CN108862287A - The preparation method of high oil absorption high-dispersion white carbon black - Google Patents
The preparation method of high oil absorption high-dispersion white carbon black Download PDFInfo
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- CN108862287A CN108862287A CN201810660590.9A CN201810660590A CN108862287A CN 108862287 A CN108862287 A CN 108862287A CN 201810660590 A CN201810660590 A CN 201810660590A CN 108862287 A CN108862287 A CN 108862287A
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- carbon black
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- white carbon
- oil absorption
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
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Abstract
The invention discloses a kind of preparation methods of high oil absorption high-dispersion white carbon black, include the following steps：(1) 65 DEG C~99 DEG C, are heated water to, albite powder is added into water, adds ethyl alcohol, is mixed；The albite powder additive amount is 0.05mol/L~2.00mol/L；The mass fraction of the ethyl alcohol is 1wt%~5wt%；(2), 98% 2.05~3.36wt% of sulfuric acid is added dropwise into step (1) mixed liquor, stirring is warming up to boiling, reacts 2~5 hours；(3), (2) reaction product pH value is 3.0~5.0 to regulating step, is separated by filtration, takes filter cake；(4), step (3) filter cake and water by etc. mass ratioes mixing, be stirred at 35~43 DEG C of temperature 1~3 hour；Filtering, it is dry.Preparation method simple process provided by the invention has good Technical Economy.
Description
Technical field
The present invention relates to white carbon black technical field, especially a kind of preparation method of high oil absorption high-dispersion white carbon black.
Background technique
White carbon black is the general name of white powder X-ray amorphous silicic acid and silicate product, is primarily referred to as precipitating dioxy
SiClx, fumed silica and superfine silicon dioxide gel also include powdered synthetic aluminium silicate and calcium silicates etc..
The traditional preparation methods of white carbon black mainly have vapor phase method and two kinds of the precipitation method.
Vapor phase method hydrolyzes the silica that smoke-like is made using silicon tetrachloride gas under Hydrogen Oxygen air-flow high temperature.Gas phase
The advantages of method, is reaction condition easy to control, and product purity is high, dispersion degree is high, particle is thin and it is spherical to be formed, and surface hydroxyl is few, because
And the nano effect with excellent reinforcement, thickening and thixotropic property and particle, the disadvantage is that high expensive, is actually also exactly
This point limits its extensive use, therefore, at present such as rubber industry, is still largely producing hard charcoal using traditional precipitation method
It is black.
The precipitation method produce white carbon black using soluble silicate and the method for inorganic acid neutralization-precipitation reaction.The precipitation method
Production technology, the equipment for preparing white carbon black are simple, and dispersing agent and raw material are easy to get, and process is simple, and scale of investment is little, but energy consumption
Height, higher to environmental requirement, Product Activity is not high, and particle is not easy to control, and affinity is poor, and reinforcing property is low, and particle surface is hydrophilic
Bonding is serious, weakens the binding force of product.With the continuous improvement of environmental consciousness, a large amount of losses of social resources propose one
Kind energy-saving and environmental protection, white carbon black preparation method at low cost, more seem with important positive effect.
Summary of the invention
In view of the deficiencies of the prior art, the present invention proposes a kind of preparation method of high oil absorption high-dispersion white carbon black, product ratios
Surface area is higher, and dispersion performance is more preferable.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：A kind of high oil absorption high-dispersion white carbon black
Preparation method includes the following steps：
(1) 65 DEG C~99 DEG C, are heated water to, albite powder is added into water, adds ethyl alcohol, is mixed；The sodium is long
Stone powder additive amount is 0.05mol/L~2.00mol/L；The mass fraction of the ethyl alcohol is 1wt%~5wt%；
(2), 98% 2.05~3.36wt% of sulfuric acid is added dropwise into step (1) mixed liquor, stirring is warming up to boiling, reaction 2
~5 hours；
(3), (2) reaction product pH value is 3.0~5.0 to regulating step, is separated by filtration, takes filter cake；
(4), step (3) filter cake and water by etc. mass ratioes mixing, be stirred at 35~43 DEG C of temperature 1~3 hour；It crosses
Filter, it is dry.
Further, (1) albite powder is to preheat 20~50 minutes to pre-process at 100 DEG C~200 DEG C to step.
Further, (2) step heats up heats for oil bath.
Further, (2) step heats up carries out for ladder.
Compared with prior art, the present invention has the following advantages that：
(1) preparation method provided by the invention is by preparing suitable reaction bottom liquid, and cooperate it is right in the subsequent reactions stage
The parameter of reaction system concentration adjusts and the addition of dispersing agent ethyl alcohol, and high-dispersity white carbon black can be prepared.The present invention
Preparation method in, aforesaid operations have synergistic effect.Preparation method simple process provided by the invention has good technology
Economy.
(2) white carbon black product prepared by the present invention has good dispersibility, is applied in rubber for tire as reinforcing agent,
It shows good reinforcing effect, can not only improve the processing performance of rubber for tire, shows as lower Mooney viscosity
With vulcanization time, its mechanical property can also be improved, be now higher 300% stress at definite elongation, 500% stress at definite elongation and stretching
Intensity, while wear-resisting property is also significantly improved.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail, the description of this part be only it is exemplary and explanatory, no
Reply protection scope of the present invention has any restriction effect.
Embodiment 1
A kind of preparation method of high oil absorption high-dispersion white carbon black, includes the following steps：
(1) 65 DEG C, are heated water to, albite powder is added into water, adds ethyl alcohol, is mixed；The albite powder
Additive amount is 2.00mol/L；The mass fraction of the ethyl alcohol is 1wt%；Albite powder is that 20 minutes pre- places are preheated at 200 DEG C
Reason；
(2), 98% sulfuric acid 3.36wt% is added dropwise into step (1) mixed liquor, stirring is warming up to boiling, reacts 2 hours；
(3), (2) reaction product pH value is 5.0 to regulating step, is separated by filtration, takes filter cake；
(4), step (3) filter cake and water by etc. mass ratioes mixing, be stirred at 35 DEG C of temperature 3 hours；Filtering, it is dry.
Embodiment 2
A kind of preparation method of high oil absorption high-dispersion white carbon black, includes the following steps：
(1) 99 DEG C, are heated water to, albite powder is added into water, adds ethyl alcohol, is mixed；The albite powder
Additive amount is 0.05mol/L；The mass fraction of the ethyl alcohol is 5wt%；Albite powder is that 50 minutes pre- places are preheated at 100 DEG C
Reason；
(2), 98% sulfuric acid 2.05wt% is added dropwise into step (1) mixed liquor, stirring is warming up to boiling, reacts 5 hours；
(3), (2) reaction product pH value is 3.0 to regulating step, is separated by filtration, takes filter cake；
(4), step (3) filter cake and water by etc. mass ratioes mixing, be stirred at 43 DEG C of temperature 1 hour；Filtering, it is dry.
Embodiment 3
A kind of preparation method of high oil absorption high-dispersion white carbon black, includes the following steps：
(1) 86 DEG C, are heated water to, albite powder is added into water, adds ethyl alcohol, is mixed；The albite powder
Additive amount is 1.10mol/L；The mass fraction of the ethyl alcohol is 4wt%；Albite powder is that 40 minutes pre- places are preheated at 130 DEG C
Reason；
(2), 98% sulfuric acid 2.76wt% is added dropwise into step (1) mixed liquor, stirring is warming up to boiling, reacts 3 hours；
(3), (2) reaction product pH value is 4.0 to regulating step, is separated by filtration, takes filter cake；
(4), step (3) filter cake and water by etc. mass ratioes mixing, be stirred at 39 DEG C of temperature 2 hours；Filtering, it is dry.
Embodiment 4
A kind of preparation method of high oil absorption high-dispersion white carbon black, includes the following steps：
(1) 83 DEG C, are heated water to, albite powder is added into water, adds ethyl alcohol, is mixed；The albite powder
Additive amount is 0.86mol/L；The mass fraction of the ethyl alcohol is 2wt%；Albite powder is that 30 minutes pre- places are preheated at 180 DEG C
Reason；
(2), 98% sulfuric acid 2.6wt% is added dropwise into step (1) mixed liquor, stirring is warming up to boiling, reacts 4 hours；
(3), (2) reaction product pH value is 3.5 to regulating step, is separated by filtration, takes filter cake；
(4), step (3) filter cake and water by etc. mass ratioes mixing, be stirred at 40 DEG C of temperature 2 hours；Filtering, it is dry.
Performance detection is carried out to the product that above-described embodiment obtains, result is as shown in the table：
| BET specific surface area (m2/g) | CTAB specific surface area (m2/g) | Oil factor (cm2/g) | D50/μm | |
| Embodiment 1 | 205 | 180 | 2.65 | 2.25 |
| Embodiment 2 | 205 | 181 | 2.66 | 2.31 |
| Embodiment 3 | 207 | 183 | 2.68 | 2.23 |
| Embodiment 4 | 206 | 182 | 2.71 | 2.19 |
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of preparation method of high oil absorption high-dispersion white carbon black, it is characterised in that：Include the following steps：
(1) 65 DEG C~99 DEG C, are heated water to, albite powder is added into water, adds ethyl alcohol, is mixed；The albite in powder
Last additive amount is 0.05mol/L~2.00mol/L；The mass fraction of the ethyl alcohol is 1wt%~5wt%；
(2), 98% 2.05~3.36wt% of sulfuric acid is added dropwise into step (1) mixed liquor, stirring is warming up to boiling, and reaction 2~5 is small
When；
(3), (2) reaction product pH value is 3.0~5.0 to regulating step, is separated by filtration, takes filter cake；
(4), step (3) filter cake and water by etc. mass ratioes mixing, be stirred at 35~43 DEG C of temperature 1~3 hour；Filtering is done
It is dry.
2. the preparation method of high oil absorption high-dispersion white carbon black as described in claim 1, it is characterised in that：Step (1) albite powder
It is pre-processed to be preheated 20~50 minutes at 100 DEG C~200 DEG C.
3. the preparation method of high oil absorption high-dispersion white carbon black as described in claim 1, it is characterised in that：(2) step heats up as oil bath
Heating.
4. the preparation method of high oil absorption high-dispersion white carbon black as described in claim 1, it is characterised in that：(2) step heats up as ladder
It carries out.
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| CN201810660590.9A CN108862287B (en) | 2018-06-25 | 2018-06-25 | Preparation method of high oil absorption and high dispersion white carbon black |
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| CN201810660590.9A CN108862287B (en) | 2018-06-25 | 2018-06-25 | Preparation method of high oil absorption and high dispersion white carbon black |
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| CN108862287B CN108862287B (en) | 2022-02-18 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6193944B1 (en) * | 1995-12-08 | 2001-02-27 | Goldendale Aluminum Company | Method of recovering fumed silica from spent potliner |
| CN103539130A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Technological method for preparing white carbon black from potassium feldspar |
| CN104445219A (en) * | 2014-11-28 | 2015-03-25 | 嵩县中科孵化器有限公司 | Preparation method of white carbon black |
| CN104480531A (en) * | 2014-11-28 | 2015-04-01 | 嵩县中科孵化器有限公司 | Process for decomposing albite |
| CN104528749A (en) * | 2015-01-20 | 2015-04-22 | 江西省源通陶瓷科技有限公司 | Process for chemically whitening feldspar concentrate |
| CN106745085A (en) * | 2016-11-30 | 2017-05-31 | 东至天孚化工有限公司 | A kind of potassium sulfate preparation method based on potassium feldspar |
-
2018
- 2018-06-25 CN CN201810660590.9A patent/CN108862287B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6193944B1 (en) * | 1995-12-08 | 2001-02-27 | Goldendale Aluminum Company | Method of recovering fumed silica from spent potliner |
| CN103539130A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Technological method for preparing white carbon black from potassium feldspar |
| CN104445219A (en) * | 2014-11-28 | 2015-03-25 | 嵩县中科孵化器有限公司 | Preparation method of white carbon black |
| CN104480531A (en) * | 2014-11-28 | 2015-04-01 | 嵩县中科孵化器有限公司 | Process for decomposing albite |
| CN104528749A (en) * | 2015-01-20 | 2015-04-22 | 江西省源通陶瓷科技有限公司 | Process for chemically whitening feldspar concentrate |
| CN106745085A (en) * | 2016-11-30 | 2017-05-31 | 东至天孚化工有限公司 | A kind of potassium sulfate preparation method based on potassium feldspar |
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