CN111875814A - Preparation method of modified rubber powder by sol-gel method - Google Patents
Preparation method of modified rubber powder by sol-gel method Download PDFInfo
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- CN111875814A CN111875814A CN202010768215.3A CN202010768215A CN111875814A CN 111875814 A CN111875814 A CN 111875814A CN 202010768215 A CN202010768215 A CN 202010768215A CN 111875814 A CN111875814 A CN 111875814A
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- rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/186—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof from or via fluosilicic acid or salts thereof by a wet process
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2319/00—Characterised by the use of rubbers not provided for in groups C08J2307/00 - C08J2317/00
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
Abstract
The invention discloses a surface modification method of waste rubber particles and a preparation method thereof, relates to the technical field of surface modification of rubber particles, and is prepared by a sol-gel method. The modified liquid comprises the following raw materials in percentage by weight: 21.8 to 35.8 weight percent of rubber powder, 43 to 52.4 weight percent of absolute ethyl alcohol, 4.5 to 5.5 weight percent of water, 4.0 to 4.9 weight percent of ammonia water, 12.5 to 15.3 weight percent of ethyl orthosilicate and 0.2 to KH 5500.09. The sum of the weight percentages of all the components is 100 percent. The method is characterized in that tetraethoxysilane generates hydrolytic polycondensation to generate silica particles under the action of an alkaline catalyst (ammonia water), and the surface of the silica particles is coated with silica by taking the rubber particles as nucleation sites, so that the surface activity of the rubber particles is changed. The modified rubber can be used in building materials such as concrete, can improve the interface between rubber and a cement matrix, enhance the mechanical property of rubber concrete, solve the problem of accumulation of waste rubber, reduce the use amount of natural aggregate, save energy and reduce emission.
Description
Technical Field
The invention relates to the field of modification of waste rubber powder, in particular to a preparation method of modified rubber powder by a sol-gel method.
Background
As a high polymer material, the rubber has the characteristics of insolubility and infusibility, and is difficult to degrade in nature. Due to the rapid development of the automobile industry, the accumulation of waste tires is becoming increasingly serious. How to effectively utilize waste rubber can reduce the problem of rubber accumulation and save resources, and becomes a problem to be solved urgently. In recent years, rubber powder has been incorporated into concrete and used as a fine aggregate. The method not only reduces the substitute amount of natural aggregate, but also effectively improves the defect of large brittleness of common concrete, enhances the toughness, shock resistance and other properties of the concrete, saves resources and meets the requirement of sustainable development.
The rubber powder is directly doped into the concrete, and due to the hydrophobicity of the rubber, weaker adhesion exists between the rubber powder and a cement matrix, a weak interface transition area is formed, so that the mechanical property of the concrete is remarkably reduced, and the use of the rubber powder in the field of building materials is limited. Therefore, when using waste rubber particles, the rubber surface is often subjected to a pretreatment, i.e., a surface modification, to enhance the adhesion between the rubber powder and the cement mortar. According to the invention, the surface coating treatment is carried out on the rubber particles by a sol-gel method, and the nano silicon dioxide generated by the reaction can obviously improve the performance of the rubber surface, enhance the bonding with a cement matrix and effectively improve the mechanical property of rubber concrete. Meanwhile, the preparation method of the sol-gel modified rubber powder provided by the invention has the advantages of mild chemical reaction, no need of conditions such as high temperature and high pressure, energy saving and environmental protection, can effectively solve the problem of rubber waste accumulation, can reduce the consumption of natural aggregate, and has important economic, environmental, social and application values.
Disclosure of Invention
The invention aims to provide a preparation method of modified rubber powder by a sol-gel method, which is characterized in that ethyl orthosilicate is subjected to hydrolytic polycondensation under alkaline catalysis by the sol-gel method, and the generated silicon dioxide particles take the rubber powder as nucleation sites to form a uniform coating on the surface of the silicon dioxide particles, so that the performance of the rubber surface is improved, and the bonding between rubber and a cement matrix is enhanced. The preparation process has the advantages of mild reaction conditions, energy conservation, environmental protection and low production cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of modified rubber powder by adopting a sol-gel method comprises the following steps: 21.8 to 35.8 weight percent of rubber powder, 43 to 52.4 weight percent of absolute ethyl alcohol, 4.5 to 5.5 weight percent of water, 4.0 to 4.9 weight percent of ammonia water, 12.5 to 15.3 weight percent of ethyl orthosilicate and 0.09 to 0.2 weight percent of silane coupling agent.
Preferably, the preparation method of the modified rubber powder by the sol-gel method provided by the invention has the advantages that the particle size of the selected rubber powder is 60-80 meshes;
preferably, the preparation method of the modified rubber powder by the sol-gel method provided by the invention adopts absolute ethyl alcohol as an analytical pure grade, and the mass fraction is more than or equal to 99.7%.
Preferably, the preparation method of the modified rubber powder by the sol-gel method provided by the invention selects deionized water as water.
Preferably, the preparation method of the modified rubber powder by the sol-gel method provided by the invention selects ammonia water as an analytical pure grade, and the effective content is 25%.
Preferably, in the preparation method of the modified rubber powder by the sol-gel method, the ethyl orthosilicate is selected as an analytical pure grade, and the effective content is 28%.
Preferably, the preparation method of the modified rubber powder by the sol-gel method provided by the invention selects the analytical pure KH550 as the silane coupling agent, and the effective content is more than or equal to 98%.
Preferably, the preparation method of the modified rubber powder by the sol-gel method provided by the invention comprises the following steps: 21.8 to 35.8 weight percent of rubber powder, 43 to 52.4 weight percent of absolute ethyl alcohol, 4.5 to 5.5 weight percent of water, 4.0 to 4.9 weight percent of ammonia water and 0.09 to 0.2 weight percent of silane coupling agent are prepared into reaction liquid in advance.
Preferably, the preparation method of the rubber powder modified by the sol-gel method provided by the invention comprises the steps of adding 12.5-15.3 wt% of tetraethoxysilane into a reaction solution, stirring for reaction for 4 hours, and then aging for 24 hours.
Preferably, the preparation method of the modified rubber powder by the sol-gel method provided by the invention adopts a mechanical stirring mode.
Compared with the prior art, the invention has the following beneficial effects: the sol-gel method adopted by the invention has mild reaction conditions, energy conservation, environmental protection, material conservation and simple process method, and the ethanol in the reaction solution can be recycled; the nano silicon dioxide coating is distributed on the surface of the prepared rubber particle, so that the performance of the surface of the rubber powder is improved, and the compatibility of the rubber powder and a cement matrix is improved; the modified rubber powder can be applied to the fields of building materials and the like, can enhance the bonding between the modified rubber powder and a concrete base material, improve the mechanical property of concrete, realize the reasonable utilization of waste rubber, reduce the use amount of natural aggregate, save energy and reduce emission.
Description of the drawings:
FIG. 1 is a scanning electron micrograph of unmodified rubber particles;
FIG. 2 is a scanning electron microscope photograph of the modified rubber of the present invention.
The specific implementation mode is as follows:
the invention is further illustrated by the following specific examples, but the invention is not limited to these examples.
Example 1:
weighing 20g of 60-mesh rubber, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.1g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the surface coating modified rubber particles.
Example 2:
weighing 20g of 60-mesh rubber, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.2g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the surface coating modified rubber particles.
Example 3:
weighing 20g of rubber with a particle size of 80 meshes, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.1g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the rubber particles with modified surface coatings.
Example 4:
weighing 20g of rubber with a particle size of 80 meshes, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.2g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the rubber particles with modified surface coatings.
Example 5:
weighing 40g of 60-mesh rubber, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.1g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the surface coating modified rubber particles.
Example 6:
weighing 40g of 60-mesh rubber, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.2g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the surface coating modified rubber particles.
Example 7:
weighing 40g of rubber with a particle size of 80 meshes, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.1g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the rubber particles with modified surface coatings.
Example 8:
weighing 40g of rubber with a particle size of 80 meshes, putting the rubber into a 250mL beaker, adding 48g of absolute ethyl alcohol, 5g of deionized water, 4.5g of ammonia water and 0.2g of silane coupling agent, mechanically stirring, adding 14g of tetraethoxysilane after uniformly mixing, continuously stirring for 4h, then sealing and aging at room temperature for 24h, filtering, washing by using deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the rubber particles with modified surface coatings.
The silicon dioxide surface modified rubber powder prepared by the process obviously improves the compatibility of the coating rubber powder and a cement matrix, improves the compressive strength by 40 to 45 percent compared with the concrete doped with the rubber powder raw material when the silicon dioxide surface modified rubber powder is used in the concrete, enhances the interface between the rubber powder and the cement matrix, and effectively improves the shock resistance, noise reduction, impact resistance and toughness of the concrete.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A preparation method of modified rubber powder by adopting a sol-gel method is characterized by comprising the following components in percentage by weight: 21.8 to 35.8 weight percent of rubber powder, 43 to 52.4 weight percent of absolute ethyl alcohol, 4.5 to 5.5 weight percent of water, 4.0 to 4.9 weight percent of ammonia water, 12.5 to 15.3 weight percent of ethyl orthosilicate and 0.09 to 0.2 weight percent of silane coupling agent.
2. The method for preparing the rubber powder modified by the sol-gel method according to claim 1, wherein the particle size of the rubber powder is 60-80 meshes;
3. the method for preparing the modified rubber powder by the sol-gel method according to claim 1, wherein the absolute ethyl alcohol is of analytical grade, and the mass fraction is greater than or equal to 99.7%.
4. The method of claim 1, wherein the water is deionized water.
5. The method of claim 1, wherein the ammonia water is of analytical grade purity and has an effective content of 25%.
6. The method for preparing modified rubber powder by sol-gel method as claimed in claim 1, wherein said tetraethoxysilane is analytical grade, and the effective content is 28%.
7. The method for preparing the modified rubber powder by the sol-gel method according to claim 1, wherein the silane coupling agent is analytical pure KH550, and the effective content is greater than or equal to 98%.
8. The method for preparing rubber powder modified by sol-gel method as claimed in claim 1, wherein the reaction solution is prepared by mixing rubber powder 21.8-35.8 wt% of absolute ethanol 43% -52.4 wt%, water 4.5-5.5 wt%, ammonia water 4.0% -4.9 wt%, and silane coupling agent 0.09-0.2 wt%.
9. The method for preparing rubber powder modified by sol-gel method as claimed in claims 1 and 8, wherein 12-15.3 wt% of tetraethoxysilane is added to the reaction solution, stirred for reaction for 4 hours, and then aged for reaction for 24 hours.
10. The process for preparing a modified rubber powder according to claims 1, 8 and 9, wherein the stirring is mechanical stirring.
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| CN202010768215.3A CN111875814A (en) | 2020-08-03 | 2020-08-03 | Preparation method of modified rubber powder by sol-gel method |
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| CN202010768215.3A CN111875814A (en) | 2020-08-03 | 2020-08-03 | Preparation method of modified rubber powder by sol-gel method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624723A (en) * | 2021-01-13 | 2021-04-09 | 杭州申华混凝土有限公司 | Freeze-thaw resistant concrete and preparation method thereof |
| WO2022165726A1 (en) * | 2021-02-02 | 2022-08-11 | 中国石油化工股份有限公司 | Coated rubber particle, preparation method therefor and use thereof |
| CN116063039A (en) * | 2022-10-25 | 2023-05-05 | 湖南泓盛新型建材有限公司 | Composite heat-insulating building block and preparation method thereof |
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| CN107216096A (en) * | 2017-07-21 | 2017-09-29 | 张娟 | A kind of preparation method of enhanced rubber powder modified concrete asphalt mortar |
| CN107674238A (en) * | 2017-10-10 | 2018-02-09 | 山西省交通科学研究院 | A kind of waste rubber powder surface modifying method |
| CN109293320A (en) * | 2018-12-07 | 2019-02-01 | 临沂宏艺科技发展有限公司 | A kind of concrete prepared using modified waste rubber powder |
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2020
- 2020-08-03 CN CN202010768215.3A patent/CN111875814A/en active Pending
Patent Citations (4)
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| CN102585250A (en) * | 2012-02-07 | 2012-07-18 | 上海焦耳蜡业有限公司 | Preparation method for wax emulsion |
| CN107216096A (en) * | 2017-07-21 | 2017-09-29 | 张娟 | A kind of preparation method of enhanced rubber powder modified concrete asphalt mortar |
| CN107674238A (en) * | 2017-10-10 | 2018-02-09 | 山西省交通科学研究院 | A kind of waste rubber powder surface modifying method |
| CN109293320A (en) * | 2018-12-07 | 2019-02-01 | 临沂宏艺科技发展有限公司 | A kind of concrete prepared using modified waste rubber powder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624723A (en) * | 2021-01-13 | 2021-04-09 | 杭州申华混凝土有限公司 | Freeze-thaw resistant concrete and preparation method thereof |
| WO2022165726A1 (en) * | 2021-02-02 | 2022-08-11 | 中国石油化工股份有限公司 | Coated rubber particle, preparation method therefor and use thereof |
| CN116063039A (en) * | 2022-10-25 | 2023-05-05 | 湖南泓盛新型建材有限公司 | Composite heat-insulating building block and preparation method thereof |
| CN116063039B (en) * | 2022-10-25 | 2024-03-19 | 湖南泓盛新型建材有限公司 | Composite heat-insulating building block and preparation method thereof |
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