CN108484996B - Anti-aging magnetic rubber powder and preparation method thereof - Google Patents
Anti-aging magnetic rubber powder and preparation method thereof Download PDFInfo
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- CN108484996B CN108484996B CN201810356160.8A CN201810356160A CN108484996B CN 108484996 B CN108484996 B CN 108484996B CN 201810356160 A CN201810356160 A CN 201810356160A CN 108484996 B CN108484996 B CN 108484996B
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Abstract
The invention discloses anti-aging magnetic rubber powder which is prepared from the following raw materials in parts by weight: anti-aging agent rd1-2, natural rubber powder 100-110, potassium oleate soap 0.4-1, ferrous chloride tetrahydrate 30-40, ferric trichloride hexahydrate 17-20, trimethylolpropane 2-3, 6-hydroxy-2-naphthoic acid 3-4, dibenzothiazyl disulfide 0.1-0.2, catalyst 0.01-0.02 and 10-12% ammonia water 25-30.
Description
Technical Field
The invention belongs to the field of rubber materials, and particularly relates to anti-aging magnetic rubber powder and a preparation method thereof.
Background
Natural Rubber (NR) is a natural polymer compound containing cis-1, 4-polyisoprene as a main component, 91 to 94% of which is rubber hydrocarbon (cis-1, 4-polyisoprene), and the balance of which is non-rubber substances such as protein, fatty acid, ash, saccharides and the like. Natural rubber is the most widely used rubber, the physical properties of natural rubber. Natural rubber has high elasticity at normal temperature, is slightly plastic, has very good mechanical strength, has small hysteresis loss, generates low heat when deformed for many times, and therefore has good flexing resistance, and has good electrical insulation performance because it is nonpolar rubber.
Chemical characteristics of natural rubber. Because of unsaturated double bonds, the natural rubber is a substance with strong chemical reaction capacity, and the aging of the rubber can be promoted by light, heat, ozone, radiation, flexion deformation, copper, manganese and other metals, and the aging resistance is the fatal weakness of the natural rubber, but the natural rubber added with the anti-aging agent still cannot be seen to change greatly after being exposed to sunlight for two months sometimes, and can still be used as usual after being stored in a warehouse for three years;
magnetic nanoparticles are of great interest, especially ferroferric oxide (and nano-iron sesquioxide (nanoparticles, because of their high magnetization, low toxicity, and many practical applications, such as nuclear magnetic resonance contrast enhancers, biological fluids, and the ability to release drugs in the transdermal direction, separate cells, and prepare various materials for magnetic properties);
meanwhile, with the continuous development of composite materials, the application of the traditional single rubber material is limited to a certain extent, so that how to endow the rubber material with new performance is the focus of current research.
Disclosure of Invention
The invention aims to provide anti-aging magnetic rubber powder and a preparation method thereof aiming at the defects and shortcomings of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the aging-resistant magnetic rubber powder is composed of the following raw materials in parts by weight:
anti-aging agent rd1-2, natural rubber powder 100-110, potassium oleate soap 0.4-1, ferrous chloride tetrahydrate 30-40, ferric trichloride hexahydrate 17-20, trimethylolpropane 2-3, 6-hydroxy-2-naphthoic acid 3-4, dibenzothiazyl disulfide 0.1-0.2, catalyst 0.01-0.02 and 10-12% ammonia water 25-30.
The catalyst is p-toluenesulfonic acid.
The preparation method of the aging-resistant magnetic rubber powder comprises the following steps:
(1) adding the anti-aging agent rd into absolute ethyl alcohol with the weight 6-10 times of that of the anti-aging agent rd, uniformly stirring, raising the temperature to 60-65 ℃, and keeping the temperature and stirring for 20-30 minutes to obtain an alcohol solution;
(2) adding natural rubber powder into the alcohol solution, performing ultrasonic treatment for 10-15 minutes, adding dibenzothiazyl disulfide, feeding into an oven, drying at 75-80 deg.C for 3-4 minutes, discharging, and cooling to obtain activated rubber powder;
(3) adding ferrous chloride tetrahydrate and ferric trichloride hexahydrate into deionized water with the weight being 20-30 times of that of the ferrous chloride tetrahydrate, adding the activated rubber powder and trimethylolpropane, raising the temperature to 50-60 ℃, dropwise adding the 10-12% ammonia water, stirring for reaction for 3-4 hours, and discharging to obtain a magnetic rubber powder solution;
(4) adding 6-hydroxy-2-naphthoic acid into the magnetic rubber powder solution, uniformly stirring, adding a catalyst, raising the temperature to 70-75 ℃, keeping the temperature and stirring for 2-3 hours, adding the rest raw materials, stirring to normal temperature, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain the aging-resistant magnetic rubber powder.
The invention has the advantages that:
the method adopts an anti-aging agent rd to treat natural rubber powder, then uses ferrous chloride tetrahydrate and ferric chloride hexahydrate as precursors to prepare magnetic particles under the action of ammonia water, introduces rubber powder treated by trimethylolpropane in the preparation process, blends the obtained magnetic rubber powder with 6-hydroxy-2-naphthoic acid, uses p-toluenesulfonic acid as a catalyst, realizes effective blending of magnetic raw materials and rubber powder, and improves the mechanical stability of finished materials;
the composite rubber powder can be used for manufacturing magnetic cores, permanent magnets, connected and fixed switches and the like, is easy to process, has good dimensional stability and is endowed with magnetism.
Detailed Description
Example 1
The aging-resistant magnetic rubber powder is composed of the following raw materials in parts by weight:
anti-aging agent rd1, natural rubber powder 100, potassium oleate soap 0.4, ferrous chloride tetrahydrate 30, ferric chloride hexahydrate 17, trimethylolpropane 2, 6-hydroxy-2-naphthoic acid 3, dibenzothiazyl disulfide 0.1, catalyst 0.01, and 10% ammonia water 25.
The catalyst is p-toluenesulfonic acid.
The preparation method of the aging-resistant magnetic rubber powder comprises the following steps:
(1) adding the antioxidant rd into absolute ethyl alcohol with the weight 6 times of that of the antioxidant rd, uniformly stirring, raising the temperature to 60 ℃, and keeping the temperature and stirring for 20 minutes to obtain an alcohol solution;
(2) adding natural rubber powder into the alcohol solution, carrying out ultrasonic treatment for 10 minutes, adding dibenzothiazyl disulfide, sending into an oven, drying at 75 ℃ for 3 minutes, discharging and cooling to obtain activated rubber powder;
(3) adding ferrous chloride tetrahydrate and ferric trichloride hexahydrate into deionized water with the weight being 20 times of that of the ferrous chloride tetrahydrate and ferric trichloride hexahydrate, adding the activated rubber powder and trimethylolpropane, raising the temperature to 50 ℃, dropwise adding the 10% ammonia water, stirring for reaction for 3 hours, and discharging to obtain a magnetic rubber powder solution;
(4) adding 6-hydroxy-2-naphthoic acid into the magnetic rubber powder solution, uniformly stirring, adding a catalyst, raising the temperature to 70 ℃, keeping the temperature and stirring for 2 hours, adding the rest raw materials, stirring to normal temperature, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain the aging-resistant magnetic rubber powder.
Example 2
The aging-resistant magnetic rubber powder is composed of the following raw materials in parts by weight:
anti-aging agent rd2, natural rubber powder 110, potassium oleate soap 1, ferrous chloride tetrahydrate 40, ferric trichloride hexahydrate 20, trimethylolpropane 3, 6-hydroxy-2-naphthoic acid 4, dibenzothiazyl disulfide 0.2, catalyst 0.02 and 10-12% ammonia water 30.
The catalyst is p-toluenesulfonic acid.
The preparation method of the aging-resistant magnetic rubber powder comprises the following steps:
(1) adding the antioxidant rd into absolute ethyl alcohol with the weight being 10 times that of the antioxidant rd, uniformly stirring, raising the temperature to 65 ℃, and keeping the temperature and stirring for 30 minutes to obtain an alcohol solution;
(2) adding natural rubber powder into the alcohol solution, carrying out ultrasonic treatment for 15 minutes, adding dibenzothiazyl disulfide, sending into an oven, drying at 80 ℃ for 4 minutes, discharging and cooling to obtain activated rubber powder;
(3) adding ferrous chloride tetrahydrate and ferric trichloride hexahydrate into deionized water 30 times of the weight of the ferrous chloride tetrahydrate and the ferric trichloride hexahydrate, adding the activated rubber powder and the trimethylolpropane, raising the temperature to 60 ℃, dropwise adding the 10-12% ammonia water, stirring for reaction for 4 hours, and discharging to obtain a magnetic rubber powder solution;
(4) adding 6-hydroxy-2-naphthoic acid into the magnetic rubber powder solution, uniformly stirring, adding a catalyst, raising the temperature to 75 ℃, keeping the temperature and stirring for 3 hours, adding the rest raw materials, stirring to normal temperature, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain the aging-resistant magnetic rubber powder.
And (3) performance testing:
the aging-resistant magnetic rubber powder of embodiment 1 of the invention:
tensile strength: 13.9 Mpa;
the saturation magnetization is 10.3 emu/g;
hot air aging test at 70 ℃ for × 70 h:
rate of decrease in tensile strength at break: 3.4%, elongation at break reduction rate: 3.1 percent;
the aging-resistant magnetic rubber powder of embodiment 2 of the invention:
tensile strength: 15.1 Mpa;
the saturation magnetization is 11.8 emu/g;
hot air aging test at 70 ℃ for × 70 h:
rate of decrease in tensile strength at break: 4.0%, elongation at break reduction rate: 3.6 percent.
Claims (2)
1. The preparation method of the aging-resistant magnetic rubber powder is characterized in that the raw materials used in the preparation method are composed of the following raw materials in parts by weight:
anti-aging agent rd1-2, natural rubber powder 100-110, potassium oleate soap 0.4-1, ferrous chloride tetrahydrate 30-40, ferric trichloride hexahydrate 17-20, trimethylolpropane 2-3, 6-hydroxy-2-naphthoic acid 3-4, dibenzothiazyl disulfide 0.1-0.2, catalyst 0.01-0.02, 10-12% ammonia water 25-30;
the preparation method of the aging-resistant magnetic rubber powder is characterized by comprising the following steps:
(1) adding the anti-aging agent rd into absolute ethyl alcohol with the weight 6-10 times of that of the anti-aging agent rd, uniformly stirring, raising the temperature to 60-65 ℃, and keeping the temperature and stirring for 20-30 minutes to obtain an alcohol solution;
(2) adding natural rubber powder into the alcohol solution, performing ultrasonic treatment for 10-15 minutes, adding dibenzothiazyl disulfide, feeding into an oven, drying at 75-80 deg.C for 3-4 minutes, discharging, and cooling to obtain activated rubber powder;
(3) adding ferrous chloride tetrahydrate and ferric trichloride hexahydrate into deionized water with the weight being 20-30 times of that of the ferrous chloride tetrahydrate, adding the activated rubber powder and trimethylolpropane, raising the temperature to 50-60 ℃, dropwise adding the 10-12% ammonia water, stirring for reaction for 3-4 hours, and discharging to obtain a magnetic rubber powder solution;
(4) adding 6-hydroxy-2-naphthoic acid into the magnetic rubber powder solution, uniformly stirring, adding a catalyst, raising the temperature to 70-75 ℃, keeping the temperature and stirring for 2-3 hours, adding the rest raw materials, stirring to normal temperature, performing suction filtration, washing a filter cake with water, and drying at normal temperature to obtain the aging-resistant magnetic rubber powder.
2. The method for preparing the aging-resistant magnetic rubber powder as recited in claim 1, wherein the catalyst is p-toluenesulfonic acid.
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| CN103709462A (en) * | 2013-12-26 | 2014-04-09 | 金猴集团威海鞋业有限公司 | Rubber magnetic shoe sole pad and preparation method thereof |
| CN104893048A (en) * | 2015-05-28 | 2015-09-09 | 安徽同丰橡塑工业有限公司 | Preparation process for magnetic chlorinated rubber |
| CN104927118A (en) * | 2015-06-03 | 2015-09-23 | 中北大学 | Fe3O4/NR magnetic elastomer composite and preparation method thereof |
| CN105622993A (en) * | 2016-01-04 | 2016-06-01 | 桂林电子科技大学 | High-performance magnetic rubber and preparation method thereof |
| CN105694032A (en) * | 2016-03-18 | 2016-06-22 | 赵守彬 | Fiber-modified magnetic composite material and preparation method thereof |
| CN107321324A (en) * | 2017-09-05 | 2017-11-07 | 霍邱金木鱼农业科技有限公司 | A kind of dye discoloration magnetic adsorptive material and preparation method thereof |
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2018
- 2018-04-19 CN CN201810356160.8A patent/CN108484996B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101230156A (en) * | 2007-12-29 | 2008-07-30 | 杨中联 | Magnetic rubber having high magnetic flux density and preparation method thereof |
| CN103709462A (en) * | 2013-12-26 | 2014-04-09 | 金猴集团威海鞋业有限公司 | Rubber magnetic shoe sole pad and preparation method thereof |
| CN104893048A (en) * | 2015-05-28 | 2015-09-09 | 安徽同丰橡塑工业有限公司 | Preparation process for magnetic chlorinated rubber |
| CN104927118A (en) * | 2015-06-03 | 2015-09-23 | 中北大学 | Fe3O4/NR magnetic elastomer composite and preparation method thereof |
| CN105622993A (en) * | 2016-01-04 | 2016-06-01 | 桂林电子科技大学 | High-performance magnetic rubber and preparation method thereof |
| CN105694032A (en) * | 2016-03-18 | 2016-06-22 | 赵守彬 | Fiber-modified magnetic composite material and preparation method thereof |
| CN107321324A (en) * | 2017-09-05 | 2017-11-07 | 霍邱金木鱼农业科技有限公司 | A kind of dye discoloration magnetic adsorptive material and preparation method thereof |
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Effective date of registration: 20230909 Address after: No. 5 Daihan Road, Huanshan Office, Wendeng District, Weihai City, Shandong Province, 264200 Patentee after: Weihai Jianxin rubber and Plastic Technology Co.,Ltd. Address before: 325011 No. 21 Yueqing Road, Zhuang Yuan Street, Longwan District, Wenzhou, Zhejiang. Patentee before: WENZHOU YINGCHUANG NEW MATERIAL TECHNOLOGY Co.,Ltd. |