CN104212204A - Production method for modified silicon dioxide - Google Patents
Production method for modified silicon dioxide Download PDFInfo
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- CN104212204A CN104212204A CN201410407421.6A CN201410407421A CN104212204A CN 104212204 A CN104212204 A CN 104212204A CN 201410407421 A CN201410407421 A CN 201410407421A CN 104212204 A CN104212204 A CN 104212204A
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- silicon dioxide
- coupling agent
- mass ratio
- production method
- dicyclohexylcarbodiimide
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Abstract
A disclosed production method for modified silicon dioxide comprises the following steps: (1) adding silicon dioxide into water, uniformly dispersing, then adding a coupling agent KH-540, and reacting at 250-300 DEG C for 1-2 h, wherein the mass ratio of silicon dioxide to the coupling agent KH-540 is 1:90.1-0.3); and (2) adding isocaprylic acid and dicyclohexylcarbodiimide into the reaction solution of the step (1), reacting at 80-120 DEG C for 2-3 h, cooling and filtering, so as to obtain the modified silicon dioxide, wherein the mass ratio of isocaprylic acid to the coupling agent KH-540 is (0.7-0.9):1, and the mass ratio of dicyclohexylcarbodiimide to the coupling agent KH-540 is (0.1-0.2):1. The obtained modified silicon dioxide has good compatability and dispersity with rubber, and the mixing time of silicon dioxide and rubber can be greatly saved.
Description
Technical field
The present invention relates to a kind of production method of improved silica.
Background technology
Also known as white carbon black on silica industry, and be widely used in the reinforcement of rubber for tire as reinforced additive.Because silicon-dioxide powdery exists the tendency of assembling when rubber disperse, not easily disperse, cause mixing time long.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides a kind of production method of improved silica, to improve the dispersiveness of silicon-dioxide in rubber.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A production method for improved silica, step is as follows:
(1) be added to the water by silicon-dioxide, after being uniformly dispersed, then add coupling agent KH-540, at 250-300 DEG C, react 1-2 hour, the mass ratio of described silicon-dioxide and coupling agent K-540 is 1:(0.1-0.3);
(2) in the reaction solution of step (1), isocaprylic acid and dicyclohexylcarbodiimide is added again, react 2-3 hour at 80-120 DEG C after, cooling, filter, obtain improved silica, the mass ratio of described isocaprylic acid and coupling agent K-540 is (0.7-0.9): 1, and the mass ratio of described dicyclohexylcarbodiimide and coupling agent K-540 is (0.1-0.2): 1.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1
200kg silicon-dioxide powdery is joined in 0.7 ton of water, be stirred to and be uniformly dispersed, and then add the coupling agent KH-540 of 20kg, be heated to 270 DEG C, react after 1 hour, be cooled to 100 DEG C, add 15kg isocaprylic acid and 4kg dicyclohexylcarbodiimide again, at 100 DEG C, be incubated 2 hours, be cooled to room temperature, filter, drying obtains improved silica.
Embodiment 2
300kg silicon-dioxide powdery is joined in 1 ton of water, be stirred to and be uniformly dispersed, and then add the coupling agent KH-540 of 50kg, be heated to 300 DEG C, react after 2 hours, be cooled to 120 DEG C, add 45kg isocaprylic acid and 5kg dicyclohexylcarbodiimide again, at 120 DEG C, be incubated 2.5 hours, be cooled to room temperature, filter, drying obtains improved silica.
Embodiment 3
200kg silicon-dioxide powdery is joined in 0.6 ton of water, be stirred to and be uniformly dispersed, and then add the coupling agent KH-540 of 60kg, be heated to 250 DEG C, react after 1.5 hours, be cooled to 80 DEG C, add 54kg isocaprylic acid and 7kg dicyclohexylcarbodiimide again, at 80 DEG C, be incubated 3 hours, be cooled to room temperature, filter, drying obtains improved silica.
Gained improved silica of the present invention and rubber have good consistency and dispersiveness, and the mixing time saving silicon-dioxide and rubber reaches 30-40%.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. a production method for improved silica, step is as follows:
(1) be added to the water by silicon-dioxide, after being uniformly dispersed, then add coupling agent KH-540, at 250-300 DEG C, react 1-2 hour, the mass ratio of described silicon-dioxide and coupling agent K-540 is 1:(0.1-0.3);
(2) in the reaction solution of step (1), isocaprylic acid and dicyclohexylcarbodiimide is added again, react 2-3 hour at 80-120 DEG C after, cooling, filter, obtain improved silica, the mass ratio of described isocaprylic acid and coupling agent K-540 is (0.7-0.9): 1, and the mass ratio of described dicyclohexylcarbodiimide and coupling agent K-540 is (0.1-0.2): 1.
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CN201410407421.6A CN104212204B (en) | 2014-08-19 | 2014-08-19 | A kind of production method of improved silica |
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CN104212204B CN104212204B (en) | 2016-03-30 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106046645A (en) * | 2016-08-19 | 2016-10-26 | 陈苹 | Antiskid composite material specially used for computer mouse |
CN106543773A (en) * | 2016-11-01 | 2017-03-29 | 蚌埠硅基材料产业技术研究院有限公司 | The scale surface treatment method of the superfine quartz powder of median≤2 μm |
CN107033630A (en) * | 2017-04-24 | 2017-08-11 | 确成硅化学股份有限公司 | A kind of preparation method of silicon rubber white carbon |
CN113041660A (en) * | 2021-03-25 | 2021-06-29 | 浙江皇马科技股份有限公司 | Emulsion type defoaming agent and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101880482A (en) * | 2010-07-12 | 2010-11-10 | 重庆大学 | Method for modifying nano metal oxide by coupling graft |
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2014
- 2014-08-19 CN CN201410407421.6A patent/CN104212204B/en active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101880482A (en) * | 2010-07-12 | 2010-11-10 | 重庆大学 | Method for modifying nano metal oxide by coupling graft |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106046645A (en) * | 2016-08-19 | 2016-10-26 | 陈苹 | Antiskid composite material specially used for computer mouse |
CN106543773A (en) * | 2016-11-01 | 2017-03-29 | 蚌埠硅基材料产业技术研究院有限公司 | The scale surface treatment method of the superfine quartz powder of median≤2 μm |
CN107033630A (en) * | 2017-04-24 | 2017-08-11 | 确成硅化学股份有限公司 | A kind of preparation method of silicon rubber white carbon |
CN107033630B (en) * | 2017-04-24 | 2019-03-29 | 确成硅化学股份有限公司 | A kind of preparation method of silicon rubber white carbon black |
CN113041660A (en) * | 2021-03-25 | 2021-06-29 | 浙江皇马科技股份有限公司 | Emulsion type defoaming agent and preparation method thereof |
CN113041660B (en) * | 2021-03-25 | 2022-07-08 | 浙江皇马科技股份有限公司 | Emulsion type defoaming agent and preparation method thereof |
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