CN113150387B - Preparation method of hydrophobic silicon micro powder - Google Patents
Preparation method of hydrophobic silicon micro powder Download PDFInfo
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- CN113150387B CN113150387B CN202110430165.2A CN202110430165A CN113150387B CN 113150387 B CN113150387 B CN 113150387B CN 202110430165 A CN202110430165 A CN 202110430165A CN 113150387 B CN113150387 B CN 113150387B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Abstract
The invention discloses a preparation method of hydrophobic silicon micro powder. The method comprises the steps of mixing a silane coupling agent N-phenyl gamma-aminopropyl trimethoxy silane, isopropanol and water for hydrolysis reaction to obtain silane coupling agent hydrolysate, atomizing the silane coupling agent hydrolysate by using an atomizer, mixing the silane coupling agent hydrolysate with silicon micropowder, and performing modification reaction to obtain the hydrophobic silicon micropowder. The method has simple process, and the prepared modified silicon micropowder has high activity, good hydrophobicity and low surface hydroxyl, and can greatly reduce the viscosity of the epoxy resin and improve the dispersibility of the epoxy resin when applied to the epoxy resin.
Description
Technical Field
The invention belongs to the field of inorganic material preparation, and relates to a preparation method of hydrophobic silicon micro powder.
Background
The silicon micropowder is used as an inorganic nonmetallic material with good temperature resistance, acid and alkali corrosion resistance, high heat conductivity coefficient and high insulation, and is widely applied to the fields of chemical industry, electronics, integrated circuits, electrical appliances, plastics, coatings, high-grade paint, rubber, national defense and the like. With the continuous development of downstream high-end application markets, the requirements on the quality and stability of the non-metallic mineral powder material are continuously improved.
The silicon micropowder has small particle size and high surface energy, and is easy to agglomerate, so that subsequent application is influenced. The problem of agglomeration of the silicon micropowder can be solved by carrying out surface modification on the silicon micropowder. For example, chinese patent application CN107841186A discloses a method for preparing modified silica, which comprises adding a silane coupling agent solution into a silica powder base material, heating to remove a solvent, and cooling to obtain the modified silica. However, the method directly adds the silane coupling agent into the powder for modification, so that the modification effect is not ideal, and the powder is easy to agglomerate when being mixed with the resin.
Disclosure of Invention
The invention aims to provide a preparation method of hydrophobic silicon micro powder. The method takes N-phenyl-gamma-aminopropyltrimethoxysilane as a silane coupling agent, adopts a spraying mode to spray the hydrolysate of the silane coupling agent into the silicon micropowder so as to uniformly mix the hydrolysate, and simultaneously regulates and controls the conditions of atomization pressure, modification temperature, pH value and the like to improve the modification effect.
The technical scheme for realizing the purpose of the invention is as follows:
a preparation method of hydrophobic silicon micropowder comprises the following steps:
step 1, hydrolysis reaction: mixing silane coupling agent N-phenyl-gamma-aminopropyl trimethoxy silane (Y9669), isopropanol and water for hydrolysis reaction to obtain silane coupling agent hydrolysate, and adjusting the pH of the hydrolysate to 7.5-8.5;
step 2, modification reaction: and atomizing the silane coupling agent hydrolysate by using an atomizer, mixing the atomized silane coupling agent hydrolysate with the silicon micropowder at the atomization pressure of 0.3-0.5 MPa, and modifying at the temperature of 100-110 ℃ to obtain the hydrophobic silicon micropowder.
Preferably, in step 1, the mass ratio of the silane coupling agent to the isopropyl alcohol to the water is 1.
Preferably, in step 1, the hydrolysis time is 20 to 40min.
Preferably, in step 2, the modification time is 20min.
In the step 2, the adding amount of the silane coupling agent is adjusted according to actual conditions, and in the specific embodiment of the invention, the adding amount of the silane coupling agent is 5 per mill of the silicon micropowder.
Preferably, in the step 1, the pH value of the silane coupling agent hydrolysate is 7.5, and the hydrolysis time is 20min; in the step 2, the atomization pressure is 0.5MPa, the modification temperature is 100 ℃, and the modification time is 20min.
Compared with the prior art, the invention has the following advantages:
(1) The invention takes N-phenyl-gamma-aminopropyl trimethoxy silane as a silane coupling agent, and the silane coupling agent is a substance with bifunctional groups and has a general formula of YRSI (OR) 3 Wherein the Y group is an organic functional group and OR represents a hydrolyzable group. The action mechanism is that firstly the silanol is generated by hydrolysis and interacts with the surface of the powder, thereby improving the powderDispersibility in the system. According to the invention, the hydrolysis degree of the silane coupling agent is regulated and controlled by regulating and controlling the hydrolysis process of the silane coupling agent, so that the silanol and the surface of the powder are fully reacted, and the action effect of the silanol and the surface of the powder is further improved.
(2) According to the invention, the silane coupling agent hydrolysate is fully atomized and then mixed with the silicon powder in an atomization mode, so that the silicon powder is mixed more uniformly, and meanwhile, the purpose of modifying the silicon powder can be achieved by fully wetting the silicon powder with little silane coupling agent hydrolysate.
(3) The invention can reduce the surface hydroxyl number of the silicon micropowder, and the phenylamino group in the silane coupling agent is grafted on the surface of the silicon micropowder, so that the silicon micropowder is converted from hydrophilicity to hydrophobicity, the dispersibility of the silicon micropowder in the epoxy resin is obviously improved, 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 can reach 100%, the oleophilic degree can reach 6.01%, and the minimum content of silicon hydroxyl is 0.47mg/g, so that when the hydrophobic silicon micro powder is used for epoxy resin, the viscosity of the epoxy resin is reduced to 0.68 Pa.S.
Drawings
FIG. 1 is a TG diagram before and after modification of fine silica powder.
FIG. 2 is an FTIR chart before and after modification of fine silica powder.
Detailed Description
In the following examples, the test methods for the various performance parameters were as follows:
(1) And (3) measuring the oleophilic degree:
transferring 50mL of deionized water into a 100mL beaker, then weighing 1.0g (accurate to 0.001 g) of silicon micropowder powder in the 100mL beaker by using a balance, dropwise adding absolute ethyl alcohol until all the silicon micropowder powder is soaked in a liquid phase, recording the dropwise adding amount V (mL) of the absolute ethyl alcohol, and calculating according to the following formula:
(2) And (3) measuring the activation degree:
measuring 50mL of distilled water, placing the distilled water in a 100mL beaker, adding 1.0g (accurate to 0.001 g) of silicon micropowder, stirring for 30min, standing for 24h, separating, drying and weighing the silicon micropowder sinking to the bottom, and calculating according to the following formula:
(3) Determination of the content of silicon hydroxyl groups:
2.0g of silica powder was weighed into a 200mL beaker, 25mL of absolute ethanol was added, followed by 75mL of 20% NaCl solution. After the mixture is stirred evenly by magnetic force, 0.1mol/L NaOH (HCl) standard solution is added dropwise to adjust the pH of the test solution to 4 (not counting volume). Then, 0.1mol/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 from 4.0 liters to 9.0; v B -blank test determination of value in milliliters (mL); m-mass of sample in grams (g); 17.007-molar mass of hydroxyl groups.
(4) 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
Adding 1.5kg of silicon micropowder into a high-speed mixing modification machine, setting the temperature to be 100 ℃, preheating for 30min, and the atomization pressure to be 0.5MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time to be 30min, the hydrolysis pH to be 7.5), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Example 2
Adding 1.5kg of silicon micropowder into a high-speed mixing modification machine, setting the temperature at 110 ℃, preheating for 30min, and the atomization pressure at 0.5MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 7.5), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Example 3
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature at 100 ℃, preheating for 30min, and the atomization pressure at 0.5MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 8.5), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Example 4
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature at 100 ℃, preheating for 30min, and the atomization pressure at 0.5MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 20min, the hydrolysis pH is 7.5), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Example 5
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature at 100 ℃, preheating for 30min, and the atomization pressure at 0.5MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 40min, the hydrolysis pH is 7.5), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Example 6
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature at 100 ℃, the atomization pressure at 0.3MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 7.5), and modifying for 20min to obtain the hydrophobic silicon micropowder for epoxy resin.
Comparative example 1
Adding 1.5kg of silicon micropowder into a high-speed mixing modification machine, setting the temperature to be 100 ℃, preheating for 30min, and the atomization pressure to be 0.5Mpa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time to be 30min, the hydrolysis pH to be 4.0), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Comparative example 2
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature at 100 ℃, preheating for 30min, and the atomization pressure at 0.5MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 4.5), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Comparative example 3
Adding 1.5kg of silicon micropowder into a high-speed mixing modification machine, setting the temperature to be 100 ℃, preheating for 30min, and the atomization pressure to be 0.5MPa, adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 6.0), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Comparative example 4
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature at 100 ℃, preheating for 30min, and the atomization pressure at 0.5MPa, adding a prehydrolyzed KH-560 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 4.0), and modifying for 20min to obtain the high-phase hydrophobic silicon micropowder for epoxy resin.
Comparative example 5
1.5kg of silicon micropowder is added into a high-speed mixing modification kettle, the temperature is set to be 100 ℃, the prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 7.5) is directly added without atomization, and the hydrophobic silicon micropowder for epoxy resin is obtained after modification for 20min.
Comparative example 6
Adding 1.5kg of silicon micropowder into a high-speed mixing and modifying machine, setting the temperature at 100 ℃, the atomization pressure at 0.6MPa, directly adding a prehydrolyzed Y9669 mixed solution (7.5 g of coupling agent, 7.5g of isopropanol and 15g of deionized water, the hydrolysis time is 30min, the hydrolysis pH is 7.5), and modifying for 20min to obtain the hydrophobic silicon micropowder for epoxy resin.
TABLE 1 test table for the performance of the fine silica powder prepared in each example and comparative example
| Examples | Degree of activation% | Degree of oleophilic transformation% | Silicon hydroxyl content mg/g | Viscosity Pa.S |
| Untreated fine silica powder as it is | 0 | 0 | 0.78 | 1.78 |
| Example 1 | 100 | 5.66 | 0.49 | 0.70 |
| Example 2 | 100 | 4.21 | 0.62 | 0.83 |
| Example 3 | 100 | 4.40 | 0.62 | 0.82 |
| Example 4 | 100 | 6.01 | 0.47 | 0.68 |
| Example 5 | 100 | 5.77 | 0.48 | 0.69 |
| Example 6 | 100 | 5.33 | 0.56 | 0.81 |
| Comparative example 1 | 93.1 | 4.03 | 0.65 | 1.68 |
| Comparative example 2 | 98.2 | 4.21 | 0.62 | 1.78 |
| Comparative example 3 | 100 | 4.49 | 0.62 | 0.92 |
| Comparative example 4 | 0 | 0 | 0.81 | 1.45 |
| Comparative example 5 | 95.6 | 4.11 | 0.64 | 1.55 |
| Comparative example 6 | 94.7 | 3.87 | 0.64 | 1.66 |
As can be seen from fig. 1, the decrease in the mass of the fine silica powder before and after modification is rapid in the range of 0 to 200 ℃ with an increase in temperature, and the mass loss before modification is greater than that after modification because of desorption of adsorbed water from the fine silica powder, but the fine silica powder after modification has a hydrophobic property and therefore has a small mass loss. However, after 200 ℃ the mass loss of the fine silica powder after modification began to be greater than that of the fine silica powder before modification because the organic group grafted to the surface of the fine silica powder began to decompose, the decomposition temperature of the phenylamino group was 370 ℃, and the molecular weight of the organic group was large, so the mass loss was large, indicating that the modifier had been grafted onto the fine silica powder.
474cm in FIG. 2 -1 The position is a bending vibration absorption peak of an Si-O-Si bond; 798cm -1 The position is an antisymmetric stretching vibration absorption peak of a Si-O-Si bond; 1107cm -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 hydrolyzed 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.
Table 1 shows the performance test tables of the original fine silica powder, the fine silica powders prepared in the examples and the comparative examples. As can be seen from table 1, compared with unmodified silica powder, silica powder modified by acidic hydrolysis, silica powder modified by other silane coupling agents, and silica powder modified under the conditions of no atomization treatment and too high atomization pressure, the activation degree and oleophilic degree of the modified silica powder subjected to alkaline hydrolysis and atomization pressure regulation are 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.
Claims (6)
1. The preparation method of the hydrophobic silicon micropowder is characterized by comprising the following steps:
step 1, hydrolysis reaction: mixing silane coupling agent N-phenyl-gamma-aminopropyltrimethoxysilane, isopropanol and water for hydrolysis reaction to obtain silane coupling agent hydrolysate, and adjusting the pH value of the hydrolysate to 7.5-8.5;
step 2, modification reaction: and atomizing the silane coupling agent hydrolysate by using an atomizer, mixing the atomized silane coupling agent hydrolysate with the silicon micropowder at the atomization pressure of 0.3-0.5 MPa, and modifying at the temperature of 100-110 ℃ to obtain the hydrophobic silicon micropowder.
2. The production method according to claim 1, wherein in step 1, the mass ratio of the silane coupling agent, isopropyl alcohol and water is 1.
3. The method according to claim 1, wherein the hydrolysis time in step 1 is 20 to 40min.
4. The method according to claim 1, wherein in the step 2, the modification time is 20min.
5. The preparation method according to claim 1, wherein in the step 2, the addition amount of the silane coupling agent is 5% o of the fine silicon powder.
6. The preparation method according to claim 1, wherein in the step 1, the pH of the silane coupling agent hydrolysate is 7.5, and the hydrolysis time is 30min; in the step 2, the atomization pressure is 0.5Mpa, the modification temperature is 100 ℃, and the modification time is 20min.
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| CN114836057B (en) * | 2022-04-07 | 2023-06-09 | 福建远翔新材料股份有限公司 | Preparation method of nano hydrated silicon dioxide through superhydrophobic modification |
| CN115028895B (en) * | 2022-06-24 | 2024-04-02 | 江苏联瑞新材料股份有限公司 | Preparation method of modified spherical alumina for enhancing strength of epoxy resin |
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| JP4986444B2 (en) * | 2005-12-12 | 2012-07-25 | 株式会社トクヤマ | Hydrophobic inorganic powder and method for producing the same |
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