A silane grinding aid for quartz powder grinding and its preparation method and application
By using silane-based aids for quartz grinding, including phenyltrimethoxysilane solution, silane coupling agent PT-172 solution, stearic acid and sodium hydroxide, the existing aids have poor grinding effect and poor dispersion, and efficient grinding effect and good powder dispersion are achieved.
Patent Information
- Application Number
- CN202310393401.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-04-13
- Publication Date
- 2025-05-23
- Estimated Expiration
- 2043-04-13
AI Technical Summary
The existing quartz grinding aids have poor grinding effect and poor dispersion, which leads to large grinding time and energy consumption, and the products are prone to agglomeration, and the dispersion does not meet the needs.
A silane-based aid for quartz grinding is used, including phenyltrimethoxysilane solution, silane coupling agent PT-172 solution, stearic acid and sodium hydroxide, and is prepared by ultrasonic mixing and other steps to form a reactive coating film to improve the rheological mechanical properties and dispersion of the powder.
It significantly improves the grinding effect of quartz powder milling and the dispersion of powder, reduces energy consumption, avoids agglomeration, and improves the activity and fluidity of powder.
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Figure CN117143565B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of quartz grinding, and in particular to a silane grinding aid for quartz grinding, a preparation method and application thereof. Background Art
[0002] Silica powder is a kind of quartz (natural quartz or fused quartz, the main component is SiO 2 ) is a multifunctional white powder made of raw materials, which is widely used in ink, coating, plastic, ceramic, rubber, electronics and other industries. The surface-treated silicon micropowder has low oil absorption and good fluidity. When used as an industrial filler, it can significantly reduce the amount of some chemical agents and reduce the user's cost of use. It is widely used in industrial anti-corrosion, floor paint, and copper-clad laminates. Quartz is hard and wear-resistant (Mohs hardness generally reaches 7). It is difficult to obtain a powder product of ideal fineness simply by relying on the grinding effect of the medium. Therefore, a certain amount of grinding aid is often added in the process of grinding silicon micropowder to improve the grinding effect.
[0003] At present, the commonly used grinding aids for quartz powder grinding include triethanolamine, DA dispersant, stearic acid, ammonium chloride, sodium chloride, alcohol, sodium oleate, sodium silicate, dodecylamine, etc. However, some of these grinding aids have poor grinding effect, and the time and energy consumption required to reach the required particle size are large. Some products are prone to agglomeration after grinding, and the dispersibility does not meet the requirements. Therefore, it is urgent to provide a grinding aid with good grinding effect, good powder dispersibility and the ability to perform surface treatment on the powder to be ground. Summary of the invention
[0004] The purpose of the present invention is to provide a silane grinding aid for quartz powder grinding and a preparation method and application thereof, so as to solve the problems of poor grinding aid effect and poor dispersibility of the existing quartz powder grinding aid.
[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0006] The present invention provides a silane grinding aid for quartz powder grinding, comprising the following raw materials in mass fractions:
[0007]
[0008]
[0009] Furthermore, in the silane grinding aid for quartz powder grinding, the phenyltrimethoxysilane solution is a mixture of propanol and phenyltrimethoxysilane, and the mass fraction of phenyltrimethoxysilane in the phenyltrimethoxysilane solution is 15-25%.
[0010] Furthermore, in the silane grinding aid for quartz powder grinding, the silane coupling agent PT-172 solution is a mixture of propanol and silane coupling agent PT-172, and the mass fraction of silane coupling agent PT-172 in the silane coupling agent PT-172 solution is 15 to 25%.
[0011] Furthermore, the silane grinding aid for quartz powder grinding includes the following raw materials in mass fractions:
[0012]
[0013] The present invention also provides a method for preparing a silane grinding aid for quartz powder grinding, comprising the following steps:
[0014] The phenyltrimethoxysilane solution and the silane coupling agent PT-172 solution are mixed, and then stearic acid and sodium hydroxide are added in sequence, and then ultrasonically mixed to obtain a silane grinding aid for quartz powder grinding.
[0015] The present invention also provides an application of a silane grinding aid for quartz powder grinding in powder grinding, wherein the amount of the silane grinding aid for quartz powder grinding is 0.1-0.3% of the total mass of the powder to be ground.
[0016] Furthermore, in the application of the silane grinding aid for quartz powder grinding in grinding, the amount of the silane grinding aid for quartz powder grinding is 0.2% of the total mass of the powder to be ground.
[0017] It can be seen from the above technical solution that compared with the prior art, the present invention has the following beneficial effects:
[0018] (1) The present invention adds a silane coupling agent, in which the -OR functional group can be hydrolyzed in water (including free water adsorbed on the surface of quartz powder) to generate silanol groups (as shown below), which can react with SiO 2 Chemically bonded or with SiO 2 The original silanol groups on the surface are combined into a homogeneous system, which not only removes SiO 2 The moisture on the surface forms a silane ether bond with the oxygen atoms therein, so that the organic functional group -R' of the high molecular weight polymer carried by the other end of the silane coupling agent is firmly covered on the surface of the quartz or silica particles to form a coating film with reactive activity. Organic functional groups such as phenyl have good affinity, which can reduce the surface energy of quartz or silica powder, improve grinding efficiency and reduce energy consumption; in addition, the formation of this new interface layer can improve the rheological properties and dispersibility of the powder;
[0019]
[0020] (2) The present invention adds stearic acid, which acts as an auxiliary surfactant to further reduce the surface tension of the powder particles, prevent mutual adsorption between mineral powders, and improve the rheological properties and dispersibility of the powder;
[0021] (3) The present invention adds a trace amount of sodium hydroxide as a pH regulator, which can promote the silane coupling agent to adhere to the surface of quartz or silicon dioxide powder more quickly. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments or the prior art are briefly introduced below.
[0023] Figure 1 This is the product packaging picture of silane coupling agent PT-172 produced by Guangdong Foshan Putuobao Chemical Co., Ltd. DETAILED DESCRIPTION
[0024] The present invention provides a silane grinding aid for quartz powder grinding, comprising the following raw materials in mass fractions:
[0025]
[0026]
[0027] In the present invention, the mass fraction of the phenyltrimethoxysilane solution is preferably 60 to 82%, more preferably 72 to 82%, and even more preferably 82%.
[0028] In the present invention, the mass fraction of the silane coupling agent PT-172 solution is preferably 10 to 26%, more preferably 10 to 17%, and even more preferably 10%.
[0029] In the present invention, the mass fraction of stearic acid is preferably 7 to 12%, more preferably 7 to 9%, and even more preferably 7%.
[0030] In the present invention, the mass fraction of sodium hydroxide is preferably 1 to 2%, more preferably 1 to 1.5%, and even more preferably 1%.
[0031] In the present invention, the phenyltrimethoxysilane solution is preferably a mixture of propanol and phenyltrimethoxysilane, and the mass fraction of phenyltrimethoxysilane in the phenyltrimethoxysilane solution is preferably 15-25%, more preferably 18-23%, and more preferably 20%.
[0032] In the present invention, the silane coupling agent PT-172 solution is preferably a mixture of propanol and silane coupling agent PT-172, and the mass fraction of silane coupling agent PT-172 in the silane coupling agent PT-172 solution is preferably 15-25%, more preferably 17-21%, and more preferably 20%. Among them, the manufacturer of silane coupling agent PT-172 is Guangdong Foshan Putuobao Chemical Co., Ltd.
[0033] The present invention also provides a method for preparing a silane grinding aid for quartz powder grinding, comprising the following steps:
[0034] The phenyltrimethoxysilane solution and the silane coupling agent PT-172 solution are mixed evenly, and then stearic acid and sodium hydroxide are added in sequence, and then ultrasonically shaken and mixed evenly to obtain a silane grinding aid for quartz powder grinding.
[0035] The present invention does not limit the ultrasonic conditions, and any method known in the art may be used.
[0036] The present invention also provides an application of a silane grinding aid for quartz powder grinding in powder grinding, wherein the amount of the silane grinding aid for quartz powder grinding is preferably 0.1-0.3% of the total mass of the powder to be ground, more preferably 0.18-0.25%, and more preferably 0.2%.
[0037] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0038] Example 1
[0039] This embodiment provides a silane grinding aid for quartz powder grinding, comprising the following raw materials in mass fractions:
[0040] 60% phenyltrimethoxysilane solution, 26% silane coupling agent PT-172 solution, 12% stearic acid, 2% sodium hydroxide, wherein the mass fraction of phenyltrimethoxysilane in the phenyltrimethoxysilane solution is 20%, and the mass fraction of silane coupling agent PT-172 in the silane coupling agent PT-172 solution is 20%;
[0041] The preparation method of silane grinding aid for quartz powder grinding is as follows:
[0042] The phenyltrimethoxysilane solution and the silane coupling agent PT-172 solution were stirred evenly at room temperature, and then stearic acid and sodium hydroxide were added in sequence and ultrasonically stirred evenly to obtain a silane grinding aid for quartz powder grinding.
[0043] The silane grinding aid obtained in Example 1 is used for powder grinding, and the amount of the silane grinding aid used is 0.2% of the total amount of quartz powder to be ground.
[0044] Example 2
[0045] This embodiment provides a silane grinding aid for quartz powder grinding, comprising the following raw materials in mass fractions:
[0046] 82% phenyltrimethoxysilane solution, 10% silane coupling agent PT-172 solution, 7% stearic acid, 1% sodium hydroxide, wherein the mass fraction of phenyltrimethoxysilane in the phenyltrimethoxysilane solution is 20%, and the mass fraction of silane coupling agent PT-172 in the silane coupling agent PT-172 solution is 20%;
[0047] The preparation method of silane grinding aid for quartz powder grinding is as follows:
[0048] The phenyltrimethoxysilane solution and the silane coupling agent PT-172 solution were stirred evenly at room temperature, and then stearic acid and sodium hydroxide were added in sequence and ultrasonically stirred evenly to obtain a silane grinding aid for quartz powder grinding.
[0049] The silane grinding aid obtained in Example 2 is used for powder grinding, and the amount of the silane grinding aid used is 0.2% of the total amount of quartz powder to be ground.
[0050] Example 3
[0051] This embodiment provides a silane grinding aid for quartz powder grinding, comprising the following raw materials in mass fractions:
[0052] 71% phenyltrimethoxysilane solution, 18% silane coupling agent PT-172 solution, 10% stearic acid, 1% sodium hydroxide, wherein the mass fraction of phenyltrimethoxysilane in the phenyltrimethoxysilane solution is 20%, and the mass fraction of silane coupling agent PT-172 in the silane coupling agent PT-172 solution is 20%;
[0053] The preparation method of silane grinding aid for quartz powder grinding is as follows:
[0054] The phenyltrimethoxysilane solution and the silane coupling agent PT-172 solution were stirred evenly at room temperature, and then stearic acid and sodium hydroxide were added in sequence and ultrasonically stirred evenly to obtain a silane grinding aid for quartz powder grinding.
[0055] The silane grinding aid obtained in Example 3 is used for powder grinding, and the amount of the silane grinding aid used is 0.2% of the total amount of quartz powder to be ground.
[0056] Example 4
[0057] The silane grinding aid obtained in Example 2 is used for powder grinding, and the amount of the silane grinding aid used is 0.1% of the total amount of quartz powder to be ground.
[0058] Example 5
[0059] The silane grinding aid obtained in Example 2 is used for powder grinding, and the amount of the silane grinding aid used is 0.3% of the total amount of quartz powder to be ground.
[0060] Comparative Example 1
[0061] The difference between the silane grinding aid obtained in Comparative Example 1 and Example 2 is that: 92% phenyltrimethoxysilane solution (a mixture of propanol and phenyltrimethoxysilane, the mass fraction of phenyltrimethoxysilane in the phenyltrimethoxysilane solution is 20%), no silane coupling agent PT-172 solution is added, stearic acid is 7%, and sodium hydroxide is 1%.
[0062] The silane grinding aid obtained in Comparative Example 1 was used for powder grinding, and the amount of the silane grinding aid used was 0.2% of the total amount of quartz powder to be ground.
[0063] Comparative Example 2
[0064] The difference between the silane grinding aid obtained in Comparative Example 2 and Example 2 is that: 92% of the silane coupling agent PT-172 solution (a mixture of propanol and the silane coupling agent PT-172, the mass fraction of the silane coupling agent PT-172 in the silane coupling agent PT-172 solution is 20%), no phenyltrimethoxysilane solution is added, stearic acid is 7%, and sodium hydroxide is 1%.
[0065] The silane grinding aid obtained in Comparative Example 2 was used for powder grinding, and the amount of the silane grinding aid used was 0.2% of the total amount of quartz powder to be ground.
[0066] Comparative Example 3
[0067] The grinding aid used in Comparative Example 3 is the currently commonly used sodium polyacrylate, and the amount of sodium polyacrylate used is 0.2% of the total amount of quartz powder to be ground.
[0068] Comparative Example 4
[0069] Comparative Example 4 is a blank control sample without using a grinding aid.
[0070] Quartz grinding effect test:
[0071] The effect of grinding aids was tested using a small experimental ball mill. The specifications of the ball mill cylinder were 0.8m(d)*1.2m(L), the filling rate was 50%, the material ball mass ratio was 1:6, the ball mill speed was 45r / min, and the ball milling time was 2h.
[0072] The quartz powder sample entering the mill is D 97≥90μm(D 97 The particle size value corresponding to the cumulative particle size distribution percentage reaching 97%) is used for the coarse powder. The ground quartz powder is tested for particle size using a Beite laser particle size analyzer, and the D value of the test result is taken. 97 As a comparison result.
[0073] The activity of quartz powder is characterized by measuring the activation degree of quartz powder. Weigh 5g of sample (accurate to 0.01g) and put it into a 250mL pear-shaped separatory funnel filled with 200mL distilled water. Close the funnel and shake it horizontally for 300 times. After standing on the iron stand for half an hour, use a sand core funnel to take out the lower sediment, dry it at 105℃ for 30min, and then weigh it. The activation degree is calculated as mass fraction H, and the calculation formula is as follows:
[0074]
[0075] Where:
[0076] m 1 is the mass of the lower sediment after drying, in grams (g);
[0077] m is the mass of the sample in grams (g).
[0078] The oil absorption of quartz powder is measured to characterize the modification effect of grinding aid on quartz powder. Weigh 5g sample (accurate to 0.01), put it on a glass plate, mix the sample with a spatula, and slowly add refined linseed oil until it reaches saturation. The measurement unit is mL / 100g. Generally, the finer the powder, the greater the oil absorption. The powder with better modification effect of the same specification has lower oil absorption.
[0079] Since a single experiment has a certain degree of randomness, each implementation method was repeated 3 times and the results were taken into a range interval, and the results are shown in Table 1.
[0080] Table 1. Quartz grinding effect test results
[0081]
[0082]
[0083] It can be seen from the test results in the table that the grinding aid prepared by the present invention has an excellent grinding aid effect on quartz powder grinding, and has a good modification effect, can effectively reduce the oil absorption of silicon micropowder, and improve the activity of powder, and has broad application prospects in the development of the quartz powder grinding field.
[0084] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A silane grinding aid for quartz powder grinding, It is characterized in that Contains the following raw materials by mass fraction: Phenyltrimethoxysilane solution 60~82%, Silane coupling agent PT-172 solution 10~26%, Stearic acid 7~12%, Sodium hydroxide 1~2%; Wherein, the mass fraction of phenyltrimethoxysilane in the phenyltrimethoxysilane solution is 15-25%; The mass fraction of the silane coupling agent PT-172 in the silane coupling agent PT-172 solution is 15-25%.
2. A silane grinding aid for quartz powder grinding as claimed in claim 1, It is characterized in that The phenyltrimethoxysilane solution is a mixture of propanol and phenyltrimethoxysilane.
3. A silane grinding aid for quartz powder grinding as claimed in claim 1, It is characterized in that The silane coupling agent PT-172 solution is a mixture of propanol and silane coupling agent PT-172.
4. A silane grinding aid for quartz powder grinding as claimed in claim 2 or 3, It is characterized in that Contains the following raw materials by mass fraction: Phenyltrimethoxysilane solution 82%, Silane coupling agent PT-172 solution 10%, Stearic acid 7%, Sodium hydroxide 1%.
5. A method for preparing a silane grinding aid for quartz powder grinding according to any one of claims 1 to 3, It is characterized in that The following steps are involved: The phenyltrimethoxysilane solution and the silane coupling agent PT-172 solution are mixed, and then stearic acid and sodium hydroxide are added in sequence, and then ultrasonically mixed to obtain a silane grinding aid for quartz powder grinding.
6. Use of a silane grinding aid for quartz grinding according to any one of claims 1 to 3 in grinding, It is characterized in that The amount of the silane grinding aid for quartz powder grinding is 0.1-0.3% of the total mass of the powder to be ground.
7. Use of a silane grinding aid for quartz grinding as claimed in claim 6 in grinding, It is characterized in that The amount of the silane grinding aid for quartz powder grinding is 0.2% of the total mass of the powder to be ground.
Citation Information
Patent Citations
Silicon wafer chemical and mechanical polishing composition with high stability
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Non-spherical primary silica nanoparticles and the use therefor
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