CN103435046B - A kind of manufacture craft of high-dispersity white carbon black of snow tire - Google Patents
A kind of manufacture craft of high-dispersity white carbon black of snow tire Download PDFInfo
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- CN103435046B CN103435046B CN201310338438.6A CN201310338438A CN103435046B CN 103435046 B CN103435046 B CN 103435046B CN 201310338438 A CN201310338438 A CN 201310338438A CN 103435046 B CN103435046 B CN 103435046B
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Abstract
A kind of manufacture craft of high-dispersity white carbon black of snow tire, by conservative control reaction process and processing parameter, obtain the white carbon black that a kind of dispersiveness is high, the technical scheme adopted is, described technique be with liquid sodium silicate and sulfuric acid be main raw material, with vitriol for auxiliary material, control temperature of reaction reaction in a kettle. and generate gained mixture, and carry out purifying and granulation.The present invention, on existing production equipment basis, does not increase equipment investment, does not increase personnel, not feed change, just adjustment reaction parameter when carry out.It is good that the product produced has dispersion effect, and product appearance microballon shape is even, and environmental protection is without dust.Stable production process, can realize scale operation.
Description
Technical field
The present invention relates to a kind of manufacture craft of white carbon black, particularly a kind of manufacture craft of high-dispersity white carbon black of snow tire.
Background technology
White carbon black is a kind of novel fine chemical product of modern industry, and along with the progress of science and technology, its performance is constantly familiar with, and purposes constantly in expansion, especially in doughnut goods, is widely used.This is because along with more and more higher to the requirement of tire green, environmental protection, safety, riding comfort, tire enterprise just must add more white carbon black in tire, and especially the better white carbon black of dispersing property could meet above requirement.Tire used in winter requires more outstanding to the gripping power in ice face, and the phenomenon reducing ice in winter road surface tyre slip occurs.Current China white carbon black level not yet reaches the requirement of tire enterprise to the high-dispersion white carbon black that this requires, its major cause is, due to the restriction of the manufacture craft of white carbon black, make white carbon black be difficult to scatter in compounding rubber, therefore the modified effect of white carbon black to tire is not clearly.
In prior art, the production method of white carbon black has Physical and chemical method, expect that active good, reinforcing high amorphous white carbon black needs to adopt chemical method.Chemical method is divided into dry method pyrolysis and wet-precipitated two kinds.Dry method pyrolysis is divided into vapor phase process and arc process; Wet-precipitated is divided into sulfuric acid, hydrochloric acid, nitric acid and carbon dioxide precipitates method etc.At present, white carbon black production mainly adopts vapor phase process and sulfuric acid, hydrochloric acid precipitation method two kinds of production technique.
Thermal silica because of its production equipment amount of investment large, set of device production capacity is generally below 5000 tons; In addition the production energy consumption of thermal silica and comprehensive cost too high, and non-modified process, powder application field is narrow, and due to the impact by all many factors such as starting material, energy consumption, cost, Application Areas, production capacity, technology, therefore the preparation of thermal silica powder has limitation.
And the white carbon black that the precipitator method are obtained, usually because surface is containing silanol base, cause the surface polarity of white carbon black larger, easily be flooded profit, and bad with the consistency of organism, hydrocarbon polymer, significantly reduce use properties and use range, so usually need its modification, obtained modified white carbon black, to strengthen its performance, to expand its use range.
From the synthesis mechanism analysis of existing precipitated silica, precipitated silica preparation process can be summarized as two class dynamic processes: one is the process of growth of the nucleus of precipitated silica, two is growth accumulation process of nucleus.At present, the production of liquid-phase precipitation method white carbon black all adopts dilute sulphuric acid two-step approach to carry out at home: the first step reaction generates rare silicon sol, parked slaking for some time, in rare silicon sol, form nucleus gradually, as the crystal seed of the second reaction; Second step is namely with the mother liquor that the solution containing crystal seed grows as gathering, water glass is added and dilute sulphuric acid carries out precipitin reaction by certain speed, after reaction certain hour, stop adding water glass, only add dilute sulphuric acid and carry out acidification, when reaction solution pH value reaches certain value, stop acid adding, ageing certain hour, then filters and with water cleaning, removes Na
2sO
4after, obtain product after sending drying, pulverizing.Finally, general employing dry method modification method, carries out modification to obtained white carbon black, obtained modified white carbon black.
Existing this technique, because reaction process state modulator is unreasonable, causes the white carbon black product dispersing property that obtains poor, can not meet the requirement of snow tire to high-dispersion white carbon black.
Summary of the invention
The invention provides a kind of manufacture craft of high-dispersity white carbon black of snow tire, by conservative control reaction process and processing parameter, obtain the white carbon black that a kind of dispersiveness is high, can be widely applied in anti-skidding and that earth-catching property requirement is high Tire used in winter.
The present invention is the technical scheme realizing goal of the invention employing, a kind of manufacture craft of high-dispersity white carbon black of snow tire, described technique be with liquid sodium silicate and sulfuric acid be main raw material, with vitriol for auxiliary material, control temperature of reaction reaction in a kettle. and generate gained mixture, and carry out purifying and granulation, key is: the described concrete steps generating gained mixture in a kettle. comprise:
A, material allocation: allotment density is 1.150 ~ 1.250g/cm
3silicate solutions, dilution after density be 1.030 ~ 1.060 g/cm
3sulphuric acid soln and density be 1.01 ~ 1.08g/cm
3sulfate liquor, for subsequent use;
It is 1.05 ~ 1.1 g/cm that B, the hot water being 40 ~ 60 DEG C by the sodium silicate solution of density listed in above-mentioned A, sulfate liquor and temperature are deployed into density
3, join in reactor afterwards, and stir until reaction terminates formation first mixing solutions;
C, intensification: above-mentioned first mixing solutions is heated to 70 ~ 85 DEG C;
D, sulphuric acid soln deployed in steps A joined in reactor and stir, until form the second mixing solutions that pH value is 7.0 ~ 8.5 in reactor;
E, to heat up again: above-mentioned second mixing solutions is heated to 85 ~ 95 DEG C;
F, add sodium silicate solution deployed in steps A and sulphuric acid soln simultaneously and stir in a kettle., and keep in whole adition process, mixture pH value in reactor is 7.5 ~ 9.0, until add with above-mentioned B in add the amount of water glass ratio be 1:(12 ~ 18);
G, continue to add sulphuric acid soln in a kettle., until generating pH value in reactor is the reaction product of 3.4 ~ 5.8.
Key of the present invention is: the product produced by the present invention has special form, particle diameter and porosity (BET/CTAB), there is good dispersive ability in the polymer, in the application of tire in the winter time, can greatly improve the anti-skidding of tire and earth-catching property.
The invention has the beneficial effects as follows: the present invention, on existing production equipment basis, does not increase equipment investment, do not increase personnel, not feed change, just adjustment reaction parameter when carry out.It is good that the product produced has dispersion effect, and product appearance microballon shape is even, and environmental protection is without dust.Stable production process, can realize scale operation.
Snow tire high-dispersion white carbon black of the present invention adopts unique production technique, control the primary partical of white carbon black, generate the special construction of white carbon black, make it combine at and rubber molecule easier with energy during compounding rubber, good to reach dispersion effect, the rubber performance after mixing is good.Can play fuel-economizing and reduce the effect of motor vehicle exhaust, ice face gripping power improves 5%, can play the skidproof effect in ice face, ensures ride safety of automobile, reduces noise and improves riding comfort, meets green tire and snow tire to the requirement of high-dispersion white carbon black.
Embodiment
A kind of manufacture craft of high-dispersity white carbon black of snow tire, described technique be with liquid sodium silicate and sulfuric acid be main raw material, with vitriol for auxiliary material, control temperature of reaction reaction in a kettle. and generate gained mixture, and carry out purifying and granulation, key is: the described concrete steps generating gained mixture in a kettle. comprise:
A, material allocation: allotment density is 1.150 ~ 1.250g/cm
3silicate solutions, dilution after density be 1.030 ~ 1.060 g/cm
3sulphuric acid soln and density be 1.01 ~ 1.08g/cm
3sulfate liquor, for subsequent use;
It is 1.05 ~ 1.1 g/cm that B, the hot water being 40 ~ 60 DEG C by the sodium silicate solution of density listed in above-mentioned A, sulfate liquor and temperature are deployed into density
3, join in reactor afterwards, and stir until reaction terminates formation first mixing solutions;
C, intensification: above-mentioned first mixing solutions is heated to 70 ~ 85 DEG C;
D, sulphuric acid soln deployed in steps A joined in reactor and stir, until form the second mixing solutions that pH value is 7.0 ~ 8.5 in reactor;
E, to heat up again: above-mentioned second mixing solutions is heated to 85 ~ 95 DEG C;
F, add sodium silicate solution deployed in steps A and sulphuric acid soln simultaneously and stir in a kettle., and keep in whole adition process, mixture pH value in reactor is 7.5 ~ 9.0, until add with above-mentioned B in add the amount of water glass ratio be 1:(12 ~ 18);
G, continue to add sulphuric acid soln in a kettle., until generating pH value in reactor is the reaction product of 3.4 ~ 5.8.
It is 2600 ~ 3000 seconds that described step D stirs the time of carrying out.
Purification in described processing step specifically comprises: obtain through press filtration washing, liquefaction the emulsus white carbon black slip that solids content is 20 ~ 24%, percentage sign is weight percentage.
Granulation in described processing step specifically comprises: the emulsus white carbon black slurry obtained in purification step is carried out press atomization through high-pressure pump, and enters drying tower drying and obtain silica particles.
The equipment that described press filtration step adopts is diaphragm filter press.
Controlling dried silica particles moisture is 4 ~ 8%, and median size is 250 ~ 300 μm.
Described vitriol is potassium sulfate or calcium sulfate or sodium sulfate.
The present invention in the specific implementation, embodiment 1:
A, material allocation: allotment density is 1.15g/cm
3silicate solutions, dilution after density be 1.03 g/cm
3sulphuric acid soln and density be 1.01g/cm
3sulfate liquor, for subsequent use;
It is 1.05g/cm that B, the hot water being 40 DEG C by the sodium silicate solution of density listed in above-mentioned A, sulfate liquor and temperature are deployed into density
3, join in reactor afterwards, and stir until reaction terminates formation first mixing solutions;
C, intensification: above-mentioned first mixing solutions is heated to 70 DEG C;
D, sulphuric acid soln deployed in steps A joined in reactor and stir, until form the second mixing solutions that pH value is 7.0 in reactor;
E, to heat up again: above-mentioned second mixing solutions is heated to 85 DEG C;
F, add sodium silicate solution deployed in steps A and sulphuric acid soln simultaneously and stir in a kettle., and keep in whole adition process, the mixture pH value in reactor is 7.5, until add with above-mentioned B in add the amount of water glass ratio be 1:12;
G, continue to add sulphuric acid soln in a kettle., until generating pH value in reactor is the reaction product of 3.4.
White carbon black is made afterwards through purification and granulation process.
Embodiment 2:
A, material allocation: allotment density is 1.250g/cm
3silicate solutions, dilution after density be 1.060 g/cm
3sulphuric acid soln and density be 1.08g/cm
3sulfate liquor, for subsequent use;
It is 1.1 g/cm that B, the hot water being 60 DEG C by the sodium silicate solution of density listed in above-mentioned A, sulfate liquor and temperature are deployed into density
3, join in reactor afterwards, and stir until reaction terminates formation first mixing solutions;
C, intensification: above-mentioned first mixing solutions is heated to 85 DEG C;
D, sulphuric acid soln deployed in steps A joined in reactor and stir, until form the second mixing solutions that pH value is 8.5 in reactor;
E, to heat up again: above-mentioned second mixing solutions is heated to 95 DEG C;
F, add sodium silicate solution deployed in steps A and sulphuric acid soln simultaneously and stir in a kettle., and keep in whole adition process, the mixture pH value in reactor is 9.0, until add with above-mentioned B in add the amount of water glass ratio be 1:18;
G, continue to add sulphuric acid soln in a kettle., until generating pH value in reactor is the reaction product of 5.8.
White carbon black is made afterwards through purification and granulation process.
Embodiment 3:
A, material allocation: allotment density is 1.2g/cm
3silicate solutions, dilution after density be 1.04g/cm
3sulphuric acid soln and density be 1.05g/cm
3sulfate liquor, for subsequent use;
It is 1.08 g/cm that B, the hot water being 50 DEG C by the sodium silicate solution of density listed in above-mentioned A, sulfate liquor and temperature are deployed into density
3, join in reactor afterwards, and stir until reaction terminates formation first mixing solutions;
C, intensification: above-mentioned first mixing solutions is heated to 80 DEG C;
D, sulphuric acid soln deployed in steps A joined in reactor and stir, until form the second mixing solutions that pH value is 7.8 in reactor;
E, to heat up again: above-mentioned second mixing solutions is heated to 90 DEG C;
F, add sodium silicate solution deployed in steps A and sulphuric acid soln simultaneously and stir in a kettle., and keep in whole adition process, the mixture pH value in reactor is 8, until add with above-mentioned B in add the amount of water glass ratio be 1:15;
G, continue to add sulphuric acid soln in a kettle., until generating pH value in reactor is the reaction product of 5.
White carbon black is made afterwards through purification and granulation process.
In the present invention, the index of the high-dispersion white carbon black of snowfield is as follows:
| Project | Index |
| BET （m 2/g） | 100-130 |
| CTAB （m 2/g） | 100-130 |
| Oil-absorption(number) (cm 3/g） | 2.00-3.50 |
| Weight loss on heating % | 4.0-8.0 |
| Burning decrement % | ≤7.0 |
| Dioxide-containing silica % | ≥90 |
| Water-soluble substance % | ≤2.0 |
| PH value | 5.0-8.0 |
| Outward appearance | Microballon |
Claims (7)
1. the manufacture craft of the high-dispersity white carbon black of a snow tire, described technique be with liquid sodium silicate and sulfuric acid be main raw material, with vitriol for auxiliary material, control temperature of reaction reaction in a kettle. and generate gained mixture, and carry out purifying and granulation, it is characterized in that: the described concrete steps generating gained mixture in a kettle. comprise:
A, material allocation: allotment density is 1.150 ~ 1.250g/cm
3silicate solutions, dilution after density be 1.030 ~ 1.060 g/cm
3sulphuric acid soln and density be 1.01 ~ 1.08g/cm
3sulfate liquor, for subsequent use;
It is 1.05 ~ 1.1 g/cm that B, the hot water being 40 ~ 60 DEG C by the sodium silicate solution of density listed in above-mentioned A, sulfate liquor and temperature are deployed into density
3, join in reactor afterwards, and stir until reaction terminates formation first mixing solutions;
C, intensification: above-mentioned first mixing solutions is heated to 70 ~ 85 DEG C;
D, sulphuric acid soln deployed in steps A joined in reactor and stir, until form the second mixing solutions that pH value is 7.0 ~ 8.5 in reactor;
E, to heat up again: above-mentioned second mixing solutions is heated to 85 ~ 95 DEG C;
F, add sodium silicate solution deployed in steps A and sulphuric acid soln simultaneously and stir in a kettle., and keep in whole adition process, mixture pH value in reactor is 7.5 ~ 9.0, until add with above-mentioned B in add the amount of water glass ratio be 1:(12 ~ 18);
G, continue to add sulphuric acid soln in a kettle., until generating pH value in reactor is the reaction product of 3.4 ~ 5.8.
2. the manufacture craft of the high-dispersity white carbon black of a kind of snow tire according to claim 1, is characterized in that: it is 2600 ~ 3000 seconds that described step D stirs the time of carrying out.
3. the manufacture craft of the high-dispersity white carbon black of a kind of snow tire according to claim 1, it is characterized in that: the purification in described processing step specifically comprises: obtain through press filtration washing, liquefaction the emulsus white carbon black slip that solids content is 20 ~ 24%, percentage sign is weight percentage.
4. the manufacture craft of the high-dispersity white carbon black of a kind of snow tire according to claim 3, it is characterized in that: the granulation in described processing step specifically comprises: the emulsus white carbon black slurry obtained in purification step is carried out press atomization through high-pressure pump, and enter drying tower drying and obtain silica particles.
5. the manufacture craft of the high-dispersity white carbon black of a kind of snow tire according to claim 3, is characterized in that: the equipment that described press filtration step adopts is diaphragm filter press.
6. the manufacture craft of the high-dispersity white carbon black of a kind of snow tire according to claim 4, is characterized in that: controlling dried silica particles moisture is 4 ~ 8%, and median size is 250 ~ 300 μm.
7. the manufacture craft of the high-dispersity white carbon black of a kind of snow tire according to claim 1, is characterized in that: described vitriol is potassium sulfate or calcium sulfate or sodium sulfate.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891505B (en) * | 2015-06-02 | 2017-04-05 | 确成硅化学股份有限公司 | A kind of preparation method of high-dispersity white carbon black |
| CN106315598B (en) * | 2016-08-09 | 2018-08-21 | 确成硅化学股份有限公司 | The preparation method of the high-dispersion white carbon black of one meridian line tyre |
| CN106829977A (en) * | 2017-03-30 | 2017-06-13 | 福建正盛无机材料股份有限公司 | A kind of preparation method of high oil absorption high-dispersion white carbon black |
| CN107140645B (en) * | 2017-06-15 | 2019-08-23 | 确成硅化学股份有限公司 | A kind of preparation method of the dedicated hydrated SiO 2 of engineering tyre |
| CN110078083A (en) * | 2019-06-05 | 2019-08-02 | 确成硅化学股份有限公司 | A kind of dedicated white carbon black of high wet-sliding resistant tire and preparation method thereof |
| CN110562991A (en) * | 2019-10-15 | 2019-12-13 | 龙星化工股份有限公司 | Production method of white carbon black for high-oil-absorption carrier |
| CN110643206A (en) * | 2019-10-18 | 2020-01-03 | 江西黑猫炭黑股份有限公司 | Production method of high-dispersion white carbon black |
| CN111517328A (en) * | 2020-04-16 | 2020-08-11 | 江西双龙硅材料科技有限公司 | Preparation method of high-dispersity white carbon black for tires |
| CN111807377B (en) * | 2020-07-03 | 2023-07-14 | 确成硅化学股份有限公司 | White carbon black for improving winter tire performance |
| CN113321217A (en) * | 2021-06-30 | 2021-08-31 | 确成硅化学股份有限公司 | Preparation method of special high-dispersion white carbon black for high-ice-surface-gripping tire |
| CN113651332B (en) * | 2021-08-11 | 2023-10-27 | 常州大学 | Preparation method of high-performance white carbon black based on styrene-butadiene rubber reinforcement |
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Denomination of invention: Production process of highly dispersed white carbon black for snow tires Effective date of registration: 20230918 Granted publication date: 20150805 Pledgee: China Construction Bank Corporation Shahe Branch Pledgor: LONGXING CHEMICAL STOCK Co.,Ltd. Registration number: Y2023980057352 |