CN112573560A - Preparation method of high-dispersion zinc oxide - Google Patents
Preparation method of high-dispersion zinc oxide Download PDFInfo
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- CN112573560A CN112573560A CN202011636284.5A CN202011636284A CN112573560A CN 112573560 A CN112573560 A CN 112573560A CN 202011636284 A CN202011636284 A CN 202011636284A CN 112573560 A CN112573560 A CN 112573560A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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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
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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 Kinetics & Catalysis (AREA)
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- Inorganic Chemistry (AREA)
- Tires In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparation method of high-dispersion zinc oxide, which comprises the following specific preparation steps: s1, weighing a certain amount of zinc acetate dihydrate and 1,3, 5-tri (1 triazolyl-methylene) -2,4, 6-trimethylbenzene, adding into a hydrothermal reaction kettle, adding a proper amount of ethanol, ultrasonically dissolving, and reacting for 4-8h at the temperature of 110-130 ℃; s2, adding acetic acid into a hydrothermal reaction kettle to adjust the pH value to 3-5, then adding 5- (1-tetrazole) isophthalic acid, adjusting the temperature to 115-145 ℃, and reacting for 10-12 h; s3, naturally cooling to room temperature, washing the product with absolute ethyl alcohol for 3-5 times, and drying in vacuum to obtain a modified intermediate; s4, subjecting the modified intermediate to fluidized calcination, wherein the fluidized calcination temperature is 300-550 ℃. The invention has small zinc content and specific gravity, can greatly reduce the rolling resistance of the tire, reduce the hysteresis loss and reduce the oil consumption. In addition, the dispersion agent also has excellent dispersion performance, is beneficial to the dispersion of the carbon black or the white carbon black in the sizing material, and can prevent the phenomena of sizing material gelation, agglomeration and the like.
Description
Technical Field
The invention relates to a preparation method of high-dispersion zinc oxide, 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 preparation method of high-dispersion zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc acetate dihydrate and 1,3, 5-tri (1 triazolyl-methylene) -2,4, 6-trimethylbenzene, adding into a hydrothermal reaction kettle, adding a proper amount of ethanol, ultrasonically dissolving, and reacting for 4-8h at the temperature of 110-130 ℃;
s2, adding acetic acid into a hydrothermal reaction kettle to adjust the pH value to 3-5, then adding 5- (1-tetrazole) isophthalic acid, adjusting the temperature to 115-145 ℃, and reacting for 10-12 h;
s3, naturally cooling to room temperature, washing the product with absolute ethyl alcohol for 3-5 times, and drying in vacuum to obtain a modified intermediate;
s4, subjecting the modified intermediate to fluidized calcination, wherein the fluidized calcination temperature is 300-550 ℃.
Preferably, in step S1, the molar ratio of the added amounts of zinc acetate dihydrate, 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethyl and 5- (1-tetrazole) isophthalic acid is 1:0.8-2: 0.5-2.2.
Preferably, in the step S1, the ultrasonic frequency of the ultrasonic dissolution is 22 to 33 kHz.
Preferably, in the step S1, the addition amount of ethanol is 50% to 60% of the total mass of the mixed solution in the step S1.
Preferably, in the step S4, the fluidizing gas velocity for fluidized calcination is 0.2-3L/min.
Has the advantages that: compared with common zinc oxide, the zinc content of the product is low in specific gravity, so that the rolling resistance of a tire can be greatly reduced, the hysteresis loss is reduced, and the oil consumption is reduced. In addition, the dispersion agent also has excellent dispersion performance, is beneficial to the dispersion of the carbon black or the white carbon black in the sizing material, and can prevent the phenomena of sizing material gelation, agglomeration and the like.
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 high-dispersion zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc acetate dihydrate and 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethylbenzene, adding into a hydrothermal reaction kettle, adding a proper amount of ethanol, ultrasonically dissolving (the ultrasonic frequency is 33 kHz), and reacting for 4 hours at the temperature of 110 ℃, wherein the adding amount of the ethanol is 50% of the total mass of the mixed solution, and the molar ratio of the adding amounts of the zinc acetate dihydrate, the 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethyl and the 5- (1-tetrazole) isophthalic acid is 1:0.8: 0.5;
s2, adding acetic acid into a hydrothermal reaction kettle to adjust the pH value to 3, then adding 5- (1-tetrazole) isophthalic acid, adjusting the temperature to 115 ℃, and reacting for 10 hours;
s3, naturally cooling to room temperature, washing the product with absolute ethyl alcohol for 3-5 times, and drying in vacuum to obtain a modified intermediate;
and S4, performing fluidized calcination on the modified intermediate, wherein the fluidized calcination temperature is 300 ℃, and the fluidizing gas speed is 0.2L/min.
Example 2
A preparation method of high-dispersion zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc acetate dihydrate and 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethylbenzene, adding into a hydrothermal reaction kettle, adding a proper amount of ethanol, ultrasonically dissolving (the ultrasonic frequency is 33 kHz), and reacting for 6 hours at 120 ℃;
s2, adding acetic acid into a hydrothermal reaction kettle to adjust the pH value to 5, then adding 5- (1-tetrazole) isophthalic acid, adjusting the temperature to 125 ℃, and reacting for 10 hours, wherein the adding amount of ethanol is 60% of the total mass of the mixed solution in the step S1, and the molar ratio of the adding amounts of zinc acetate dihydrate, 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethyl and 5- (1-tetrazole) isophthalic acid is 1:1: 1.2;
s3, naturally cooling to room temperature, washing the product with absolute ethyl alcohol for 3-5 times, and drying in vacuum to obtain a modified intermediate;
and S4, performing fluidized calcination on the modified intermediate, wherein the fluidized calcination temperature is 400 ℃, and the fluidizing gas speed is 1.5L/min.
Example 3
A preparation method of high-dispersion zinc oxide comprises the following specific preparation steps:
s1, weighing a certain amount of zinc acetate dihydrate and 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethylbenzene, adding into a hydrothermal reaction kettle, adding a proper amount of ethanol, ultrasonically dissolving, and reacting for 8 hours at 130 ℃;
s2, adding acetic acid into a hydrothermal reaction kettle to adjust the pH value to 5, then adding 5- (1-tetrazole) isophthalic acid, adjusting the temperature to 145 ℃, and reacting for 12 hours, wherein the adding amount of ethanol is 60% of the total mass of the mixed solution in the step S1, and the molar ratio of the adding amounts of zinc acetate dihydrate, 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethyl and 5- (1-tetrazole) isophthalic acid is 1: 2: 2.2;
s3, naturally cooling to room temperature, washing the product with absolute ethyl alcohol for 3-5 times, and drying in vacuum to obtain a modified intermediate;
and S4, performing fluidized calcination on the modified intermediate, wherein the fluidized calcination temperature is 550 ℃, and the fluidizing gas speed is 2.2L/min.
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
| Test items | Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 |
| Shore A hardness | 57 | 58 | 59 | 63 |
| Tensile strength/MPa | 27.7 | 28.2 | 29.3 | 23.7 |
| Elongation at break/% | 629 | 634 | 623 | 582 |
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 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. A preparation method of high-dispersion zinc oxide is characterized by comprising the following specific preparation steps:
s1, weighing a certain amount of zinc acetate dihydrate and 1,3, 5-tri (1 triazolyl-methylene) -2,4, 6-trimethylbenzene, adding into a hydrothermal reaction kettle, adding a proper amount of ethanol, ultrasonically dissolving, and reacting for 4-8h at the temperature of 110-130 ℃;
s2, adding acetic acid into a hydrothermal reaction kettle to adjust the pH value to 3-5, then adding 5- (1-tetrazole) isophthalic acid, adjusting the temperature to 115-145 ℃, and reacting for 10-12 h;
s3, naturally cooling to room temperature, washing the product with absolute ethyl alcohol for 3-5 times, and drying in vacuum to obtain a modified intermediate;
s4, subjecting the modified intermediate to fluidized calcination, wherein the fluidized calcination temperature is 300-550 ℃.
2. The method of claim 1, wherein in step S1, the molar ratio of the zinc acetate dihydrate to the 1,3, 5-tris (1-triazolyl-methylene) -2,4, 6-trimethyl and 5- (1-tetrazole) isophthalic acid is 1:0.8-2: 0.5-2.2.
3. The method for preparing highly dispersed zinc oxide according to claim 1, wherein in step S1, the ultrasonic frequency of ultrasonic dissolution is 22 to 33 kHz.
4. The method of claim 1, wherein in step S1, the amount of ethanol added is 50-60% of the total mass of the mixed solution in step S1.
5. The method for preparing highly dispersed zinc oxide according to claim 1, wherein in step S4, the fluidizing gas velocity for fluidized calcination is 0.2-3L/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479184A (en) * | 2022-02-28 | 2022-05-13 | 江苏爱特恩高分子材料有限公司 | Preparation method of high-dispersion zinc oxide |
Citations (4)
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| CN102061023A (en) * | 2010-12-07 | 2011-05-18 | 江苏爱特恩高分子材料有限公司 | Novel rubber antioxidant and preparation method thereof |
| CN102061022A (en) * | 2010-12-07 | 2011-05-18 | 江苏爱特恩高分子材料有限公司 | Novel rubber activator and preparation method thereof |
| CN102602983A (en) * | 2012-04-10 | 2012-07-25 | 南京师范大学 | Method for solvothermal-method synthesis of zinc oxide nano particle assembly assisted by nitrogen-contained organic micromolecule ligand |
| CN104843764A (en) * | 2015-03-31 | 2015-08-19 | 南京工业大学 | Method for preparing nano zinc oxide by fluidized calcination of basic zinc carbonate |
-
2020
- 2020-12-31 CN CN202011636284.5A patent/CN112573560A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061023A (en) * | 2010-12-07 | 2011-05-18 | 江苏爱特恩高分子材料有限公司 | Novel rubber antioxidant and preparation method thereof |
| CN102061022A (en) * | 2010-12-07 | 2011-05-18 | 江苏爱特恩高分子材料有限公司 | Novel rubber activator and preparation method thereof |
| CN102602983A (en) * | 2012-04-10 | 2012-07-25 | 南京师范大学 | Method for solvothermal-method synthesis of zinc oxide nano particle assembly assisted by nitrogen-contained organic micromolecule ligand |
| CN104843764A (en) * | 2015-03-31 | 2015-08-19 | 南京工业大学 | Method for preparing nano zinc oxide by fluidized calcination of basic zinc carbonate |
Non-Patent Citations (1)
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| 刘冬菊: "柔性配体配合物的合成、结构、性质及氧化锌纳米粒子的合成与表征", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479184A (en) * | 2022-02-28 | 2022-05-13 | 江苏爱特恩高分子材料有限公司 | Preparation method of high-dispersion zinc oxide |
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Application publication date: 20210330 |