solved. The activation degree of the hydrophobic silicon micro powder prepared by the invention reaches 96.2 percent, the oleophilic degree reaches 2.79 percent, the minimum content of silicon hydroxyl is 0.62mg/g, and when the hydrophobic silicon micro powder is used for epoxy resin, the viscosity of an epoxy resin system is reduced to 1.18 Pa.S.
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FIG. 1 is a graph comparing FTIR before and after modification of silica fume.
Detailed Description
The technical solution of the present invention is described in more detail below with reference to specific examples. So that those skilled in the art can further understand the present invention without constituting a limitation to the right of the present invention.
In the following examples, the test methods for the various performance parameters were as follows:
(1) And (3) measuring the activation degree:
measuring 50 mL of distilled water, placing the distilled water in a 100 mL beaker, adding 1.0 g (accurate to 0.001 g) of silicon micropowder, stirring for 30min, standing for 24 h, separating, drying and weighing the silicon micropowder sinking to the bottom, and calculating according to the following formula:
(2) Determination of the content of silicon hydroxyl groups:
2.0 g of silica powder was weighed into a 200 mL beaker, 25 mL of absolute ethanol was added, followed by 75 mL of 20% NaCl solution. After the mixture is stirred evenly by magnetic force, 0.1 mol/L NaOH (HCl) standard solution is added dropwise to adjust the pH of the test solution to 4 (not counting volume). Then, 0.1 mol/L NaOH was slowly added dropwise to adjust the pH to 9, and the pH was maintained for 20 seconds and was calculated according to the following formula:
α OH -silicon hydroxyl content in mg/g; C-NaOH solution concentration, unit is mol per liter (mol/L); v pH4-9 The volume of NaOH consumed in milliliters (mL) for pH values ranging from 4.0 to 9.0; v B -blank test determination of value in milliliters (mL); m-mass of sample in grams (g); 17.007 -the molar mass of the hydroxyl groups.
(3) Measurement of viscosity:
weighing 96g of silicon powder and 64g of epoxy resin to prepare a resin mixture, stirring for 10min under a high-speed stirrer, vacuumizing for 1h in a vacuum oven at 60 ℃, preheating for 30min at 60 ℃ in an oil bath pan, adjusting the rotating speed to 60rpm by using a Bohler flying rotary viscosity tester and measuring the viscosity of the resin mixture at 20min by using a rotor type S04.
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Example 1: preparation method experiment I for epoxy resin system silicon micropowder
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature to be 140 ℃, adding prehydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane mixed liquor (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, hydrolyzing for 20min, and hydrolyzing the pH value of the mixture to be 4.0), and modifying for 20min to obtain primary modified silicon micropowder; adding 1.5kg of primary modified silicon micro powder into a wet modification machine, adding a prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane mixed solution (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), setting the temperature to 80 ℃, and modifying for 60min to obtain the hydrophobic silicon micro powder for the epoxy resin.
Referring to FIG. 1, 474 cm in FIG. 1 -1 A bending vibration absorption peak of a Si-O-Si bond; 798 cm of -1 The position is an antisymmetric telescopic vibration absorption peak of a Si-O-Si bond; 1107 cm of -1 The absorption peak is the symmetrical stretching vibration absorption peak of the Si-O-Si bond; 3400cm -1 The peak is the stretching vibration peak of-OH. As can be seen from the infrared image, the modified sample is 3100-3400cm -1 The stretching vibration absorption of the hydroxyl group is obviously weakened, which shows that the content of the hydroxyl group on the surface of the modified silicon micro powder is reduced, the hydrophobicity is improved, and the activity is improved.
Example 2: preparation method experiment II for epoxy resin system silicon micro powder
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature to be 150 ℃, adding prehydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane mixed liquor (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, hydrolyzing for 20min, and hydrolyzing the pH value of the mixture to be 4.0), and modifying for 20min to obtain primary modified silicon micropowder; adding 1.5kg of primary modified silicon micro powder into a wet modification machine, adding a prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane mixed solution (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), setting the temperature to 80 ℃, and modifying for 60min to obtain the hydrophobic silicon micro powder for the epoxy resin.
Example 3: preparation method experiment III for epoxy resin system silicon micro powder
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature to be 150 ℃, adding prehydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane mixed liquor (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, hydrolyzing for 20min, and hydrolyzing the pH value of the mixture to be 4.0), and modifying for 20min to obtain primary modified silicon micropowder; adding 1.5kg of once modified silicon micro powder into a wet modification machine, adding a prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane mixed solution (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), setting the temperature to be 90 ℃, and modifying for 60min to obtain the hydrophobic silicon micro powder for the epoxy resin.
Example 4: preparation method experiment four for epoxy resin system silicon micro powder
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature to be 150 ℃, adding prehydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane mixed liquor (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, hydrolyzing for 20min, and hydrolyzing the pH value of the mixture to be 4.0), and modifying for 20min to obtain primary modified silicon micropowder; adding 1.5kg of primary modified silicon micro powder into a wet modification machine, adding a prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane mixed solution (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, the hydrolysis time is 20min, the hydrolysis pH is 8.5), setting the temperature to be 90 ℃, and modifying for 60min to obtain the hydrophobic silicon micro powder for the epoxy resin.
Example 5: preparation method experiment five for epoxy resin system silicon micro powder
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature to be 150 ℃, adding prehydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane mixed liquor (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, hydrolyzing for 20min, and hydrolyzing the pH value of 5.0), and modifying for 20min to obtain primary modified silicon micropowder; adding 1.5kg of once modified silicon micro powder into a wet modification machine, adding a prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane mixed solution (7.5 g of coupling agent, 7.5g of ethanol and 15g of deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), setting the temperature to be 90 ℃, and modifying for 60min to obtain the hydrophobic silicon micro powder for the epoxy resin.
Comparative experiment 1:
adding 1.5kg of silicon micropowder into a high-speed mixing modification machine, setting the temperature to be 150 ℃, adding a prehydrolyzed gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, hydrolyzing for 20min, wherein the hydrolysis pH is 4.0), and modifying for 20min to obtain the silicon micropowder for the epoxy resin.
Comparative experiment 2:
adding 1.5kg of silicon micropowder into a high-speed mixing modification machine, setting the temperature to be 140 ℃, adding a prehydrolyzed gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, hydrolyzing for 30min, wherein the hydrolysis pH is 4.0), and modifying for 20min to obtain the silicon micropowder for the epoxy resin.
Comparative experiment 3
Adding 1.5kg of silicon micropowder into a wet modification machine, setting the temperature to be 80 ℃, adding prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane mixed liquor (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, hydrolyzing for 30min, and hydrolyzing the pH value to be 7.5), and modifying for 60min to obtain the silicon micropowder for the epoxy resin.
Comparative experiment 4
Adding 1.5kg of silicon micropowder into a wet modification machine, setting the temperature to be 90 ℃, adding prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane mixed liquor (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, hydrolyzing for 20min, and hydrolyzing the pH value to be 7.5), and modifying for 60min to obtain the silicon micropowder for the epoxy resin.
TABLE 1 test table for the performance of the fine silica powder prepared in each example and comparative example
Table 1 shows the performance test tables of the untreated fine silica powder as it is, and the fine silica powders obtained in each example and comparative example. As can be seen from Table 1, compared with the unmodified silica powder, the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane modified silica powder and the N-phenyl-gamma-aminopropyl trimethoxy silane modified silica powder, the activation degree of the silica powder after secondary modification is obviously improved, the number of hydroxyl groups on the surface of the silica powder is greatly reduced, and the hydrophobicity of the silica powder is enhanced. When the silicon micro powder is applied to epoxy resin, the viscosity of the resin mixture is greatly reduced, the dispersibility of the silicon micro powder in the epoxy resin is improved, and the processability of the epoxy resin is improved.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. A preparation method for epoxy resin system silica micropowder is characterized by comprising the following steps: adopting silane coupling agent to modify in two steps, namely adopting prehydrolyzed gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane to modify by a mixer dry method at a proper temperature to obtain primary modified silicon micropowder; then carrying out wet modification on the prehydrolyzed N-phenyl-gamma-aminopropyltrimethoxysilane by using a stirrer at a proper temperature to obtain secondary modified silicon micropowder;
the method for hydrolyzing the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane comprises the following steps: mixing a silane coupling agent gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, ethanol and water for hydrolysis reaction, wherein the mass ratio of the silane coupling agent to the isopropanol to the water is 1:0.8-1.2:1.8-2.2, the hydrolysis time is 20-30min, and the hydrolysis pH is 4.0-5.0;
the dry modification temperature is 140 to 150 ℃, and the modification time is 15 to 25min; the wet modification temperature is 80-90 ℃, and the modification time is 55-65min;
the method for hydrolyzing the N-phenyl-gamma-aminopropyl trimethoxy silane comprises the following steps: mixing N-phenyl-gamma-aminopropyltrimethoxysilane, isopropanol and water for hydrolysis reaction, wherein the mass ratio of the N-phenyl-gamma-aminopropyltrimethoxysilane to the isopropanol to the water is 1:0.8-1.2:1.8-2.2, the hydrolysis time is 20-30min, and the hydrolysis pH is 7.5-8.5.
2. The preparation method of the epoxy resin system silica micropowder according to claim 1, characterized by comprising the steps of: the hydrolysis time is 20min, and the hydrolysis pH is 4.0; the mass ratio of the silane coupling agent to the isopropanol to the water is 1.
3. The method for preparing the silica powder for the epoxy resin system according to claim 1, wherein the method comprises the following steps: the mass ratio of the N-phenyl-gamma-aminopropyltrimethoxysilane to the isopropanol to the water is 1.
4. The method for preparing the silica powder for the epoxy resin system according to claim 1, wherein the method comprises the following steps: the dry modification temperature is 150 ℃, and the modification time is 20min; the wet modification temperature is 90 ℃, and the modification time is 60min.
5. The method for preparing the silica powder for the epoxy resin system according to claim 1, wherein the method comprises the following steps: when dry modification and wet modification are carried out, the addition amount of the silane coupling agent is 4-6 per mill of the mass of the silicon micropowder respectively.
6. The method for preparing the silica powder for the epoxy resin system according to claim 5, wherein the method comprises the following steps: and when the dry method modification and the wet method modification are carried out, the adding amount of the silane coupling agent is 5 per mill of the mass of the silicon micro powder respectively.
7. The preparation method of the silica powder for the epoxy resin system according to any one of claims 1 to 6, characterized by comprising the following specific steps:
(1) And (3) hydrolysis reaction: mixing a silane coupling agent gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, ethanol and water for hydrolysis reaction to obtain silane coupling agent hydrolysate, and adjusting the pH of the hydrolysate to be 4.0 to 5.0;
mixing a silane coupling agent N-phenyl-gamma-aminopropyltrimethoxysilane, isopropanol and water for hydrolysis reaction to obtain a silane coupling agent hydrolysate, and adjusting the pH of the hydrolysate to 7.5 to 8.5;
(2) Modification reaction: mixing the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane hydrolysate with silicon micropowder, and performing dry modification at the temperature of 140-150 ℃ by using a high-speed mixer to obtain primary modified silicon micropowder; and carrying out wet modification on the N-phenyl-gamma-aminopropyltrimethoxysilane hydrolysate and the primary modified silicon micro powder at the temperature of between 80 and 90 ℃ by using a high-speed mixer to obtain secondary modified silicon micro powder.
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