CN101514263A - Modified white carbon black and preparation method thereof - Google Patents
Modified white carbon black and preparation method thereof Download PDFInfo
- Publication number
- CN101514263A CN101514263A CNA2009100300857A CN200910030085A CN101514263A CN 101514263 A CN101514263 A CN 101514263A CN A2009100300857 A CNA2009100300857 A CN A2009100300857A CN 200910030085 A CN200910030085 A CN 200910030085A CN 101514263 A CN101514263 A CN 101514263A
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- China
- Prior art keywords
- carbon black
- white carbon
- modified
- coupling agent
- modified white
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Abstract
The invention discloses a modified white carbon black and a preparation method thereof, belonging to the technical field of non-metallic inorganic material. The silane coupling agent modification treatment is firstly carried out on the white carbon black, then stearic acid solid is put into acetone solution to be dissolved; according to the mass ratio, the adding quantity of stearic acid is 1:1-2:1 of coupling agent; the white carbon black modified by the silane coupling agent is added into the mixed solution, and the modified white carbon black powder is obtained after being dried; the surface of the modified white carbon black powder contains CH3(CH2)16-CONH-(CH2)-Si-O-Si radical. The modified white carbon black prepared by the technical proposal of the invention has even particle size and high white content; meanwhile, as the surface of the modified white carbon black contains CH3(CH2)16 radical, hydrophobic oleophylic property of the white carbon black that is modified for a second time is good. The invention uses the coupling agent and the stearic acid which are low in price and has simple preparation technique. Therefore, the modified white carbon black prepared by the method has low cost and is favorable to large-scale popularization and application.
Description
Technical field
The present invention relates to a kind ofly, particularly a kind of modified white carbon black and preparation method thereof belongs to technical field of inorganic nonmetallic materials.
Background technology
The chemical name of white carbon black is hydration soft silica or colloid silica (SiO
2NH
2O), be a kind of white, nontoxic, amorphous fine meal, excellent properties such as have that porous, specific surface area are big, high dispersive, light weight, chemical stability are good, high temperature resistant, do not burn, electrical insulating property is good as a kind of new inorganic material, is widely used in all trades and professions of national economy.Now, the white carbon black in the whole world about 70% is mainly used in rubber industry, and it can improve cementing property and tear strength as a kind of good rubber reinforcing filler, and performance is far superior to ordinary carbon black.Yet, because the activated silica alcohol radical that the white carbon black outside surface exists makes it be wetting ability, in organic phase, be difficult to moistening and dispersion, and, because the hydroxyl that its surface exists makes its surface energy bigger, particle always tends to cohesion, thereby the application performance of product is affected, and need improve the consistency of they and organic materials by surface modification.White carbon black is after modification, because the surface inserted lipophilicity hydrophobic group, thereby improves the affinity of itself and organic materials, has reduced particle agglomeration, so improved its effect, has expanded its Application Areas.
At present, method of modifying is mostly adopted in the white carbon black modification one time, promptly by being modified as lipophilic group with properties-correcting agent generation chemical reaction hydrophilic radical that it is surperficial.Used properties-correcting agent is mainly now: organochlorosilane, siloxanes, silane coupling agent and alcohol compound etc.Though with silane coupler modified, its performance reaches certain lipophilic-hydrophobic property, still can not meet the demands under the situation that the organism consistency is had relatively high expectations.
Summary of the invention
In order to overcome the deficiency that prior art exists, the invention provides a kind of lipophilic-hydrophobic property that can effectively improve white carbon black, strengthen modified white carbon black of itself and organic Additive consistency and preparation method thereof.
For achieving the above object, technical scheme of the present invention is: a kind of modified white carbon black, and at the surface grafting CH of white carbon black
3(CH
2)
16-CONH-(CH
2)-Si-O-Si group.
The preparation method of above-mentioned modified white carbon black, step is as follows:
1. press mass ratio, water: alcohol=1: 6～1: 9 preparation aqueous ethanolic solution, white carbon black is dissolved in the above-mentioned solution, fully disperse, slowly drip silane coupling agent, the add-on of silane coupling agent is 1～10% of a white carbon black quality, be warming up to 100～130 ℃ gradually, high-speed stirring 1.5～3 hours is reduced to room temperature, drying, obtains silane coupler modified white carbon black;
2. place acetone soln to dissolve the stearic acid solid, press mass ratio, stearic add-on is 1: 1～2: 1 of coupling agent, add the white carbon black after silane coupler modified again, fully stirred 1～3 hour, after centrifugation is handled, use organic solvent washing 1～3 time, obtain the modified white carbon black powder after the drying, CH is contained on its surface
3(CH
2)
16-CONH-(CH
2)-Si-O-Si group.
Silane coupling agent of the present invention is a γ-An Bingjisanyiyangjiguiwan.
The present invention adopts silane coupling agent and stearic acid that white carbon black is carried out twice-modified processing, and its principle is: silane coupling agent γ-An Bingjisanyiyangjiguiwan, molecular formula are H
2N (CH
2)
3Si (OC
2H
5)
3, wherein ,-OC
2H
5Group is a hydrolysable group, the silane coupling agent γ-An Bingjisanyiyangjiguiwan can be decomposed in less water generate silanol and ethanol, and its reaction formula is:
H
2N(CH
2)
3Si(OC
2H
5)
3+H
2O-H
2N(CH
2)
3Si(OH)
3+C
2H
5OH
React between the Si-OH group on white carbon black surface and the silanol, form the covering shape material of crosslinking structures such as chemical bond, hydrogen bond, physical adsorption, after the drying, in surface adhesion, form the Si-O-Si key, promptly surperficial final group is H
2N-(CH
2)-Si-O-Si group; Stearic molecular formula is CH
3(CH
2)
16COOH, it contains-the COOH group, energy and H
2N-(CH
2In the)-Si-O-Si group-H
2The N group forms amide group (CONH), at the final CH of formation in white carbon black surface
3(CH
2)
16-CONH-(CH
2)-Si-O-Si group, wherein CH
3(CH
2)
16The hydrophobic oleophylic performance of group is very good.
Because the utilization of technique scheme, compared with prior art, the present invention has the following advantages:
1. the modified white carbon black epigranular of technical solution of the present invention preparation, the whiteness height, after tested, it reaches 130～150 degree with the contact angle of dibutyl phthalate (DBP) (DBP), is 15～25 to spend with the contact angle of water, and oil-absorption(number) reaches 4～5cm
3/ g, modified effect is good.
2. coupling agent used in the present invention and stearic acid are cheap, and preparation technology is simple, and therefore, the cost of its preparation modified white carbon black is low, helps large-scale promotion and uses.
3. the reagent that uses in the present invention's reaction can be recycled; Reaction product is water and ethanol, and required reagent is nontoxic, and is pollution-free.
Description of drawings
Fig. 1 is the infrared spectrogram of the modified white carbon black powder of the technical scheme preparation that provides by the embodiment of the invention 1.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further described.
Embodiment 1:
Get the 500g white carbon black, 4.5L ethanol, 0.5L water, 30g silane coupling agent γ-An Bingjisanyiyangjiguiwan adopts JH-A110, puts into there-necked flask, adds condensing works, rises to 110 ℃, is incubated 1.5 hours, fully stirs, and take out the cooling back, filter wash, oven dry;
Join 5L acetone, with the dissolving of 40g stearic acid, the white carbon black of the first step modification is put into, fully stirred 1 hour, use organic solvent washing, drying obtains the modified white carbon black powder product.
Referring to accompanying drawing 1, it is the infrared spectrogram of the modified white carbon black powder of present embodiment preparation.As seen from Figure 1: curve is respectively at 1647.062cm among the figure
-1And 1544.9cm
-1The flexural vibration absorption peak that acid amides C=0 stretching vibration absorption and N-H occur is at 2850cm
-1And 2950cm
-1Appearance-CH and-CH
2Group stretching vibration absorption peak proves that silane coupling agent and stearic acid all have been grafted on silica particles, and its surface grafting group is CH
3(CH
2)
16-CONH-(CH
2)-Si-O-Si.
After tested, the contact angle of product and DBP is 140 degree, with the contact angle of water be 22 degree, oil-absorption(number) 4.5cm
3/ g.
Embodiment 2:
Get the 500g white carbon black, 4.5L ethanol, 0.5L water, 25g silane coupling agent JH-A110 puts into there-necked flask, adds condensing works, rises to 120 ℃, insulation 2h, and fully stir, take out the cooling back, filter wash, oven dry; Secondly, join 5L acetone, the 30g stearic acid is put into the white carbon black of the first step modification, fully stirs 1.5h, uses solvent wash, and drying promptly gets product at last.Product performance: with DBP contact angle 130 degree, with water 25 degree, oil-absorption(number) 4.2cm
3/ g.
Embodiment 3:
Get the 500g white carbon black, 4.5L ethanol, 0.5L water, 40g silane coupling agent JH-A110 puts into there-necked flask, adds condensing works, rises to 120 ℃, insulation 1.5h, and fully stir, take out the cooling back, filter wash, oven dry; Secondly, join 5L acetone, the 60g stearic acid is put into the white carbon black of the first step modification, fully stirs 1.5h, uses solvent wash, and drying promptly gets product at last.Product performance: with DBP contact angle 145 degree, with water contact angle 18 degree, oil-absorption(number) 4.7cm
3/ g.
Claims (3)
1. a modified white carbon black is characterized in that: at the surface grafting CH of white carbon black
3(CH
2)
16-CONH-(CH
2)-Si-O-Si group.
2. the preparation method of a modified white carbon black is characterized in that step is as follows:
(1) preparation aqueous ethanolic solution, by quality than water: alcohol=1: 6～1: 9, white carbon black is dissolved in the above-mentioned solution, fully disperse, slowly drip silane coupling agent, the add-on of silane coupling agent is 1～10% of a white carbon black quality, be warming up to 100～130 ℃ gradually, high-speed stirring 1.5～3 hours is reduced to room temperature, drying, obtains silane coupler modified white carbon black;
(2) place acetone soln to dissolve the stearic acid solid, press mass ratio, stearic add-on is 1: 1～2: 1 of coupling agent, add silane coupler modified white carbon black again, fully stirred 1～3 hour, after centrifugation is handled, use organic solvent washing powder 1～3 time, obtain the modified white carbon black powder after the drying, its surface grafting CH
3(CH
2)
16-CONH-(CH
2)-Si-O-Si group.
3. the preparation method of a kind of modified white carbon black according to claim 2, it is characterized in that: described silane coupling agent is a γ-An Bingjisanyiyangjiguiwan.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100300857A CN101514263A (en) | 2009-04-01 | 2009-04-01 | Modified white carbon black and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100300857A CN101514263A (en) | 2009-04-01 | 2009-04-01 | Modified white carbon black and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101514263A true CN101514263A (en) | 2009-08-26 |
Family
ID=41038888
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2009100300857A Pending CN101514263A (en) | 2009-04-01 | 2009-04-01 | Modified white carbon black and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101514263A (en) |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229758A (en) * | 2011-04-06 | 2011-11-02 | 福建正盛无机材料股份有限公司 | Preparation method of high dispersed white carbon black |
| CN102504613A (en) * | 2011-11-11 | 2012-06-20 | 山东久隆高分子材料有限公司 | Preparation method of modified fumed silica for LED packaging reinforcement |
| CN103015041A (en) * | 2013-01-14 | 2013-04-03 | 江苏领瑞新材料科技有限公司 | Preparation method of white carbon black enhanced UHMWPE (ultrahigh molecular weight polyethylene) fiber composite non-weft fabric |
| CN104073029A (en) * | 2014-06-24 | 2014-10-01 | 宋雨谦 | Method for producing lightweight shale opal powder |
| CN104629494A (en) * | 2015-01-29 | 2015-05-20 | 苏州大学 | Polycarboxyl silicon dioxide nanoparticles and preparation method thereof |
| CN104910649A (en) * | 2015-04-23 | 2015-09-16 | 信阳核工业恒达实业公司 | Quartz powder surface active composite modification method |
| CN105214626A (en) * | 2015-11-11 | 2016-01-06 | 刘沐琛 | A kind of slaughterhouse oiliness sewage treatment agent based on modified hydrophobic oil suction solid fraction white carbon and preparation method |
| CN106833027A (en) * | 2017-01-12 | 2017-06-13 | 温州市炬邦新材料有限公司 | A kind of improved silica production technology |
| CN107602964A (en) * | 2017-09-27 | 2018-01-19 | 三浦橡胶（无锡）有限公司 | A kind of rubber composition, preparation method and include its tire |
| CN107722380A (en) * | 2017-09-27 | 2018-02-23 | 三浦橡胶（无锡）有限公司 | A kind of environment-friendlyinner inner tire and its production method |
| CN107973935A (en) * | 2017-12-07 | 2018-05-01 | 沈阳化工大学 | A kind of modified white carbon black and preparation method thereof |
| CN108467609A (en) * | 2018-03-30 | 2018-08-31 | 江苏新亿源环保科技有限公司 | A kind of preparation method of modified hydrophobic dispersing type white carbon |
| CN108862288A (en) * | 2018-07-26 | 2018-11-23 | 安徽锦华氧化锌有限公司 | A kind of processing method of yellowing-resistant white carbon black |
| CN108948797A (en) * | 2018-07-18 | 2018-12-07 | 武汉金牛经济发展有限公司 | A kind of preparation method of modified manometer silicon dioxide |
| CN109096799A (en) * | 2018-08-03 | 2018-12-28 | 蚌埠市万科硅材料科技有限公司 | A kind of tire twice-modified white carbon black |
| CN110003527A (en) * | 2019-04-10 | 2019-07-12 | 合肥华凌股份有限公司 | Modified aerogels, hard polyurethane foams and preparation method thereof, electric appliance |
| CN111777873A (en) * | 2019-04-04 | 2020-10-16 | 深圳先进技术研究院 | Surface modification method of nano silicon dioxide |
| CN111812141A (en) * | 2020-07-10 | 2020-10-23 | 赛轮集团股份有限公司 | Test method for evaluating coupling capacity of white carbon black and silane coupling agent |
| CN112280526A (en) * | 2020-09-21 | 2021-01-29 | 平湖阿莱德实业有限公司 | High-thermal-conductivity self-leveling modified ceramic liquid encapsulating material and preparation method thereof |
| CN115651424A (en) * | 2022-10-24 | 2023-01-31 | 山东阳谷华泰化工股份有限公司 | Preparation method of modified white carbon black and obtained product |
-
2009
- 2009-04-01 CN CNA2009100300857A patent/CN101514263A/en active Pending
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229758A (en) * | 2011-04-06 | 2011-11-02 | 福建正盛无机材料股份有限公司 | Preparation method of high dispersed white carbon black |
| CN102229758B (en) * | 2011-04-06 | 2013-09-11 | 福建正盛无机材料股份有限公司 | Preparation method of high dispersed white carbon black |
| CN102504613A (en) * | 2011-11-11 | 2012-06-20 | 山东久隆高分子材料有限公司 | Preparation method of modified fumed silica for LED packaging reinforcement |
| CN103015041A (en) * | 2013-01-14 | 2013-04-03 | 江苏领瑞新材料科技有限公司 | Preparation method of white carbon black enhanced UHMWPE (ultrahigh molecular weight polyethylene) fiber composite non-weft fabric |
| CN104073029A (en) * | 2014-06-24 | 2014-10-01 | 宋雨谦 | Method for producing lightweight shale opal powder |
| CN104629494A (en) * | 2015-01-29 | 2015-05-20 | 苏州大学 | Polycarboxyl silicon dioxide nanoparticles and preparation method thereof |
| CN104910649A (en) * | 2015-04-23 | 2015-09-16 | 信阳核工业恒达实业公司 | Quartz powder surface active composite modification method |
| CN105214626A (en) * | 2015-11-11 | 2016-01-06 | 刘沐琛 | A kind of slaughterhouse oiliness sewage treatment agent based on modified hydrophobic oil suction solid fraction white carbon and preparation method |
| CN105214626B (en) * | 2015-11-11 | 2018-01-23 | 刘沐琛 | A kind of slaughterhouse oiliness sewage treatment agent and preparation method based on modified hydrophobic oil suction solid fraction white carbon |
| CN106833027A (en) * | 2017-01-12 | 2017-06-13 | 温州市炬邦新材料有限公司 | A kind of improved silica production technology |
| CN107602964A (en) * | 2017-09-27 | 2018-01-19 | 三浦橡胶（无锡）有限公司 | A kind of rubber composition, preparation method and include its tire |
| CN107722380A (en) * | 2017-09-27 | 2018-02-23 | 三浦橡胶（无锡）有限公司 | A kind of environment-friendlyinner inner tire and its production method |
| CN107973935A (en) * | 2017-12-07 | 2018-05-01 | 沈阳化工大学 | A kind of modified white carbon black and preparation method thereof |
| CN108467609A (en) * | 2018-03-30 | 2018-08-31 | 江苏新亿源环保科技有限公司 | A kind of preparation method of modified hydrophobic dispersing type white carbon |
| CN108948797A (en) * | 2018-07-18 | 2018-12-07 | 武汉金牛经济发展有限公司 | A kind of preparation method of modified manometer silicon dioxide |
| CN108862288A (en) * | 2018-07-26 | 2018-11-23 | 安徽锦华氧化锌有限公司 | A kind of processing method of yellowing-resistant white carbon black |
| CN109096799A (en) * | 2018-08-03 | 2018-12-28 | 蚌埠市万科硅材料科技有限公司 | A kind of tire twice-modified white carbon black |
| CN111777873A (en) * | 2019-04-04 | 2020-10-16 | 深圳先进技术研究院 | Surface modification method of nano silicon dioxide |
| CN110003527A (en) * | 2019-04-10 | 2019-07-12 | 合肥华凌股份有限公司 | Modified aerogels, hard polyurethane foams and preparation method thereof, electric appliance |
| CN111812141A (en) * | 2020-07-10 | 2020-10-23 | 赛轮集团股份有限公司 | Test method for evaluating coupling capacity of white carbon black and silane coupling agent |
| CN112280526A (en) * | 2020-09-21 | 2021-01-29 | 平湖阿莱德实业有限公司 | High-thermal-conductivity self-leveling modified ceramic liquid encapsulating material and preparation method thereof |
| WO2022057083A1 (en) * | 2020-09-21 | 2022-03-24 | 平湖阿莱德实业有限公司 | High-thermal-conductivity self-leveling modified ceramic liquid potting material and preparation method therefor |
| CN115651424A (en) * | 2022-10-24 | 2023-01-31 | 山东阳谷华泰化工股份有限公司 | Preparation method of modified white carbon black and obtained product |
| CN115651424B (en) * | 2022-10-24 | 2024-01-23 | 山东阳谷华泰化工股份有限公司 | Preparation method of modified white carbon black and obtained product |
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Open date: 20090826 |