CN112574472A - Preparation method of modified zinc oxide - Google Patents
Preparation method of modified zinc oxide Download PDFInfo
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- CN112574472A CN112574472A CN202011636351.3A CN202011636351A CN112574472A CN 112574472 A CN112574472 A CN 112574472A CN 202011636351 A CN202011636351 A CN 202011636351A CN 112574472 A CN112574472 A CN 112574472A
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- zinc oxide
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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
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Tires In General (AREA)
Abstract
The invention discloses a preparation method of modified zinc oxide, S1, weighing a certain amount of zinc oxide and water, and mixing to obtain zinc oxide suspension; s2, adding a certain amount of dimethyl imidazole into the suspension, and performing ultrasonic mixing to obtain an intermediate mixed solution; and S3, adding a certain amount of octadecyl triethoxy silane and bisphenol A polyoxyethylene ether into the intermediate mixed solution, ultrasonically mixing, adjusting the temperature to 55-95 ℃, reacting for 40-60min, performing suction filtration and washing, and performing vacuum drying to obtain the modified zinc oxide. The invention can effectively reduce zinc pollution in the tire rubber material and the weight of the tire without influencing the vulcanization performance of the rubber, thereby realizing energy conservation and emission reduction.
Description
Technical Field
The invention relates to a preparation method of modified zinc oxide, belonging to the field of rubber additives.
Background
In addition to strict restrictions on the oils used in tires, the european union REACH regulations are also gradually meeting environmental requirements for the content of lead, zinc and other heavy metals. As an activator, zinc oxide is used in a large amount in the rubber industry, but during the production, handling and recovery of rubber products, zinc is easily released to the environment by abrasion of tires, and the release of zinc has a very adverse effect on the environment, human health and particularly on aquatic life, so that it is required that the zinc content in the rubber compound is as low as possible.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the preparation method of the modified zinc oxide, which can effectively reduce zinc pollution in tire rubber materials and the weight of tires while not influencing the vulcanization performance of rubber, thereby realizing energy conservation and emission reduction.
The invention mainly adopts the technical scheme that:
a preparation method of modified zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc oxide and water, and mixing to obtain a zinc oxide suspension, wherein the zinc oxide accounts for 40-65% of the total mass of the suspension;
s2, adding a certain amount of dimethyl imidazole into the suspension, ultrasonically mixing, and reacting at 60-80 ℃ for 20-60min to obtain an intermediate mixed solution;
and S3, adding a certain amount of octadecyl triethoxy silane and bisphenol A polyoxyethylene ether into the intermediate mixed liquid obtained in the step S2, ultrasonically mixing, adjusting the temperature to 55-95 ℃, reacting for 40-60min, performing suction filtration and washing, and performing vacuum drying to obtain the modified zinc oxide.
Preferably, the molar ratio of the dimethyl imidazole to the zinc oxide in the step S2 is 2-4: 1.
Preferably, in the steps S2 and S3, the ultrasonic frequency of the ultrasonic dissolution is 22-33 kHz.
Preferably, in the step S3, the addition amount of the octadecyl triethoxy silane is 1-58% of the mass of the zinc oxide.
Preferably, in the step S3, the addition amount of the bisphenol a polyoxyethylene ether in the step S3 is 1-60% of the mass of the zinc oxide.
Has the advantages that: the invention provides a preparation method of modified zinc oxide, which has the following advantages compared with the prior art:
1. the surface of the zinc oxide particles and the dimethyl imidazole are subjected to coordination reaction to form a porous metal organic framework structure which can be in better interface contact with other additives in a rubber mixing formula, so that the compatibility of the zinc oxide in the rubber is improved;
2. the octadecyl triethoxy silane can be subjected to water phase modification with zinc oxide under the action of amphipathy of bisphenol A polyoxyethylene ether, the octadecyl triethoxy silane is wrapped by the bisphenol A polyoxyethylene ether to form suspension liquid drops, and hydrophobic long-chain alkyl is introduced to the surface of the zinc oxide, so that the dispersibility of the zinc oxide is improved, and the coagulation phenomenon of the zinc oxide is prevented.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Example 1
A preparation method of modified zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc oxide and water, and mixing to obtain a zinc oxide suspension, wherein the zinc oxide accounts for 40% of the total mass of the suspension;
s2, adding a certain amount of dimethyl imidazole (the molar ratio of dimethyl imidazole to zinc oxide is 2: 1) into the suspension, ultrasonically mixing, and reacting at 60 ℃ for 40min to obtain an intermediate mixed solution;
and S3, adding a certain amount of octadecyl triethoxy silane (23 percent of the mass of the zinc oxide) and bisphenol A polyoxyethylene ether (24 percent of the mass of the zinc oxide) into the intermediate mixed liquid obtained in the step S2, ultrasonically mixing, adjusting the temperature to 55 ℃, reacting for 30min, performing suction filtration and washing, and performing vacuum drying to obtain the modified zinc oxide.
Example 2
A preparation method of modified zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc oxide and water, and mixing to obtain a zinc oxide suspension, wherein the zinc oxide accounts for 50% of the total mass of the suspension;
s2, adding a certain amount of dimethyl imidazole (the molar ratio of dimethyl imidazole to zinc oxide is 3: 1) into the suspension, ultrasonically mixing (the ultrasonic frequency is 22 kHz), and reacting at 70 ℃ for 40min to obtain an intermediate mixed solution;
and S3, adding a certain amount of octadecyl triethoxy silane (45 percent of the mass of the zinc oxide) and bisphenol A polyoxyethylene ether (45 percent of the mass of the zinc oxide) into the intermediate mixed liquid obtained in the step S2, ultrasonically mixing, adjusting the temperature to 75 ℃, reacting for 30min, performing suction filtration and washing, and performing vacuum drying to obtain the modified zinc oxide.
Example 3
A preparation method of modified zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc oxide and water, and mixing to obtain a zinc oxide suspension, wherein the zinc oxide accounts for 65% of the total mass of the suspension;
s2, adding a certain amount of dimethyl imidazole (the molar ratio of dimethyl imidazole to zinc oxide is 4: 1) into the suspension, ultrasonically mixing (the ultrasonic frequency is 33 kHz), and reacting at 80 ℃ for 30min to obtain an intermediate mixed solution;
and S3, adding a certain amount of octadecyl triethoxy silane (58% of the mass of the zinc oxide) and bisphenol A polyoxyethylene ether (60% of the mass of the zinc oxide) into the intermediate mixed liquid obtained in the step S2, ultrasonically mixing, adjusting the temperature to 95 ℃, reacting for 30min, performing suction filtration and washing, and performing vacuum drying to obtain the modified zinc oxide.
Examples 1, 2 and 3 and ordinary zinc oxide were kneaded according to the kneading formulations shown in table 1 to obtain sample 1, sample 2, sample 3 and sample 4, respectively.
Table 1: the addition amount of each component in the mixing formula
The physical and mechanical properties of the rubber compounds obtained by mixing the above samples 1, 2, 3 and 4 were measured according to the national standards, and the results are shown in table 2.
TABLE 2 results of measuring physical and mechanical properties of each sample
The following conclusions can be drawn from the above experimental results: the modified zinc oxide can basically realize the uniform dispersion on the molecular level in the rubber material and can fully react with other auxiliary agents during vulcanization, so that a certain amount of cross-linked networks with uniform distribution are generated in the vulcanized rubber, the network chains can uniformly bear stress, and the tensile strength and the elongation at break of the rubber material are improved. In addition, in the mixing formula, the addition amount of the modified zinc oxide is less than that of the common zinc oxide, so that the performance of the modified zinc oxide is not influenced, the mechanical property of the rubber is further improved, and the zinc pollution in the tire rubber material is favorably reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. The preparation method of the modified zinc oxide is characterized by comprising the following specific preparation steps:
s1, weighing a certain amount of zinc oxide and water, and mixing to obtain a zinc oxide suspension, wherein the zinc oxide accounts for 40-65% of the total mass of the suspension;
s2, adding a certain amount of dimethyl imidazole into the suspension, ultrasonically mixing, and reacting at 60-80 ℃ for 20-60min to obtain an intermediate mixed solution;
and S3, adding a certain amount of octadecyl triethoxy silane and bisphenol A polyoxyethylene ether into the intermediate mixed liquid obtained in the step S2, ultrasonically mixing, adjusting the temperature to 55-95 ℃, reacting for 40-60min, performing suction filtration and washing, and performing vacuum drying to obtain the modified zinc oxide.
2. The method of claim 1, wherein the molar ratio of dimethylimidazole to zinc oxide in step S2 is 2-4: 1.
3. The method of claim 1, wherein the ultrasonic dissolving is performed at a frequency of 22kHz to 33kHz in the steps S2 and S3.
4. The method for preparing highly dispersed zinc oxide according to claim 1, wherein in step S3, the amount of octadecyltriethoxysilane added is 1% -58% by mass of zinc oxide.
5. The method of claim 1, wherein in step S3, the bisphenol A polyoxyethylene ether is added in an amount of 1-60% by mass of the zinc oxide in step S3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202011636351.3A CN112574472A (en) | 2020-12-31 | 2020-12-31 | Preparation method of modified zinc oxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011636351.3A CN112574472A (en) | 2020-12-31 | 2020-12-31 | Preparation method of modified zinc oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113439984A (en) * | 2021-09-01 | 2021-09-28 | 南通铭源纺织有限公司 | Heating wear-resistant carpet and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107867712A (en) * | 2016-07-07 | 2018-04-03 | 安徽省含山县锦华氧化锌厂 | A kind of active nano-ZnO |
| US20190284364A1 (en) * | 2016-05-16 | 2019-09-19 | Harima Chemicals, Incorporated | Filler for tires, rubber composition for tires, tire, method for producing filler for tires, and aggregation inhibitor |
-
2020
- 2020-12-31 CN CN202011636351.3A patent/CN112574472A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190284364A1 (en) * | 2016-05-16 | 2019-09-19 | Harima Chemicals, Incorporated | Filler for tires, rubber composition for tires, tire, method for producing filler for tires, and aggregation inhibitor |
| CN107867712A (en) * | 2016-07-07 | 2018-04-03 | 安徽省含山县锦华氧化锌厂 | A kind of active nano-ZnO |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113439984A (en) * | 2021-09-01 | 2021-09-28 | 南通铭源纺织有限公司 | Heating wear-resistant carpet and preparation method thereof |
| CN113439984B (en) * | 2021-09-01 | 2021-11-02 | 南通铭源纺织有限公司 | Heating wear-resistant carpet and preparation method thereof |
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Application publication date: 20210330 |