CN104909373A - Preparation method of white carbon black having high oil factor - Google Patents
Preparation method of white carbon black having high oil factor Download PDFInfo
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- CN104909373A CN104909373A CN201510294599.9A CN201510294599A CN104909373A CN 104909373 A CN104909373 A CN 104909373A CN 201510294599 A CN201510294599 A CN 201510294599A CN 104909373 A CN104909373 A CN 104909373A
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Abstract
The invention provides a preparation method of white carbon black having a high oil factor. The preparation method comprises the steps of (1) dissolving solid sodium silicate Na2O.nSiO2 with water to form a Na2OSiO3 solution, and regulating the concentration of the Na2OSiO3 solution to 0.3-0.6mol/L; (2) heating to 80-100 DEG C, adding concentrated sulfuric acid for neutralization until the pH value of the terminal point is 9-11, further adding a 4-6mol/L sulfuric acid solution, and stirring and reacting for 50-70 min until the pH value of the terminal point is 5-6; (3) cooling to 60-70 DEG C, and aging for 20-25 min to obtain slurry; (4) cooling the slurry to 40-60 DEG C, regulating the pH value to 2-5, carrying out filter pressing, and washing to obtain a wet filter cake; and (5) dispersing the wet filter cake into a mixed water solution of propyl alcohol and ethyl alcohol, heating while stirring, refluxing, filtering in vacuum and drying to obtain the white carbon black. The white carbon black obtained by adopting the method provided by the invention has an oil factor being as high as 3.1cm<3>/g.
Description
Technical field
The present invention relates to a kind of preparation method of white carbon black of high oil-absorption(number).
Background technology
White carbon black is the general name of white powder X-ray amorphous silicic acid and silicate product, mainly refers to precipitated silica, aerosil, superfine silicon dioxide gel and aerogel, also comprises Powdered synthetic aluminium silicate and Calucium Silicate powder etc.White carbon black is porous material, and it forms available SiO
2nH
2o represents, wherein nH
2o exists with the form of surface hydroxyl.White carbon black can be dissolved in caustic alkali and hydrofluoric acid, the acid beyond water insoluble, solvent and hydrofluoric acid, have high temperature resistant, do not fire, tasteless, odorless, good electrical insulating property.White carbon black, as the auxiliary agent of a kind of environmental protection, excellent performance, is mainly used in rubber item (comprising high-temperature silicon disulfide rubber), weaving, papermaking, agricultural chemicals, foodstuff additive field.
The index of white carbon black oil-absorption(number) embodies a key property of white carbon black secondary structure, in the Application Areas of white carbon black, requires that the oil-absorption(number) of white carbon black at least reaches more than 2.5.
Summary of the invention
The invention provides a kind of preparation method of white carbon black of high oil-absorption(number), apply white carbon black oil-absorption(number) that method of the present invention prepares up to 3.1.
The invention provides a kind of preparation method of white carbon black of high oil-absorption(number), step is as follows:
(1) with water dissolution sodium silicate solid Na
2onSiO
2form Na
2siO
3solution, and by Na
2siO
3the concentration adjustment of solution is to 0.3-0.6mol/L, and wherein n is 2.6-2.9;
(2) by Na prepared by step (1)
2siO
3solution warms, to 80-100 DEG C, adds the vitriol oil and neutralizes, and terminal pH is 9-11; Continue to add the sulphuric acid soln stirring reaction 50-70min that concentration is 4-6mol/L, terminal pH is 5-6;
(3) be cooled to 60-70 DEG C, aging 20-25min, wherein, stir speed (S.S.) is 15rpm-20rpm, obtains slurries;
(4) after slurries being cooled to 40-60 DEG C, adjust pH to 2-5, press filtration, washing obtain wet cake;
(5) be scattered in the mixed aqueous solution of propyl alcohol and ethanol by the wet cake that step (4) obtains, wherein the concentration of propyl alcohol is 1-2mol/L, and the concentration of ethanol is 0.5-0.8mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.
Apply white carbon black oil-absorption(number) that method of the present invention prepares up to 3.1cm
3/ g, can meet the demand of each field to high oil-absorption(number) white carbon black.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the process flow sheet of preparation method of the present invention.
Embodiment
Following embodiment is convenient to understand the present invention better, but does not limit the present invention.Experimental technique in following embodiment, if no special instructions, is ordinary method.
embodiment 1
Preparation method's step of the white carbon black of high oil-absorption(number) of the present invention is as follows:
(1) with water dissolution sodium silicate solid Na
2onSiO
2form Na
2siO
3solution, and by Na
2siO
3the concentration adjustment of solution is to 0.5mol/L, and wherein n is 2.8;
(2) by Na prepared by step (1)
2siO
3solution warms to 90 DEG C, adds the vitriol oil and neutralizes, and terminal pH is 10; Continue to add the sulphuric acid soln stirring reaction 60min that concentration is 5mol/L, terminal pH is 5.5;
(3) be cooled to 65 DEG C, aging 22min, wherein, stir speed (S.S.) is 18rpm, obtains slurries;
(4) after slurries being cooled to 45 DEG C, adjust pH to 4, press filtration, washing obtain wet cake;
(5) be scattered in the mixed aqueous solution of propyl alcohol and ethanol by the wet cake that step (4) obtains, wherein the concentration of propyl alcohol is 1.5mol/L, and the concentration of ethanol is 0.6mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.
embodiment 2
Preparation method's step of the white carbon black of high oil-absorption(number) of the present invention is as follows:
(1) with water dissolution sodium silicate solid Na
2onSiO
2form Na
2siO
3solution, and by Na
2siO
3the concentration adjustment of solution is to 0.3mol/L, and wherein n is 2.9;
(2) by Na prepared by step (1)
2siO
3solution warms to 100 DEG C, adds the vitriol oil and neutralizes, and terminal pH is 9; Continue to add the sulphuric acid soln stirring reaction 70min that concentration is 6mol/L, terminal pH is 5;
(3) be cooled to 60 DEG C, aging 25min, wherein, stir speed (S.S.) is 20rpm, obtains slurries;
(4) after slurries being cooled to 60 DEG C, adjust pH to 2, press filtration, washing obtain wet cake;
(5) be scattered in the mixed aqueous solution of propyl alcohol and ethanol by the wet cake that step (4) obtains, wherein the concentration of propyl alcohol is 2mol/L, and the concentration of ethanol is 0.5mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.
embodiment 3
Preparation method's step of the white carbon black of high oil-absorption(number) of the present invention is as follows:
(1) with water dissolution sodium silicate solid Na
2onSiO
2form Na
2siO
3solution, and by Na
2siO
3the concentration adjustment of solution is to 0.6mol/L, and wherein n is 2.6;
(2) by Na prepared by step (1)
2siO
3solution warms to 80 DEG C, adds the vitriol oil and neutralizes, and terminal pH is 11; Continue to add the sulphuric acid soln stirring reaction 50min that concentration is 4mol/L, terminal pH is 6;
(3) be cooled to 70 DEG C, aging 20min, wherein, stir speed (S.S.) is 15rpm, obtains slurries;
(4) after slurries being cooled to 40 DEG C, adjust pH to 5, press filtration, washing obtain wet cake;
(5) be scattered in the mixed aqueous solution of propyl alcohol and ethanol by the wet cake that step (4) obtains, wherein the concentration of propyl alcohol is 1mol/L, and the concentration of ethanol is 0.8mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.
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 preparation method for the white carbon black of high oil-absorption(number), is characterized in that: step is as follows:
(1) with water dissolution sodium silicate solid Na
2onSiO
2form Na
2siO
3solution, and by Na
2siO
3the concentration adjustment of solution is to 0.3-0.6mol/L, and wherein n is 2.6-2.9;
(2) by Na prepared by step (1)
2siO
3solution warms, to 80-100 DEG C, adds the vitriol oil and neutralizes, and terminal pH is 9-11; Continue to add the sulphuric acid soln stirring reaction 50-70min that concentration is 4-6mol/L, terminal pH is 5-6;
(3) be cooled to 60-70 DEG C, aging 20-25min, wherein, stir speed (S.S.) is 15rpm-20rpm, obtains slurries;
(4) after slurries being cooled to 40-60 DEG C, adjust pH to 2-5, press filtration, washing obtain wet cake;
(5) be scattered in the mixed aqueous solution of propyl alcohol and ethanol by the wet cake that step (4) obtains, wherein the concentration of propyl alcohol is 1-2mol/L, and the concentration of ethanol is 0.5-0.8mol/L, heats while stirring, backflow, and suction filtration is dry, obtains white carbon black.
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|---|---|---|---|
| CN201510294599.9A CN104909373A (en) | 2015-06-02 | 2015-06-02 | Preparation method of white carbon black having high oil factor |
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|---|---|
| CN104909373A true CN104909373A (en) | 2015-09-16 |
Family
ID=54078886
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858668A (en) * | 2016-03-30 | 2016-08-17 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN106629756A (en) * | 2017-01-11 | 2017-05-10 | 冷水江三A新材料科技有限公司 | Method for improving oil absorption value by treating white carbon black through alcohols |
| CN107445171A (en) * | 2017-06-30 | 2017-12-08 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low index of refraction high transparency type silica |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858668A (en) * | 2016-03-30 | 2016-08-17 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN105858668B (en) * | 2016-03-30 | 2017-03-22 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide with high oil absorption value and high water absorption capacity for washing powder |
| CN106629756A (en) * | 2017-01-11 | 2017-05-10 | 冷水江三A新材料科技有限公司 | Method for improving oil absorption value by treating white carbon black through alcohols |
| CN107445171A (en) * | 2017-06-30 | 2017-12-08 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low index of refraction high transparency type silica |
| CN107445171B (en) * | 2017-06-30 | 2018-05-29 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low index of refraction high transparency type silica |
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Application publication date: 20150916 |