CN101774591B - Production technology of white microsphere high-strength white carbon black - Google Patents
Production technology of white microsphere high-strength white carbon black Download PDFInfo
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- CN101774591B CN101774591B CN2010101146483A CN201010114648A CN101774591B CN 101774591 B CN101774591 B CN 101774591B CN 2010101146483 A CN2010101146483 A CN 2010101146483A CN 201010114648 A CN201010114648 A CN 201010114648A CN 101774591 B CN101774591 B CN 101774591B
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Abstract
The invention discloses a production technology of white microsphere high-strength white carbon black, which takes sodium silicate and concentrated sulfuric acid as the main raw materials, uses the steps of dissolving, synthesizing, filter pressing, slurrying, drying and the like, and especially adopts the mode of adding aluminum oxide in the slurring step and combining the pressure type drying with fluidized bed secondary drying in the drying step to produce the white microsphere high-strength white carbon black with high strength, low broken rate, environment protection and easy dispersion. The microsphere high-strength white carbon black is very suitable for tire industry, can enhance fluidity and improve mixing capability of rubber.
Description
Technical field
The present invention relates to the production technique of WHITE CARBON BLACK, specifically, is a kind of production technique of white microsphere high-strength white carbon black.
Background technology
The chemical name of WHITE CARBON BLACK is the hydration soft silica, and molecular formula is SiO
2NH
2O is a kind of reinforcing filler of widespread use in rubber and the plastics industry, has porous, specific surface area is big, water-absorbent is strong, high temperature resistant, numerous advantages such as electrical insulating property is good.Producing the topmost method of WHITE CARBON BLACK is the precipitator method and vapor phase process; Vapor phase process is because complex process and with high costs and less with it; And be that traditional precipitator method of main raw material mainly adopt centrifugal drying plant with water glass and sulfuric acid; Products obtained therefrom is Powdered, in use very easily disperses, and environment is caused very big pollution.The granulation briquetting can effectively solve the problem that powder disperses, but the bad dispersibility of granulation product is unfavorable for that WHITE CARBON BLACK gives full play to its excellent reinforcement filling effect.
How the feature of environmental protection and polymolecularity being melted into a whole, is the developing direction of WHITE CARBON BLACK product of new generation.
Summary of the invention
The object of the invention is to provide a kind of production technique of white microsphere high-strength white carbon black; This technology is with low cost, method simple, safety and environmental protection; Both environmental protection and very easily disperseing of the WHITE CARBON BLACK of producing, intensity is high simultaneously, percentage of damage is low, is particularly suitable for being applied to tyre industry; Can strengthen flowability, improve the mixing ability of rubber.
Above-mentioned purpose realizes through following technique means:
With the water glass and the vitriol oil is main raw material, through dissolving, synthetic, press filtration, pulp, drying and other steps, has particularly adopted twice exsiccant technology of dried equipment of pressure-type spray and fluidized-bed, produces not only environmental protection but also dispersive microbead-shaped white carbon black very easily.
Concrete production technique comprises the steps:
(1) dissolving: with sodium silicate solid (Na
2OnSiO
2) and water add in the dissolving cylinder according to 2: 1 mass ratio, feed clean Sweet natural gas or warm air, under the pressure of 0.4~0.8Mpa, fully dissolved 2~3 hours, obtain transparent pure liquid soluble glass after leaching throw out, wherein Na
2OnSiO
2Degree Beaume (15.6 ℃) be 30~38 ° of B é;
(2) regulate: in the liquid soluble glass of step (1), add the water of its quality 1/4~1/8, to adjust wherein Na
2OnSiO
2Degree Beaume (15.6 ℃) to 20~30 ° of B é;
(3) synthetic: be 98% the vitriol oil with adjusted liquid soluble glass and concentration in the step (2) according to (15~16): 1 volume ratio adds in the synthesis reaction vessel simultaneously, and reaction is 90 minutes under 80 ℃~98 ℃ temperature, Na in the assurance reaction kettle in the reaction process
2The residual equivalent concentration of O is 7.0 ± 0.5, drips 98% the vitriol oil again PH is transferred to 4.6 ± 0.5, obtains silica slurry;
Reaction equation is following: Na
2OnSiO
2+ H
2SO
4→ nSiO
2+ Na
2SO
4+ H
2O;
Wherein modulus n is 3.2~3.5;
(4) press filtration: the silica slurry that step (3) obtains is passed through pressure filter; Charging 10~20 minutes under the pressure of 0.4~0.6Mpa earlier; Under the pressure of 0.5~0.6Mpa, washed 30~60 minutes then; Under the pressure of 0.4~0.8Mpa, squeezed 1~5 minute again, under the pressure of 0.4~0.8Mpa, be blown into clean Sweet natural gas or warm air 1~5 minute at last, to remove impurity Na wherein
2SO
4, form filter cake, guarantee that solid content in the filter cake is 20.0%~24.0%, sulphate content≤2.0%;
(5) pulp: the filter cake that step (4) is obtained adds in the pulp jar, to wherein adding aluminum oxide (every 7.5m
3Filter cake add 8 kilograms of aluminum oxide), be liquefied as the liquid of pasty state with whisking appliance, through the pulp transferpump constantly circulation with the viscosity controller of slurry below 1000cp, drip 98% the vitriol oil again PH transferred between 6.0~6.8;
(6) drying: the liquid that step (5) obtains is dry in the dried equipment of pressure-type spray earlier, carry out redrying through fluidized-bed again, promptly obtain white microsphere high-strength white carbon black of the present invention.
The present invention is a main raw material with the cheap water glass and the vitriol oil; Through dissolving, regulate, synthetic, press filtration, pulp, dry several simple process steps; Particularly in drying process, successively adopted the redrying technology of pressure type drying and fluidised bed drying; Both made that drying was more thorough; Can realize control through the pore size of spray gun and the feed pressure and the solid content of material in the dried equipment of adjusting pressure-type spray again, be prone to the dispersive microbead-shaped white carbon black thereby prepare uniform particles for microballon shape particle size; On the other hand, owing in the pulp process, added aluminum oxide, make the WHITE CARBON BLACK intensity for preparing obviously improve.The HS microbead-shaped white carbon black for preparing with production technique of the present invention neither is prone to disperse in air, has good dispersiveness again, is particularly suitable for being applied to tyre industry, can strengthen flowability, improves the mixing ability of rubber.
Embodiment
Below further describe the present invention through embodiment; Can know by technological general knowledge; The present invention also can describe through other the scheme that does not break away from technical characterictic of the present invention, thus all within the scope of the present invention or the change that is equal in the scope of the invention all comprised by the present invention.
Embodiment 1:
(1) with sodium silicate solid (Na
2OnSiO
2) and water add in the dissolving cylinder according to 2: 1 mass ratio, feed clean warm air, under the pressure of 0.4~0.8Mpa, fully dissolved 2~3 hours, obtain transparent pure liquid soluble glass after leaching throw out, wherein Na
2OnSiO
2Degree Beaume (15.6 ℃) be 30~38 ° of B é;
(2) water of its quality 1/4~1/8 of adding in the liquid soluble glass of step (1) is to adjust wherein Na
2OnSiO
2Degree Beaume (15.6 ℃) to 20~30 ° of B é;
(3) being 98% the vitriol oil with adjusted liquid soluble glass and concentration in the step (2) adds in the synthesis reaction vessel according to 15: 1 volume ratio simultaneously, and reaction is 90 minutes under 80 ℃~98 ℃ temperature, guarantees Na in the reaction kettle in the reaction process
2The residual equivalent concentration of O is 7.0 ± 0.5, drips 98% the vitriol oil again PH is transferred to 4.6 ± 0.5, obtains silica slurry;
(4) the silica slurry process pressure filter that step (3) is obtained; Charging 10~20 minutes under the pressure of 0.4~0.6Mpa earlier; Under the pressure of 0.5~0.6Mpa, washed 30~60 minutes then; Under the pressure of 0.4~0.8Mpa, squeezed 1~5 minute again, under the pressure of 0.4~0.8Mpa, be blown into clean Sweet natural gas or warm air 1~5 minute at last, to remove impurity Na wherein
2SO
4, form filter cake, guarantee that solid content in the filter cake is 20.0%~24.0% and sulphate content≤2.0%;
(5) filter cake that step (4) is obtained adds in the pulp jar, to wherein adding aluminum oxide (every 7.5m
3Filter cake add 8 kilograms of aluminum oxide); The control solid content is not less than 24%; Be liquefied as the liquid (can not add water in this process) of pasty state with whisking appliance; Through the pulp transferpump constantly circulation with the viscosity controller of slurry below 1000cp, drip 98% the vitriol oil again PH transferred between 6.0~6.8;
(6) the control feed pressure is 1.5~2Mpa; The liquid that step (5) is obtained carries out drying with the speed of 2500kg/h earlier in the dried equipment of TFD-800-N/B-FB10 type pressure-type spray of Denmark NIRO company; Carry out redrying through fluidized-bed again; Moisture controlled is separated fine powder through bag filter 6.0~7.0%, promptly obtains white microsphere high-strength white carbon black.
Claims (1)
1. the production technique of a white microsphere high-strength white carbon black is characterized in that, comprises the steps:
(1) dissolving: sodium silicate solid and water are dissolved in the cylinder according to 2: 1 mass ratio adding; Feed clean Sweet natural gas or warm air; Under the pressure of 0.4~0.8MPa, fully dissolved 2~3 hours; Obtain transparent pure liquid soluble glass after leaching throw out, wherein 15.6 of sodium silicate solid ℃ degree Beaume is 30~38 ° of B é;
(2) regulate: in the liquid soluble glass of step (1), add the water of its quality 1/4~1/8, to adjust wherein 15.6 ℃ degree Beaume to the 20~30 ° B é of sodium silicate solid;
(3) synthetic: be 98% the vitriol oil with adjusted liquid soluble glass and concentration in the step (2) according to (15~16): 1 volume ratio adds in the synthesis reaction vessel simultaneously, and reaction is 90 minutes under 80 ℃~98 ℃ temperature, Na in the assurance reaction kettle in the reaction process
2The residual equivalent concentration of O is 7.0 ± 0.5, drips 98% the vitriol oil again pH is transferred to 4.6 ± 0.5, obtains silica slurry;
Reaction equation is following: Na
2OnSiO
2+ H
2SO
4→ nSiO
2+ Na
2SO
4+ H
2O;
Wherein modulus n is 3.2~3.5;
(4) press filtration: the silica slurry that step (3) obtains is passed through pressure filter; Charging 10~20 minutes under the pressure of 0.4~0.6MPa earlier; Under the pressure of 0.5~0.6MPa, washed 30~60 minutes then; Under the pressure of 0.4~0.8MPa, squeezed 1~5 minute again, under the pressure of 0.4~0.8MPa, be blown into clean Sweet natural gas or warm air 1~5 minute at last, to remove impurity Na wherein
2SO
4, form filter cake, guarantee that solid content in the filter cake is 20.0%~24.0%, sulphate content≤2.0%;
(5) pulp: the filter cake that step (4) is obtained adds in the pulp jar, to wherein adding aluminum oxide, every 7.5m
3Filter cake add 8 kilograms of aluminum oxide, be liquefied as the liquid of pasty state with whisking appliance, through the pulp transferpump constantly circulation with the viscosity controller of slurry below 1000cp, drip 98% the vitriol oil again pH transferred between 6.0~6.8;
(6) drying: the liquid that step (5) obtains is dry in the dried equipment of pressure-type spray earlier, carry out redrying through fluidized-bed again, promptly obtain white microsphere high-strength white carbon black.
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Families Citing this family (9)
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CN102923722B (en) * | 2012-11-22 | 2015-04-01 | 株洲兴隆新材料股份有限公司 | Preparation method for white carbon black |
CN103332695B (en) * | 2013-06-13 | 2015-08-19 | 福建远翔化工有限公司 | A kind of white carbon black redrying method |
CN103466640B (en) * | 2013-09-02 | 2016-03-09 | 无锡恒诚硅业有限公司 | A kind of method reducing the standby white carbon black specific surface area BET of sulfuric acid precipitation legal system |
CN105329903A (en) * | 2014-08-08 | 2016-02-17 | 焦作市广安化工有限公司 | Preparation method for white carbon black |
CN104276577B (en) * | 2014-09-22 | 2016-08-24 | 无锡恒诚硅业有限公司 | A kind of have the precipitated silica of granule homogeneity, preparation method and its usage |
CN105060307B (en) * | 2015-09-09 | 2017-04-05 | 确成硅化学股份有限公司 | A kind of high-specific surface area white carbon and its production method |
CN106629754A (en) * | 2016-10-11 | 2017-05-10 | 福建正盛无机材料股份有限公司 | Preparation method for high-oil absorption microsphere-shaped 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 |
CN107686564B (en) * | 2017-10-30 | 2020-07-28 | 无锡恒诚硅业有限公司 | Preparation method of hydrophobic white carbon black |
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CN1699163A (en) * | 2005-06-08 | 2005-11-23 | 卢元健 | Process for producing white carbon black and sodium sulphite by sodium sulfate method |
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CN1699163A (en) * | 2005-06-08 | 2005-11-23 | 卢元健 | Process for producing white carbon black and sodium sulphite by sodium sulfate method |
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