CN112499666A - Method for preparing high-dispersion zinc oxide by recycling alkali-reduced wastewater - Google Patents
Method for preparing high-dispersion zinc oxide by recycling alkali-reduced wastewater Download PDFInfo
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- CN112499666A CN112499666A CN202011621329.1A CN202011621329A CN112499666A CN 112499666 A CN112499666 A CN 112499666A CN 202011621329 A CN202011621329 A CN 202011621329A CN 112499666 A CN112499666 A CN 112499666A
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- C—CHEMISTRY; METALLURGY
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- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- 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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Abstract
The invention discloses a method for preparing high-dispersion zinc oxide by recycling alkali decrement wastewater, and S1, refining terephthalic acid slurry by using the alkali decrement wastewater; s2, adding the refined terephthalic acid slurry and the calcium hydroxide slurry prepared in the step S1 into a crystallizer according to a proportion to react for 0.5-3 h; s3, adding zinc hydroxide slurry into the crystallizer according to a proportion, adjusting the temperature to be 50-60 ℃, then adding ammonia water to adjust the pH value of the solution to be 8-10, and aging for 5-12 h; s4, sequentially carrying out filter pressing and vacuum drying on the aged solution, and then carrying out heat treatment at the temperature of 250-400 ℃ for 0.5h to obtain the high-dispersion nano zinc oxide. Compared with common zinc oxide, the zinc oxide prepared by mixing and modifying the organic polymer with the aromatic double ligand activated group and the zinc oxide has small zinc content and specific gravity, and can greatly reduce the rolling resistance of tires, reduce hysteresis loss and reduce oil consumption.
Description
Technical Field
The invention relates to a method for preparing high-dispersion zinc oxide by recycling alkali-reduced wastewater, which is characterized by belonging to the field of rubber additives.
Background
The European Union REACH regulation, besides making strict restrictions on the oil used on tires, the restrictions on lead content, zinc content and other heavy metal elements are gradually brought into environmental requirements.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the preparation method of the high-dispersion 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 method for preparing high-dispersion zinc oxide by recycling alkali decrement wastewater comprises the following specific preparation steps:
s1, adding coagulant accounting for 5-20% of the mass of the wastewater into the alkali-reduction wastewater, stirring quickly, adjusting the pH value of the wastewater to 10-11, stirring slowly, filtering the fully-stirred wastewater through waste coal slag to obtain a precipitate to obtain a filtrate, adsorbing the filtrate through an activated carbon layer, filtering the filtrate through a waste coal slag layer to obtain a clear solution, adding terephthalic acid powder accounting for 0.05-1% of the mass of the wastewater into the clear solution, slowly adding dilute acid, and standing for 15min after the pH value of the clear solution is reduced to 2-3 to obtain refined terephthalic acid slurry;
s2, adding the refined terephthalic acid slurry and the calcium hydroxide slurry prepared in the step S1 into a crystallizer according to a proportion, adjusting the temperature to be 60-80 ℃, and reacting for 0.5-3 h;
s3, adding zinc hydroxide slurry into the crystallizer according to a proportion, adjusting the temperature to be 50-60 ℃, then adding ammonia water to adjust the pH value of the solution to be 8-10, and aging for 5-12 h;
s4, sequentially carrying out filter pressing and vacuum drying on the aged solution, and then carrying out heat treatment at the temperature of 250-400 ℃ for 0.5h to obtain the high-dispersion nano zinc oxide.
Preferably, the terephthalic acid powder in the step S1 is a 500-mesh or 800-mesh terephthalic acid powder.
Preferably, the coagulant in step S1 is one of polyaluminum chloride, polyferric silicate sulfate or polyaluminum silicate chloride.
Preferably, the calcium hydroxide slurry in step S2 is prepared by dissolving and dispersing solid calcium hydroxide in hot water at 40-80 ℃ and pulping, and the mass concentration of the calcium hydroxide slurry is 15% -25%.
Preferably, the zinc hydroxide slurry is obtained by dissolving and dispersing solid zinc hydroxide in hot water at 70-90 ℃ and pulping, and the mass concentration of the zinc hydroxide slurry is 25-30%.
Preferably, the molar ratio of the terephthalic acid to the calcium hydroxide to the zinc hydroxide is as follows: 0.9-1.2: 0.9-1.1:1.
Has the advantages that: the invention provides a method for preparing high-dispersion zinc oxide by recycling alkali decrement wastewater, which has the following advantages compared with the prior art:
1) compared with common zinc oxide, the zinc oxide prepared by mixing and modifying the organic polymer with the aromatic double ligand activated group and the zinc oxide has small specific gravity of zinc content, can greatly reduce the rolling resistance of tires, reduce hysteresis loss and reduce oil consumption.
2) The dispersion agent has excellent dispersion performance, is beneficial to the dispersion of carbon black or white carbon black in rubber, and can prevent the phenomena of rubber gelation, agglomeration and the like.
3) The organic polymer with the aromatic bidentate ligand activated group is prepared by utilizing the alkali decrement wastewater, three wastes are not generated in the production process, the resource utilization efficiency is improved, and the environmental pollution is reduced.
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 method for preparing high-dispersion zinc oxide by recycling alkali decrement wastewater comprises the following specific preparation steps:
s1, adding polyaluminium chloride accounting for 5% of the mass of the wastewater into the alkali-reduction wastewater, stirring quickly, adjusting the pH value of the wastewater to 11, stirring slowly, filtering the wastewater subjected to full stirring through waste coal slag to obtain a precipitate, adsorbing the precipitate through an activated carbon layer, filtering through a waste coal slag layer to obtain a clear solution, adding terephthalic acid powder accounting for 0.05% of the mass of the wastewater and being screened with a 500-mesh sieve into the clear solution, slowly adding dilute acid, and standing for 15min after the pH value of the clear solution is reduced to 2 to obtain refined terephthalic acid slurry;
s2, adding the refined terephthalic acid slurry and the calcium hydroxide slurry prepared in the step S1 into a crystallizer according to a proportion, adjusting the temperature to be 60-80 ℃, and reacting for 0.5-3h, wherein the calcium hydroxide slurry is prepared by dissolving and dispersing solid calcium hydroxide in hot water at 80 ℃ and pulping, and the mass concentration of the calcium hydroxide slurry is 15%;
s3, adding zinc hydroxide slurry into the crystallizer according to a proportion, adjusting the temperature to 60 ℃, adding ammonia water to adjust the pH value of the solution to 8, and aging for 5 hours, wherein the zinc hydroxide slurry is obtained by dissolving and dispersing solid zinc hydroxide into hot water at 90 ℃ and pulping, the mass concentration of the zinc hydroxide slurry is 25%, and the molar ratio of terephthalic acid, calcium hydroxide and zinc hydroxide is as follows: 0.9: 0.9: 1;
and S4, sequentially carrying out filter pressing and vacuum drying on the aged solution, and then carrying out heat treatment at the temperature of 400 ℃ for 0.5h to obtain the high-dispersion nano zinc oxide.
Example 2
A method for preparing high-dispersion zinc oxide by recycling alkali decrement wastewater comprises the following specific preparation steps:
s1, adding ferric polysilicate sulfate accounting for 15% of the mass of the wastewater into the alkali-reduced wastewater, stirring quickly, adjusting the pH value of the wastewater to 10, stirring slowly, filtering the wastewater subjected to full stirring through waste coal slag to obtain a precipitate to obtain a filtrate, adsorbing the filtrate through an activated carbon layer, filtering through a waste coal slag layer to obtain a clear solution, adding 800-mesh-sieve terephthalic acid powder accounting for 0.5% of the mass of the wastewater into the clear solution, slowly adding dilute acid, and standing for 15min after the pH value of the clear solution is reduced to 3 to obtain refined terephthalic acid slurry;
s2, adding the refined terephthalic acid slurry and the calcium hydroxide slurry prepared in the step S1 into a crystallizer according to a proportion, adjusting the temperature to 80 ℃, and reacting for 3 hours, wherein the calcium hydroxide slurry is obtained by dissolving and dispersing solid calcium hydroxide in hot water at 80 ℃ and pulping, and the mass concentration of the calcium hydroxide slurry is 20%;
and S3, adding zinc hydroxide slurry into the crystallizer according to a ratio, adjusting the temperature to be 60 ℃, adding ammonia water to adjust the pH value of the solution to be 8, and aging for 8 hours, wherein the zinc hydroxide slurry is obtained by dissolving and dispersing solid zinc hydroxide into hot water at 90 ℃ and pulping, the mass concentration of the zinc hydroxide slurry is 30%, and the molar ratio of terephthalic acid, calcium hydroxide and zinc hydroxide is 1: 1: 1;
and S4, sequentially carrying out filter pressing and vacuum drying on the aged solution, and then carrying out heat treatment at the temperature of 400 ℃ for 0.5h to obtain the high-dispersion nano zinc oxide.
Example 3
A method for preparing high-dispersion zinc oxide by recycling alkali decrement wastewater comprises the following specific preparation steps:
s1, adding polyaluminium chloride accounting for 20% of the mass of the wastewater into the alkali-reduction wastewater, stirring quickly, adjusting the pH value of the wastewater to 10, stirring slowly, filtering the wastewater subjected to full stirring through waste coal slag to obtain a precipitate to obtain a filtrate, adsorbing the filtrate through an activated carbon layer, filtering through a waste coal slag layer to obtain a clear solution, adding 800-mesh terephthalic acid powder accounting for 1% of the mass of the wastewater into the clear solution, slowly adding dilute acid, and standing for 15min after the pH value of the clear solution is reduced to 3 to obtain refined terephthalic acid slurry;
s2, adding the refined terephthalic acid slurry and the calcium hydroxide slurry prepared in the step S1 into a crystallizer according to a proportion, adjusting the temperature to 80 ℃, and reacting for 3 hours, wherein the calcium hydroxide slurry is obtained by dissolving and dispersing solid calcium hydroxide in hot water at 80 ℃ and pulping, and the mass concentration of the calcium hydroxide slurry is 25%;
and S3, adding zinc hydroxide slurry into the crystallizer according to a ratio, adjusting the temperature to be 60 ℃, adding ammonia water to adjust the pH value of the solution to be 8, aging for 12 hours, wherein the zinc hydroxide slurry is obtained by dissolving and dispersing solid zinc hydroxide into hot water at 790 ℃ and pulping, the mass concentration of the zinc hydroxide slurry is 30%, and the molar ratio of terephthalic acid, calcium hydroxide and zinc hydroxide is 1.2: 1.1: 1;
and S4, sequentially carrying out filter pressing and vacuum drying on the aged solution, and then carrying out heat treatment at the temperature of 400 ℃ for 0.5h to obtain the high-dispersion nano 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 and scorch time of the rubber compounds obtained by mixing the above samples 1, 2, 3, and 4 were measured according to the national standards, and the test results are specifically shown in table 2.
TABLE 2 Performance test results for each sample
| Test items | Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 |
| Shore A hardness | 61 | 62 | 62 | 65 |
| Tensile strength/MPa | 25.7 | 27.2 | 26.3 | 23.7 |
| Elongation at break/% | 621 | 612 | 603 | 581 |
| 100% stress at definite elongation/MPa | 1.75 | 1.72 | 1.84 | 2.65 |
| Scorch time ts1/min | 6.12 | 6.15 | 6.23 | 5.45 |
The following conclusions can be drawn from the above experimental results: the modified zinc oxide can basically realize the uniform dispersion of the modified zinc oxide in the rubber material at the molecular level 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, the tensile strength and the elongation at break of the rubber material are improved, a certain delay effect on the scorching is realized, and the safety of rubber production is 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 (6)
1. A method for preparing high-dispersion zinc oxide by recycling alkali decrement wastewater is characterized by comprising the following specific preparation steps:
s1, adding coagulant accounting for 5-20% of the mass of the wastewater into the alkali-reduction wastewater, stirring quickly, adjusting the pH value of the wastewater to 10-11, stirring slowly, filtering the fully-stirred wastewater through waste coal slag to obtain a precipitate to obtain a filtrate, adsorbing the filtrate through an activated carbon layer, filtering the filtrate through a waste coal slag layer to obtain a clear solution, adding terephthalic acid powder accounting for 0.05-1% of the mass of the wastewater into the clear solution, slowly adding dilute acid, and standing for 15min after the pH value of the clear solution is reduced to 2-3 to obtain refined terephthalic acid slurry;
s2, adding the refined terephthalic acid slurry and the calcium hydroxide slurry prepared in the step S1 into a crystallizer according to a proportion, adjusting the temperature to be 60-80 ℃, and reacting for 0.5-3 h;
s3, adding zinc hydroxide slurry into the crystallizer according to a proportion, adjusting the temperature to be 50-60 ℃, then adding ammonia water to adjust the pH value of the solution to be 8-10, and aging for 5-12 h;
s4, sequentially carrying out filter pressing and vacuum drying on the aged solution, and then carrying out heat treatment at the temperature of 250-400 ℃ for 0.5h to obtain the high-dispersion nano zinc oxide.
2. The method for preparing highly dispersed zinc oxide by recycling alkali-reduced wastewater according to claim 1, wherein the terephthalic acid powder in step S1 is a 500-mesh or 800-mesh terephthalic acid powder.
3. The method for preparing highly dispersed zinc oxide by recycling alkali-reduced wastewater according to claim 1, wherein the coagulant in step S1 is one of polyaluminum chloride, polyferric silicate sulfate or polyaluminum silicate chloride.
4. The method for preparing highly dispersed zinc oxide by recycling alkali-reduced wastewater according to claim 1, wherein the calcium hydroxide slurry in step S2 is prepared by dissolving and dispersing solid calcium hydroxide and pulping in hot water at 40-80 ℃ and has a mass concentration of 15% -25%.
5. The method for preparing highly dispersed zinc oxide by recycling alkali-reduced wastewater according to claim 1, wherein the zinc hydroxide slurry is obtained by dissolving and dispersing solid zinc hydroxide in hot water at 70-90 ℃ and pulping, and the mass concentration of the zinc hydroxide slurry is 25-30%.
6. The method for preparing highly dispersed zinc oxide by recycling alkali-reduced wastewater according to claim 1, wherein the molar distribution ratio of terephthalic acid, calcium hydroxide and zinc hydroxide is 0.9-1.2: 0.9-1.1:1.
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| CN202011621329.1A CN112499666A (en) | 2020-12-31 | 2020-12-31 | Method for preparing high-dispersion zinc oxide by recycling alkali-reduced wastewater |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503353A (en) * | 2009-03-05 | 2009-08-12 | 浙江大学 | Technique for purifying crude terephthalic acid from alkali deweighting wastewater |
| CN104671506A (en) * | 2015-03-03 | 2015-06-03 | 常州市博洋新材料科技有限公司 | Method for extracting terephthalic acid from alkali-decrement wastewater |
| CN105753687A (en) * | 2016-02-15 | 2016-07-13 | 常州市五洲化工有限公司 | Method for acquiring large-particle terephthalic acid crystals from alkali peeling wastewater |
| CN111499923A (en) * | 2020-04-30 | 2020-08-07 | 常州市五好新材料科技有限公司 | Method for preparing organic calcium molding material by using alkali reduction wastewater |
| CN111607127A (en) * | 2020-06-09 | 2020-09-01 | 江西宝弘纳米科技有限公司 | Rubber vulcanization activator and preparation method and application thereof |
-
2020
- 2020-12-31 CN CN202011621329.1A patent/CN112499666A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503353A (en) * | 2009-03-05 | 2009-08-12 | 浙江大学 | Technique for purifying crude terephthalic acid from alkali deweighting wastewater |
| CN104671506A (en) * | 2015-03-03 | 2015-06-03 | 常州市博洋新材料科技有限公司 | Method for extracting terephthalic acid from alkali-decrement wastewater |
| CN105753687A (en) * | 2016-02-15 | 2016-07-13 | 常州市五洲化工有限公司 | Method for acquiring large-particle terephthalic acid crystals from alkali peeling wastewater |
| CN111499923A (en) * | 2020-04-30 | 2020-08-07 | 常州市五好新材料科技有限公司 | Method for preparing organic calcium molding material by using alkali reduction wastewater |
| CN111607127A (en) * | 2020-06-09 | 2020-09-01 | 江西宝弘纳米科技有限公司 | Rubber vulcanization activator and preparation method and application thereof |
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