CN113336235A - Preparation method of high-dispersion white carbon black special for high-controllability tire - Google Patents
Preparation method of high-dispersion white carbon black special for high-controllability tire Download PDFInfo
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- CN113336235A CN113336235A CN202110733996.7A CN202110733996A CN113336235A CN 113336235 A CN113336235 A CN 113336235A CN 202110733996 A CN202110733996 A CN 202110733996A CN 113336235 A CN113336235 A CN 113336235A
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- value
- solution
- sodium silicate
- carbon black
- reaction kettle
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000006229 carbon black Substances 0.000 title claims abstract description 26
- 239000006185 dispersion Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 33
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 18
- HRQDCDQDOPSGBR-UHFFFAOYSA-M sodium;octane-1-sulfonate Chemical compound [Na+].CCCCCCCCS([O-])(=O)=O HRQDCDQDOPSGBR-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000002535 acidifier Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 12
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 12
- 235000011152 sodium sulphate Nutrition 0.000 claims description 12
- 238000010009 beating Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 241000227425 Pieris rapae crucivora Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
-
- 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
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of high-dispersion white carbon black special for a high-controllability tire. The preparation method comprises the following steps: (1) adding a certain amount of electrolyte solution and sodium octyl sulfonate into a reaction kettle; (2) then adding a sodium silicate solution into the reaction kettle until the pH value is 9-10, and heating to 70-75 ℃; (3) continuously adding a sodium silicate solution into the reaction kettle, and adding an acidifying agent to keep the pH value at 10-11; (4) and after the sodium silicate solution is added, continuously adding an acidifying agent to adjust the pH value to 5-6 in a stepped manner, and reacting to obtain the white carbon black. Compared with the prior art, the preparation method is simple to operate and low in cost, and the tire can obtain better control experience by adding the high-dispersion white carbon black prepared by the method.
Description
Technical Field
The invention relates to a preparation method of high-dispersion white carbon black special for a high-controllability tire.
Background
The high handling of the tires has a very important impact on the safety of the vehicle and the driving experience. The prior art mainly improves the handling performance of the tire through tread patterns or rubber tire formulations.
White carbon black, SiO2·nH2O, has the characteristics of high temperature resistance, non-combustion, tastelessness and no odor, and is an excellent rubber tire reinforcing filler. Compared with common white carbon black, the high-dispersion white carbon black can be added into the tire by 40-60 parts of the high-dispersion white carbon black per hundred parts of rubber material due to the special pore structure and disintegration property of the high-dispersion white carbon blackUp to 80 parts. Therefore, it is very beneficial to improve the handling property of the tire by improving the performance of the high-dispersion white carbon black.
Disclosure of Invention
Based on the prior art, the invention aims to provide a preparation method of high-dispersion white carbon black special for a high-controllability tire.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-dispersion white carbon black special for a high-controllability tire comprises the following steps:
(1) adding a certain amount of electrolyte solution and sodium octyl sulfonate into a reaction kettle;
(2) then adding a sodium silicate solution into the reaction kettle until the pH value is 9-10, and heating to 70-75 ℃;
(3) continuously adding a sodium silicate solution into the reaction kettle, and adding an acidifying agent to keep the pH value at 10-11;
(4) and after the sodium silicate solution is added, continuously adding an acidifying agent to adjust the pH value to 5-6 in a stepped manner, and reacting to obtain the white carbon black.
Preferably, the electrolyte solution is a sodium sulfate solution.
More preferably, the concentration of the sodium sulfate solution is 10%, and the addition amount of the sodium sulfate solution is 1/6-1/7 of the volume of the reaction kettle.
Preferably, sodium octyl sulfonate is added in SiO20.5-5 per mill of the weight of the sodium silicate.
Preferably, the concentration of the sodium silicate solution is 20-25 wt%.
Preferably, the acidifying agent is a sulfuric acid solution.
More preferably, the concentration of the sulfuric acid solution is 10 wt%.
Preferably, in the step (3), the sodium silicate solution is stopped adding after the volume of the reaction solution reaches 2/3-3/4 of the volume of the reaction kettle.
Preferably, in the step (4), the specific step of stepwise adjusting the pH value is:
firstly, adjusting the pH value to 8-9, and reacting for 0.1-0.5 h;
adjusting the pH value to 6.5-7, and reacting for 0.1-0.5 h;
and finally, adjusting the pH value to 5-6, and reacting for 0.1-1 hour.
And (4) after the reaction is finished, carrying out post-treatment such as filtering, washing, beating, drying and the like on the reaction slurry to obtain the white carbon black.
The BET specific surface area of the high-dispersion white carbon black prepared by the method is 145-175 m2The dispersion grade is more than or equal to 9.5, and the loss factor tan delta @60 ℃ of the corresponding vulcanized rubber is 0.3-0.4.
Compared with the prior art, the preparation method is simple to operate and low in cost, and the tire can obtain better control experience by adding the high-dispersion white carbon black prepared by the method.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A preparation method of high-dispersion white carbon black special for a high-controllability tire comprises the following steps:
raw materials: a sodium sulfate solution with a concentration of 10 wt%, a sulfuric acid solution with a concentration of 10 wt%, a sodium silicate solution with a concentration of 20 wt%.
(1) Adding sodium sulfate solution into the reaction kettle according to 1/6 of the volume of the reaction kettle, and adding sodium Silicate (SiO)2Calculated) 1 wt% of the total amount, sodium octyl sulfonate (CAS: 5324-84-5), the stirring is started, the stirring speed is set to 70 revolutions per minute.
(2) After the mixture is uniformly stirred, adding a sodium silicate solution into the reaction kettle until the pH value of the system is 9-10, and then heating to 70 ℃.
(3) And after the set temperature is reached, continuously adding a sodium silicate solution into the reaction kettle, adding a sulfuric acid solution, and keeping the pH value of the system at 10-11 in the feeding process.
(4) And stopping adding the sodium silicate solution after the volume of the reaction solution reaches 2/3 of the volume of the reaction kettle, continuously adding the sulfuric acid solution, regulating the pH value to 5-6 in a stepped manner, and then carrying out heat preservation reaction for 10 minutes.
The specific process of stepwise adjusting the pH value is as follows:
after the addition of sodium silicate is stopped, firstly reducing the pH value to 8-9, and reacting for 15 minutes;
then reducing the pH value to 6.5-7, and continuing to react for 10 minutes;
and finally, reducing the pH value to 5-6.
(5) And after the reaction is finished, performing conventional filter pressing, washing, beating and drying treatment on the slurry to obtain the white carbon black.
Example 2
A preparation method of high-dispersion white carbon black special for a high-controllability tire comprises the following steps:
raw materials: a sodium sulfate solution with a concentration of 10 wt%, a sulfuric acid solution with a concentration of 10 wt%, a sodium silicate solution with a concentration of 25 wt%.
(1) Adding sodium sulfate solution into the reaction kettle according to 1/6 of the volume of the reaction kettle, and adding sodium Silicate (SiO)2Calculated) 1wt per mill of the total amount, adding sodium octyl sulfonate into the reaction kettle, starting stirring, and setting the stirring speed at 70 revolutions per minute.
(2) After the mixture is uniformly stirred, adding a sodium silicate solution into the reaction kettle until the pH value of the system is 9-10, and then heating to 75 ℃.
(3) And after the set temperature is reached, continuously adding a sodium silicate solution into the reaction kettle, adding a sulfuric acid solution, and keeping the pH value of the system at 10-11 in the feeding process.
(4) And stopping adding the sodium silicate solution after the volume of the reaction solution reaches 2/3 of the volume of the reaction kettle, continuously adding the sulfuric acid solution, regulating the pH value to 5-6 in a stepped manner, and then carrying out heat preservation reaction for 6 minutes.
The specific process of stepwise adjusting the pH value is as follows:
after the addition of sodium silicate is stopped, firstly reducing the pH value to 8-9, and reacting for 10 minutes;
then reducing the pH value to 6.5-7, and continuing to react for 10 minutes;
and finally, reducing the pH value to 5-6.
(5) And after the reaction is finished, performing conventional filter pressing, washing, beating and drying treatment on the slurry to obtain the white carbon black.
Example 3
A preparation method of high-dispersion white carbon black special for a high-controllability tire comprises the following steps:
raw materials: a sodium sulfate solution with a concentration of 10 wt%, a sulfuric acid solution with a concentration of 10 wt%, a sodium silicate solution with a concentration of 20 wt%.
(1) Adding sodium sulfate solution into the reaction kettle according to 1/6 of the volume of the reaction kettle, and adding sodium Silicate (SiO)2Calculated) 1.5wt per mill of the total amount, adding sodium octyl sulfonate into the reaction kettle, starting stirring, and setting the stirring speed at 70 revolutions per minute.
(2) After the mixture is uniformly stirred, adding a sodium silicate solution into the reaction kettle until the pH value of the system is 9-10, and then heating to 70 ℃.
(3) And after the set temperature is reached, continuously adding a sodium silicate solution into the reaction kettle, adding a sulfuric acid solution, and keeping the pH value of the system at 10-11 in the feeding process.
(4) And stopping adding the sodium silicate solution after the volume of the reaction solution reaches 2/3 of the volume of the reaction kettle, continuously adding the sulfuric acid solution, regulating the pH value to 5-6 in a stepped manner, and then carrying out heat preservation reaction for 10 minutes.
The specific process of stepwise adjusting the pH value is as follows:
after the addition of sodium silicate is stopped, firstly reducing the pH value to 8-9, and reacting for 10 minutes;
then reducing the pH value to 6.5-7, and continuing to react for 10 minutes;
and finally, reducing the pH value to 5-6.
(5) And after the reaction is finished, performing conventional filter pressing, washing, beating and drying treatment on the slurry to obtain the white carbon black.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of high-dispersion white carbon black special for a high-controllability tire comprises the following steps:
(1) adding a certain amount of electrolyte solution and sodium octyl sulfonate into a reaction kettle;
(2) then adding a sodium silicate solution into the reaction kettle until the pH value is 9-10, and heating to 70-75 ℃;
(3) continuously adding a sodium silicate solution into the reaction kettle, and adding an acidifying agent to keep the pH value at 10-11;
(4) and after the sodium silicate solution is added, continuously adding an acidifying agent to adjust the pH value to 5-6 in a stepped manner, and reacting to obtain the white carbon black.
2. The method of claim 1, wherein: the electrolyte solution is a sodium sulfate solution.
3. The method of claim 2, wherein: the concentration of the sodium sulfate solution is 10%, and the addition amount of the sodium sulfate solution is 1/6-1/7 of the volume of the reaction kettle.
4. The method of claim 1, wherein: the addition amount of the sodium octyl sulfonate is SiO20.5-5 per mill of the weight of the sodium silicate.
5. The method of claim 1, wherein: the concentration of the sodium silicate solution is 20-25 wt%.
6. The method of claim 1, wherein: the acidifying agent is a sulfuric acid solution.
7. The method of claim 6, wherein: the concentration of the sulfuric acid solution was 10 wt%.
8. The method of claim 1, wherein: in the step (3), after the volume of the reaction liquid reaches 2/3-3/4 of the volume of the reaction kettle, the addition of the sodium silicate solution is stopped.
9. The method of claim 1, wherein: in the step (4), the step-type pH value adjustment comprises the following specific steps:
firstly, adjusting the pH value to 8-9, and reacting for 0.1-0.5 h;
adjusting the pH value to 6.5-7, and reacting for 0.1-0.5 h;
and finally, adjusting the pH value to 5-6, and reacting for 0.1-1 hour.
10. The method of claim 1, wherein: and (4) after the reaction is finished, filtering, washing, beating and drying to obtain the white carbon black.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110733996.7A CN113336235A (en) | 2021-06-30 | 2021-06-30 | Preparation method of high-dispersion white carbon black special for high-controllability tire |
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| CN202110733996.7A CN113336235A (en) | 2021-06-30 | 2021-06-30 | Preparation method of high-dispersion white carbon black special for high-controllability tire |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115710000A (en) * | 2022-09-08 | 2023-02-24 | 确成硅化学股份有限公司 | Preparation method of special white carbon black for storage battery separator |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000053412A (en) * | 1998-08-07 | 2000-02-22 | Oji Paper Co Ltd | Production of powder white carbon |
| CN105236429A (en) * | 2015-09-14 | 2016-01-13 | 安徽确成硅化学有限公司 | Ultrahighly-dispersed white carbon black preparation method |
| CN110127709A (en) * | 2019-06-05 | 2019-08-16 | 确成硅化学股份有限公司 | A kind of method of gradient pH precipitation method preparation high dispersive silica |
-
2021
- 2021-06-30 CN CN202110733996.7A patent/CN113336235A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000053412A (en) * | 1998-08-07 | 2000-02-22 | Oji Paper Co Ltd | Production of powder white carbon |
| CN105236429A (en) * | 2015-09-14 | 2016-01-13 | 安徽确成硅化学有限公司 | Ultrahighly-dispersed white carbon black preparation method |
| CN110127709A (en) * | 2019-06-05 | 2019-08-16 | 确成硅化学股份有限公司 | A kind of method of gradient pH precipitation method preparation high dispersive silica |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115710000A (en) * | 2022-09-08 | 2023-02-24 | 确成硅化学股份有限公司 | Preparation method of special white carbon black for storage battery separator |
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Application publication date: 20210903 |