CN106044790A - Method for preparing white carbon black with precipitation method - Google Patents
Method for preparing white carbon black with precipitation method Download PDFInfo
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- CN106044790A CN106044790A CN201610395299.4A CN201610395299A CN106044790A CN 106044790 A CN106044790 A CN 106044790A CN 201610395299 A CN201610395299 A CN 201610395299A CN 106044790 A CN106044790 A CN 106044790A
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- white carbon
- carbon black
- ammonium chloride
- hydrochloric acid
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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
- 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
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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
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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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- 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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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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
- C01P2006/80—Compositional purity
Abstract
The invention relates to white carbon black preparation in the field of chemical engineering, in particular to a method for preparing white carbon black with a precipitation method. The method for preparing white carbon black with the precipitation method comprises the following steps: (1) an n-butanol aqueous solution and sodium chloride are added to a reactor, a water glass solution is added, then a cationic surfactant is added, the mixture is stirred and heated, and the water glass solution, an ammonium chloride aqueous solution and hydrochloric acid are added to the reactor in a continuous parallel flow manner; (2) the pH value of a reaction is controlled to be 8-9 until the water glass solution is all added; (3) the ammonium chloride aqueous solution and hydrochloric acid are added, the pH value is regulate to be 4-5, aging is performed for 2 h, and slurry is obtained; (3) the slurry is filtered, washed with water and washed with ethanol; (5) a filter cake is ground and subjected to microwave drying and calcination, and white carbon black is obtained. The method has the advantages that the pH of the reaction is easy to control and primary particles are not prone to self-polymerization, and the prepared white carbon black has the characteristics of high specific surface area, high main content, high pore volume and the like.
Description
Technical field
The present invention relates to the preparation of chemical field white carbon, a kind of method being specifically related to preparing white carbon black by precipitation method.
Background technology
White carbon, as a kind of environmental protection, the auxiliary agent of excellent performance, has good activity and adsorption rate, and reinforcing effect is good,
There are the highest insulating properties, water insoluble and sour (except Fluohydric acid .), are dissolved in caustic soda, do not decomposed by high temperature.
White carbon is broadly divided into fume colloidal silica and precipitated silica by production method.Fume colloidal silica has relatively
Wholesale specific surface area, product purity is up to 99%, and particle diameter can reach 10-20nm, but this method reaction process is complicated, and product price
Costliness, is only used for only a few special industry.The tradition sedimentation method refer to sulphuric acid, hydrochloric acid, CO2It is that base stock is raw with waterglass
The technique producing white carbon, its yield is high, and technique is simple, is easily formed scale, and product quality relatively vapor phase method is poor, and it is widely used in rubber
The industries such as glue, the packing strengthening agent of plastics, electric industry insulation and thermal insulation filler and daily-use chemical industry raw material.But this method production process
In primary partical between autohemagglutination problem more serious, granular size is wayward, the particle diameter of product compared with big, pore volume is little and dispersibility
Difference.For improving white carbon black product performance, expand the application of product, base oneself upon tradition sedimentation method production technology exploitation high-quality Linesless charcoal
The preparation method of black product is particularly important.
Chinese patent CN 105329903 A discloses " preparation method of a kind of white carbon ", the white carbon that thus method prepares
There is preferable hot strength, but it uses concentrated sulphuric acid to participate in reaction, be unfavorable for controlling the pH of reaction, and to the requirement of equipment relatively
Height, adds production cost, and the method is preparing during white carbon easy autohemagglutination, specific surface area and hole between primary partical
Hold and remain a need for doing raising further.
Summary of the invention
For the deficiencies in the prior art, a kind of method that the invention provides preparing white carbon black by precipitation method, this method produced
In journey, the pH of reaction is easy to control, and primary partical is difficult to autohemagglutination, and product has the spies such as specific surface area content high, main is high, pore volume is big
Point.
For realizing object above, the present invention is achieved by the following technical programs:
A kind of method of preparing white carbon black by precipitation method, specifically includes following steps:
(1) n-butanol aqueous solution and sodium chloride are joined in the reactor with agitating device, add water glass solution,
Make the mass concentration of waterglass in reactor reach 1.5%-1.8%, add cationic surfactant, stirring, control to turn
Speed is 200r/min-300r/min, and temperature rises to 70-80 DEG C, keeps constant temperature, continuously adds water glass solution, ammonium chloride water
Solution and hydrochloric acid, continuously and to be added drop-wise in reactor in the way of flowing；
(2) with the pH value of accurate pH test paper detection reaction system, the pH value controlling reaction is 8-9, until water glass solution
Add；
(3) continuously adding aqueous ammonium chloride solution and hydrochloric acid, regulation rotating speed, to 150r/min-200r/min, slowly regulates pH
It is worth to 4-5, aging 2h, obtains slurry；
(4) releasing slurry from reactor, vacuum filters, washes after Cake Wash to neutrality with ethanol with deionized water again
Wash once；
(5) by filter cake pulverizing, microwave drying, at 600 DEG C, calcine 5h after being dried, obtain white carbon.
Preferably, in described n-butanol aqueous solution, the volume ratio of n-butyl alcohol and water is 1:15-1:19.
Preferably, the modulus of described water glass solution is 3.1-3.5, and mass concentration is 10%-25%, aqueous ammonium chloride solution
For saturated aqueous ammonium chloride, the mass concentration of hydrochloric acid is 25%-30%.
Preferably, the aqueous ammonium chloride solution added in described step (1) is 1:2-2:1 with the volume ratio of hydrochloric acid.
Preferably, described cationic surfactant is Dodecyl trimethyl ammonium chloride, cetyl trimethyl chlorination
One in ammonium, cetyl trimethylammonium bromide.
Preferably, the method controlling pH in described step (2) is: survey a pH value every 5min, if pH value is not in institute
In the range of Xuing, then suitably reduce or increase the flow of hydrochloric acid.
The present invention uses the aqueous solution of strong acid weak base salt ammonium chloride to carry out a point reaction with hydrochloric acid together as acid and waterglass,
The addition of hydrochloric acid ensure that reaction rate, and ammonium chloride can dilute H in aqueous slowly+, pH can be prevented effectively from and become
Changing excessive, additionally react and carry out in the basic conditions, the particle that reaction is generated is electronegative, can attract NH4 +With the Na in solution+
Form electric double layer, by the Coulomb repulsion effect between electric double layer, balance ion surface electric charge, so that occurring between particle
Reunite gravitation be substantially reduced.
Adding n-butyl alcohol in water and be because waterglass when being acidified in aqueous ,-ONa changes into-OH, is a kind of high table
The microgranule of area, the surface adsorption at it has substantial amounts of water, if dehydration, this combination will occur rapidly, increase rapidly into
Thick granule, and the existence of the polar molecule n-butyl alcohol added can play the effect of isolation, n-butanol molecule is by raw with top oxygen
Become hydrogen bond to stop top oxygen to form silicon-oxygen connection, thus prepare short grained white carbon.
It is electronegative in nucleation process that addition cationic surfactant is because white carbon, described cation surface activating
Agent can form micelle in the solution, adsorbs and wraps up and makes on microgranule, thus play the growth of suppression nucleus, control size
Effect.Due to the parcel of cationic surfactant, the foreign ion absorption to white carbon can be stoped, simultaneously in high-temperature calcination
Under, described cationic surfactant can decompose completely, will not introduce impurity, thus ensure that the purity of white carbon.
In reactant liquor, add appropriate inorganic electrolyte sodium chloride can weaken electrostatic as dispersant, the cation brought into
Effect, at SiO2Form a diffusion electric double layer around primary partical, mutually arrange between the cation of electric double layer shell positively charged
Repulsion is stablized more than the Van der Waals force between micelle, beneficially particle.
First be washed with deionized water to neutrality when filtering, then with washing with alcohol can make water in gel by ethanol replacement, when
When gel is dried and calcines, owing to the surface tension of water is shunk, pore volume is made to reduce, and after washing with alcohol, owing to water is by alcohol
Replace, the more difficult generation of above-mentioned phenomenon, thus produce bigger pore volume.
Microwave one quefrency of microwave drying is at the electromagnetic radiation as waves of 0.3-300GHz, and it is main with common mode of heating
Being different from its mode of heating is interior heating, and the latter is external heat, when therefore microwave heating can effectively eliminate heating process
Temperature gradient explained, there is homogeneous heating, heat time heating time is short and yield is high a little.The purpose carrying out calcining after drying be for
Removing surfactant, and the most dried calcining is to be to make the moisture in white carbon duct slowly remove at a lower temperature
Go, when temperature can be avoided too high, cause the pore structure of white carbon to change due to capillarity.
The invention has the beneficial effects as follows: a kind of method that the invention provides preparing white carbon black by precipitation method, this method produced
Journey use the aqueous solution of strong acid weak base salt ammonium chloride react with waterglass together with aqueous hydrochloric acid solution, it is ensured that reaction speed
Rate, makes again the pH of reaction easily controllable, simultaneously cationic surface controlling agent, sodium chloride, n-butyl alcohol synergism under, make former
Raw particle is difficult to autohemagglutination, and granular size is easy to control.In washing step, add the step of washing with alcohol and use microwave drying equal
Specific surface area and the pore volume of white carbon can be effectively improved.The preparation method of the present invention is simply efficient, beneficially industrialized production, by
The white carbon that the preparation method of the present invention prepares has the features such as specific surface area content high, main is high, pore volume is big.
Detailed description of the invention
In order to be more fully understood that the present invention, describe technical scheme in detail with instantiation below, but this
Invention is not limited thereto.
Embodiment 1:
A kind of method of preparing white carbon black by precipitation method, specifically includes following steps:
(1) n-butanol aqueous solution and sodium chloride are joined in the reactor with agitating device, add modulus be 3.3,
Mass concentration is the water glass solution of 20%, makes the mass concentration of waterglass in reactor reach 1.6%, adds dodecyl
Trimethyl ammonia chloride, stirring, controls rotating speed is 250r/min, and temperature rises to 75 DEG C, holding constant temperature, continuously add modulus be 3.3,
Mass concentration is the hydrochloric acid that water glass solution, saturated aqueous ammonium chloride and mass concentration are 28% of 20%, with continuously and flow
Mode be added drop-wise in reactor；
(2) with the pH value of accurate pH test paper detection reaction system, a pH value is surveyed every 5min, if pH value is not at 8-9
In the range of, then suitably reduce or increase the flow of aqueous hydrochloric acid solution, until water glass solution adds；
(3) continuously adding above-mentioned aqueous ammonium chloride solution and hydrochloric acid, regulation rotating speed is to 180r/min, and slowly regulation pH value is extremely
4.5, aging 2h, obtain slurry；
(4) releasing slurry from reactor, vacuum filters, washes after Cake Wash to neutrality with ethanol with deionized water again
Wash once；
(5) by filter cake pulverizing, microwave drying, at 600 DEG C, calcine 5h after being dried, obtain white carbon.
In described n-butanol aqueous solution, n-butyl alcohol is 1:17 with the volume ratio of water.
The aqueous ammonium chloride solution added in described step (1) is 1:1 with the volume ratio of hydrochloric acid.
Embodiment 2:
A kind of method of preparing white carbon black by precipitation method, specifically includes following steps:
(1) n-butanol aqueous solution and sodium chloride are joined in the reactor with agitating device, add modulus be 3.5,
Mass concentration is the water glass solution of 10%, makes the mass concentration of waterglass in reactor reach 1.8%, adds cetyl
Trimethyl ammonium chloride, stirring, control rotating speed is 200r/min, and temperature rises to 80 DEG C, keeps constant temperature, and continuously adding modulus is
3.5, mass concentration is the hydrochloric acid that water glass solution, saturated aqueous ammonium chloride and mass concentration are 25% of 10%, with continuously
And the mode flowed is added drop-wise in reactor；
(2) with the pH value of accurate pH test paper detection reaction system, a pH value is surveyed every 5min, if pH value is not at 8-9
In the range of, then suitably reduce or increase the flow of aqueous hydrochloric acid solution, until water glass solution adds；
(3) continuously adding above-mentioned aqueous ammonium chloride solution and hydrochloric acid, regulation rotating speed is to 200r/min, and slowly regulation pH value is to 4,
Aging 2h, obtains slurry；
(4) releasing slurry from reactor, vacuum filters, washes after Cake Wash to neutrality with ethanol with deionized water again
Wash once；
(5) by filter cake pulverizing, microwave drying, at 600 DEG C, calcine 5h after being dried, obtain white carbon.
In described n-butanol aqueous solution, n-butyl alcohol is 1:19 with the volume ratio of water.
The aqueous ammonium chloride solution added in described step (1) is 1:2 with the volume ratio of hydrochloric acid.
Embodiment 3:
A kind of method of preparing white carbon black by precipitation method, specifically includes following steps:
(1) n-butanol aqueous solution and sodium chloride are joined in the reactor with agitating device, add modulus be 3.1,
Mass concentration is the water glass solution of 25%, makes the mass concentration of waterglass in reactor reach 1.5%, then adds cetyl three
Methyl bromide ammonium, stirring, controls rotating speed is 300r/min, and temperature rises to 70 DEG C, holding constant temperature, continuously add modulus be 3.1,
Mass concentration is the hydrochloric acid that water glass solution, saturated aqueous ammonium chloride and mass concentration are 30% of 25%, with continuously and flow
Mode be added drop-wise in reactor；
(2) with the pH value of accurate pH test paper detection reaction system, a pH value is surveyed every 5min, if pH value is not at 8-9
In the range of, then suitably reduce or increase the flow of aqueous hydrochloric acid solution, until water glass solution adds；
(3) continuously adding above-mentioned aqueous ammonium chloride solution and hydrochloric acid, regulation rotating speed is to 150r/min, and slowly regulation pH value is to 5,
Aging 2h, obtains slurry；
(4) releasing slurry from reactor, vacuum filters, washes after Cake Wash to neutrality with ethanol with deionized water again
Wash once；
(5) by filter cake pulverizing, microwave drying, at 600 DEG C, calcine 5h after being dried, obtain white carbon.
In described n-butanol aqueous solution, n-butyl alcohol is 1:19 with the volume ratio of water.
The aqueous ammonium chloride solution added in described step (1) is 2:1 with the volume ratio of hydrochloric acid.
Embodiment 4:
A kind of method of preparing white carbon black by precipitation method, specifically includes following steps:
(1) n-butanol aqueous solution and sodium chloride are joined in the reactor with agitating device, add modulus be 3.4,
Mass concentration is the water glass solution of 15%, makes the mass concentration of waterglass in reactor reach 1.5%, adds cetyl
Trimethylammonium bromide, stirring, control rotating speed is 280r/min, and temperature rises to 77 DEG C, keeps constant temperature, and continuously adding modulus is
3.4, mass concentration is the hydrochloric acid that water glass solution, saturated aqueous ammonium chloride and mass concentration are 25% of 15%, with continuously
And the mode flowed is added drop-wise in reactor；
(2) with the pH value of accurate pH test paper detection reaction system, a pH value is surveyed every 5min, if pH value is not at 8-9
In the range of, then suitably reduce or increase the flow of aqueous hydrochloric acid solution, until water glass solution adds；
(3) continuously adding above-mentioned aqueous ammonium chloride solution and hydrochloric acid, regulation rotating speed is to 160r/min, and slowly regulation pH value is to 4,
Aging 2h, obtains slurry；
(4) releasing slurry from reactor, vacuum filters, washes after Cake Wash to neutrality with ethanol with deionized water again
Wash once；
(5) by filter cake pulverizing, microwave drying, at 600 DEG C, calcine 5h after being dried, obtain white carbon.
In described n-butanol aqueous solution, n-butyl alcohol is 1:18 with the volume ratio of water.
The aqueous ammonium chloride solution added in described step (1) is 2:1 with the volume ratio of hydrochloric acid.
Performance test:
Respectively the white carbon prepared in embodiment 1-4 being carried out performance detection, testing result is shown in Table 1.
The performance test of table 1 white carbon
As shown in Table 1, the preparation method of the present invention white carbon particle diameter content little, main preparing gained is high, is significantly larger than
Technology requirement, and the oil factor that had and high specific surface area.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, on the premise of without departing from the inventive method, it is also possible to makes some improvement and supplements, and these improve and supplement and should be regarded as this
The protection domain of invention.
Claims (6)
1. the method for a preparing white carbon black by precipitation method, it is characterised in that specifically include following steps:
(1) n-butanol aqueous solution and sodium chloride are joined in the reactor with agitating device, add water glass solution, make anti-
Answering the mass concentration of waterglass in device to reach 1.5%-1.8%, add cationic surfactant, stirring, controlling rotating speed is
200r/min-300r/min, rises to 70-80 DEG C by temperature, keeps constant temperature, continuously adds water glass solution, aqueous ammonium chloride solution
And hydrochloric acid, continuously and to be added drop-wise in reactor in the way of flowing；
(2) with the pH value of accurate pH test paper detection reaction system, the pH value controlling reaction is 8-9, until water glass solution adds；
(3) continuously adding aqueous ammonium chloride solution and hydrochloric acid, regulation rotating speed is to 150r/min-200r/min, and slowly regulation pH value is extremely
4-5, aging 2h, obtain slurry；
(4) releasing slurry from reactor, vacuum filters, and will use washing with alcohol one again with deionized water after Cake Wash to neutrality
Secondary；
(5) by filter cake pulverizing, microwave drying, at 600 DEG C, calcine 5h after being dried, obtain white carbon.
The method of preparing white carbon black by precipitation method the most according to claim 1, it is characterised in that in described n-butanol aqueous solution
N-butyl alcohol is 1:15-1:19 with the volume ratio of water.
The method of preparing white carbon black by precipitation method the most according to claim 1, it is characterised in that the mould of described water glass solution
Number is 3.1-3.5, and mass concentration is 10%-25%, and aqueous ammonium chloride solution is saturated aqueous ammonium chloride, the mass concentration of hydrochloric acid
For 25%-30%.
The method of preparing white carbon black by precipitation method the most according to claim 1, it is characterised in that add in described step (1)
The volume ratio of aqueous ammonium chloride solution and hydrochloric acid be 1:2-2:1.
The method of preparing white carbon black by precipitation method the most according to claim 1, it is characterised in that described cation surface activating
Agent is the one in Dodecyl trimethyl ammonium chloride, hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide.
The method of preparing white carbon black by precipitation method the most according to claim 1, it is characterised in that control in described step (2)
The method of pH is: survey a pH value every 5min, if pH value is the most within the required range, then suitably reduces or increase the stream of hydrochloric acid
Amount.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110769A (en) * | 2018-10-19 | 2019-01-01 | 广州市飞雪材料科技有限公司 | A kind of high dispersive silica and preparation method thereof |
| CN109319793A (en) * | 2018-11-12 | 2019-02-12 | 浙江新纳材料科技有限公司 | A kind of preparation method of Gao Bibiao, high oil absorption white carbon black |
| CN110627074A (en) * | 2019-11-11 | 2019-12-31 | 浙江新纳材料科技股份有限公司 | Preparation method and application of low-heat-conductivity and low-bulk-density white carbon black |
| CN112938989A (en) * | 2021-03-17 | 2021-06-11 | 江苏微纳光膜科技有限公司 | High-purity silicon dioxide for optical coating and preparation process thereof |
| CN113652004A (en) * | 2021-09-27 | 2021-11-16 | 无锡恒诚硅业有限公司 | White carbon black for green tires and preparation method thereof |
| CN113753905A (en) * | 2021-09-27 | 2021-12-07 | 无锡恒诚硅业有限公司 | Preparation method of high-dispersion white carbon black |
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| US20050192395A1 (en) * | 2004-02-03 | 2005-09-01 | Degussa Ag | Hydrophobic precipitated silica for defoamer formulations |
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| CN102583397A (en) * | 2012-01-09 | 2012-07-18 | 河北科技大学 | Method for preparing silicon dioxide and hydrogen chloride by means of hydrolysis of polysilicon by-product silicon tetrachloride |
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| US20050192395A1 (en) * | 2004-02-03 | 2005-09-01 | Degussa Ag | Hydrophobic precipitated silica for defoamer formulations |
| CN102167336A (en) * | 2011-03-21 | 2011-08-31 | 厦门大学 | Preparation method of mesoporous silicon dioxide hollow sphere |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110769A (en) * | 2018-10-19 | 2019-01-01 | 广州市飞雪材料科技有限公司 | A kind of high dispersive silica and preparation method thereof |
| WO2020078029A1 (en) * | 2018-10-19 | 2020-04-23 | 广州市飞雪材料科技有限公司 | High-dispersion silica and preparation method therefor |
| CN109319793A (en) * | 2018-11-12 | 2019-02-12 | 浙江新纳材料科技有限公司 | A kind of preparation method of Gao Bibiao, high oil absorption white carbon black |
| CN109319793B (en) * | 2018-11-12 | 2022-07-15 | 浙江新纳材料科技股份有限公司 | Preparation method of high-specific-surface high-oil-absorption white carbon black |
| CN110627074A (en) * | 2019-11-11 | 2019-12-31 | 浙江新纳材料科技股份有限公司 | Preparation method and application of low-heat-conductivity and low-bulk-density white carbon black |
| CN110627074B (en) * | 2019-11-11 | 2023-09-15 | 浙江新纳材料科技股份有限公司 | Preparation method and application of low-heat-conductivity low-bulk-density white carbon black |
| CN112938989A (en) * | 2021-03-17 | 2021-06-11 | 江苏微纳光膜科技有限公司 | High-purity silicon dioxide for optical coating and preparation process thereof |
| CN112938989B (en) * | 2021-03-17 | 2023-07-25 | 江苏微纳光膜科技有限公司 | High-purity silicon dioxide for optical coating and preparation process thereof |
| CN113652004A (en) * | 2021-09-27 | 2021-11-16 | 无锡恒诚硅业有限公司 | White carbon black for green tires and preparation method thereof |
| CN113753905A (en) * | 2021-09-27 | 2021-12-07 | 无锡恒诚硅业有限公司 | Preparation method of high-dispersion white carbon black |
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Denomination of invention: Method for preparing white carbon black by precipitation method Effective date of registration: 20210728 Granted publication date: 20180109 Pledgee: Hanshan County sub branch of Postal Savings Bank of China Limited Pledgor: ANHUI HANSHAN JINHUA ZINC OXIDE PLANT Registration number: Y2021980006904 |