CN111498859A - Preparation method of high-transparency high-dispersibility white carbon black - Google Patents
Preparation method of high-transparency high-dispersibility white carbon black Download PDFInfo
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2321/00—Characterised by the use of unspecified rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
Abstract
The invention discloses a preparation method of high-transparency high-dispersity white carbon black, which comprises the following operation steps: synthesizing a magnesium aluminum silicate dispersion inducer: adding water and silicate into a reaction kettle in sequence under the condition of stirring, heating to 60-80 ℃, adding a magnesium compound solution under vigorous stirring, and reacting to form a magnesium and silicon-containing base solution slurry; dropwise adding an aluminum compound aqueous solution, adjusting the pH value of the slurry to 10-14 by using a saturated alkali solution, and continuously reacting to obtain a dispersion inducer magnesium aluminum silicate suspension; a second part: synthesizing a high-transparency high-dispersity white carbon black covering layer by using a magnesium aluminum silicate dispersion inducer: adding the magnesium aluminum silicate suspension and bottom water into a reaction kettle, adding silicate, stirring and heating to 75-95 ℃ to ensure that the pH of the bottom liquid is 8-10, simultaneously adding silicate and acidifying agent, keeping the pH of 8-10, stopping adding the silicate, and continuing adding the acidifying agent until the pH value is 3.5-5.0 to obtain the high-transparency high-dispersity high-whiteness carbon black slurry; filtering, washing, drying and briquetting to obtain the granular high-transparency high-dispersity white carbon black product.
Description
Technical Field
The invention relates to a preparation method of an inorganic powder material, in particular to a preparation method of high-transparency high-dispersity white carbon black.
Background
The precipitated hydrated silicon dioxide is also called white carbon black, and is a non-toxic, tasteless and pollution-free non-metallic material. White carbon black is an important chemical raw material and is widely applied to various fields of rubber, silicon rubber, paint, coating, high-grade daily cosmetics and the like. The high-dispersion silica has special properties different from the conventional white carbon black, so that the high-dispersion silica has high added value application. In rubber application, the white carbon black cannot be well dispersed in a rubber polymer structure after rubber is added due to more micropores of the white carbon black, so that the processing performance is poor and the heat generation is high; on the other hand, the micropores can adsorb more accelerators, so that rubber macromolecules cannot contact with the white carbon black, the vulcanization rate is influenced, and the vulcanization is delayed.
The transparency and the dispersibility of the white carbon black have great influence on the application performance of the product, but the transparency and the dispersibility have great contradiction. Because the size of the primary particles of the white carbon black can affect the transparency of the product, when the particle size of the primary particles becomes smaller, the transparency of the white carbon black is correspondingly improved; however, the specific surface area of the white carbon black produced by the primary particles with small particle size is correspondingly increased, so that the surface energy of the white carbon black is correspondingly increased, and further, different particles are easy to agglomerate, so that the dispersion performance of the white carbon black is reduced. The refractive index of the white carbon black is 1.46-1.52, which is close to the refractive index of 1.4-1.5 of the common rubber, so that the white carbon black can be used as the reinforcing agent to fill the rubber to prepare white or colored transparent products. With the improvement of the performance of the precipitated white carbon black product and the rising of the demand of the color rubber product, the application of the high-transparency high-dispersity white carbon black product in the rubber industry has wide development space.
Patent CN102229758B discloses a "preparation method of highly dispersed white carbon black", which mainly comprises performing synthesis reaction in two steps, firstly synthesizing fine silica crystal seeds, then performing modification treatment, wherein the modification treatment is a precipitation reaction performed under the action of organic surfactant SDS and a composite silane coupling agent, and then performing particle surface coating and modification treatment, washing and drying to obtain the highly dispersed precipitated white carbon black of a high-performance tire; although this method is surface-treated, the deterioration of dispersibility due to self-aggregation of primary particles is a disadvantage of this process. On the basis, the patentee discloses a process method for preparing high-transparency high-dispersity white carbon black by in-situ synthesis of a magnesium aluminum silicate dispersion inducer through further development, and aims to ensure that the white carbon black product has higher transparency while keeping higher dispersity in the application of rubber, silicon rubber and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of high-transparency high-dispersity white carbon black, so that the prepared white carbon black has good transparency and dispersity in rubber, silicon rubber and other applications.
In order to realize the purpose, the preparation method of the high-transparency high-dispersity white carbon black adopts the in-situ synthesis of the aluminum magnesium silicate dispersion inducer to prepare the high-transparency high-dispersity white carbon black product, and the operation steps are as follows:
A. in-situ synthesis of a magnesium aluminum silicate dispersion inducer:
a1, adding water into a reaction kettle, and adding water according to a volume ratio V: adding silicate with the modulus of 2.5-3.5 under the stirring condition, heating to 60-80 ℃, gradually adding a magnesium compound aqueous solution with the mass fraction of 10.0-30.0% under vigorous stirring, and reacting within 0.5-2.0 h to form a magnesium and silicon-containing base solution slurry;
a2, adding an aluminum compound aqueous solution with the mass fraction of 40.0-60.0% into the slurry prepared in the step A1, dropwise adding the aluminum compound aqueous solution within 0.5-2.0 h, adjusting the pH of the slurry to 10-14 with a saturated alkali solution, and continuously reacting for 0.5-2.0 h to obtain a dispersion inducer magnesium aluminum silicate suspension, wherein the suspension can be directly applied to the next reaction for synthesizing high-transparency high-dispersibility silicon dioxide;
the volume ratio of the magnesium compound to the aluminum compound is V magnesium compound: the V aluminum compound is 2: 3-7: 3, and the adding amount of the V aluminum compound and the V silicate is as follows according to the volume ratio: the total amount of the magnesium compound and the aluminum compound is 1: 3-6: 3;
B. synthesizing a high-transparency high-dispersity white carbon black covering layer by using a magnesium aluminum silicate dispersion inducer:
b1, adding the magnesium aluminum silicate suspension obtained from the step A2 and bottom water into a reaction kettle, adding silicate with the modulus of 2.5-3.5, and heating to 75-95 ℃ under the stirring condition to enable the pH of the bottom liquid in the reaction kettle to be 8-10; the adding amount of the aluminum magnesium silicate solution accounts for 0.5 to 5.0 percent of the mass fraction of the total components;
b2, adding silicate with the modulus of 2.5-3.5 and an acidifying agent with the mass fraction of 50% -98% into the reaction bottom material obtained in the step B1 simultaneously, so that the pH of the reaction medium is 8-10; the flow rate of the silicate is 10-20 m3The flow velocity of the acidifying agent is 0.5-2.0 m3H, of silicates and acidifying agentsThe feeding time is 1-2 h;
b3, stopping adding the silicate, and continuously adding an acidifying agent into the reaction kettle, wherein the flow rate of the acidifying agent is 0.5-2.0 m3Feeding for 20-60 min, and stopping adding the acidifying agent until the pH value reaches 3.5-5.0 to obtain the high-transparency high-dispersity high-white carbon black slurry;
b4, filtering, washing and drying the slurry obtained in the step B3 to obtain a powdery or microbead-shaped white carbon black product, and briquetting to obtain a granular high-transparency high-dispersity white carbon black product, wherein the product comprises an aluminum magnesium silicate dispersion inducer and a silicon dioxide covering layer, and the aluminum magnesium silicate accounts for 0.5-5.0% of the total weight of the components; the aluminum magnesium silicate comprises the following components in percentage by mass: na (Na)2O 1.0％～10.0％、MgO 5.0％～15.0％、Al2O325.0％～35.0％、SiO230.0％～50.0％、H2O 5.0％～15.0％。
The acidifying agent is any form of acid including sulfuric acid, nitric acid, oxalic acid, preferably concentrated sulfuric acid.
The silicate is any form of silicate including potassium silicate, sodium silicate, ethyl silicate, preferably sodium silicate.
The aluminum compound is any form of water soluble aluminum including aluminum chloride, aluminum nitrate, potassium aluminum sulfate dodecahydrate, aluminum sulfate, preferably aluminum sulfate.
The magnesium compound is any form of water soluble magnesium including magnesium oxide, magnesium carbonate, magnesium chloride, magnesium sulphate, preferably magnesium sulphate.
The alkali solution is any form of water soluble alkali including lithium hydroxide, sodium hydroxide, potassium hydroxide, preferably sodium hydroxide.
The reaction is carried out under the condition of stirring, and the stirring frequency is 38-47 Hz, preferably 40-45 Hz.
The magnesium aluminum silicate dispersion inducer has a unique three-dimensional chain structure and a special needle and rod-shaped crystal structure, forms a 'card palace' type association network structure in an aqueous medium, has good suspension stability, bonding thixotropy, adsorbability and stability, can inhibit the agglomeration of silicon dioxide, and improves the dispersibility of the silicon dioxide.
The preparation method of the high-transparency high-dispersity white carbon black has the following technical characteristics and beneficial effects:
1. the magnesium aluminum silicate dispersion inducer is obtained through prefabrication, so that silicon dioxide is attached to the surface of magnesium aluminum silicate and grows orderly, and falls off when the silicon dioxide covering layer reaches a certain thickness, thereby being beneficial to uniform growth of primary particles of the silicon dioxide and enabling the white carbon black product to have higher transparency.
2. The suspension property of the magnesium aluminum silicate inhibits the sedimentation of silicon dioxide, the agglomeration is not easy to occur, the uniform silicon dioxide particles are favorably formed, the particle size distribution is narrow, the compatibility of the white carbon black product in a rubber polymer matrix is improved, and the reinforcing property of the rubber is improved.
3. Magnesium silicate and other substances are generated in the process of magnesium aluminum silicate composite reaction, and the substances have certain adsorbability to pigment substances and can further promote the transparency of the white carbon black product.
Detailed Description
The preparation method of the high-transparency high-dispersibility white carbon black of the invention is further described in detail with reference to the specific embodiments.
Example 1
The preparation method of the high-transparency high-dispersity white carbon black is operated according to the following steps:
A. in-situ synthesis of a magnesium aluminum silicate dispersion inducer:
a1, adding 5.0L of water into a 50.0L reaction kettle, adding 12.0L of sodium silicate under the condition of stirring, introducing steam, heating to 60 ℃, and gradually adding a magnesium sulfate aqueous solution under vigorous stirring, wherein the modulus of the sodium silicate is 2.5, the adding time of the magnesium sulfate aqueous solution is 30min, the mass fraction of the magnesium sulfate aqueous solution is 20.0%, and the adding amount of the magnesium sulfate aqueous solution is 5.0L, so that magnesium and silicon-containing bottom liquid slurry is formed through reaction;
a2, adding an aluminum sulfate aqueous solution into the slurry, after dropwise addition within 1.0h, adjusting the pH of the slurry to 14 by using a sodium hydroxide solution, and continuing to react for 1.0 to obtain an aluminum magnesium silicate suspension, wherein the mass fraction of the aluminum sulfate aqueous solution is 45.0%, and the addition amount of the aluminum sulfate aqueous solution is 7.0L;
the magnesium aluminum silicate dispersion inducer prepared by the in-situ synthesis method is directly applied to the next reaction for synthesizing the high-transparency high-dispersity silicon dioxide without separation and drying.
B. Synthesizing a high-transparency high-dispersity white carbon black covering layer by using a magnesium aluminum silicate dispersion inducer:
b1, taking the magnesium aluminum silicate suspension liquid 500m L obtained from A2 and bottom water 7.0L, introducing steam, heating to 80 ℃, adding sodium silicate, and uniformly stirring to keep the pH value in the reaction kettle at 9.0, wherein the modulus of the sodium silicate is 2.5;
b2, adding sodium silicate and concentrated sulfuric acid into the reaction substrate at the same time, wherein the flow rate of the sodium silicate is 70m L/min, the modulus is 2.5, the flow rate of the concentrated sulfuric acid is 5.0m L/min, the feeding time of the sulfuric acid and the sodium silicate is 60min, and the pH value of the reaction medium is kept at 9.0;
b3, stopping adding silicate, continuing to add concentrated sulfuric acid into the reaction kettle until the pH value of the obtained reaction slurry is 4.0, and stopping adding sulfuric acid, wherein the flow rate of the concentrated sulfuric acid is 5.0m L/min, the feeding time is 30min, and the high-transparency high-dispersibility white carbon black product suspension is obtained after curing;
and B4, filtering and washing the suspension obtained in the step B3, and then obtaining a powdery or microbead-shaped white carbon black product after flash drying or spray drying, and obtaining a granular high-transparency high-dispersity white carbon black product after briquetting.
Example 2
The reaction temperature in step B1 was 85 ℃ and the other steps and parameters were the same as in example 1.
Example 3
Step B1 magnesium aluminium silicate suspension 1000m L, the other steps and parameters were the same as in example 1.
The comparative analysis of the comprehensive chemical property indexes of the high-transparency high-dispersity white carbon black product prepared by the three examples and the common white carbon black is shown in table 1.
TABLE 1 comparison of the chemical indexes of the respective products
| Technical index | Example 1 | Example 2 | Example 3 | Common white carbon black |
| Degree of transparency% | 96 | 96 | 96 | 90 |
| Coefficient of Dispersion WK (S) | 0.8 | 0.8 | 0.7 | 1.7 |
| BET，m2/g | 184 | 176 | 182 | 185 |
| CTAB，m2/g | 172 | 175 | 171 | 158 |
| Oil absorption number, cm3/g | 2.35 | 2.36 | 2.41 | 2.32 |
| Surface hydroxyl groups, mmol/5g | 15.31 | 15.42 | 15.41 | 19.60 |
As can be seen from Table 1, the white carbon black products prepared by the three embodiments of the preparation method of the high-transparency high-dispersibility white carbon black have higher transparency than the common white carbon black product, and the dispersion coefficient is obviously smaller than that of the common white carbon black product, which indicates that the white carbon black product prepared by the invention is easier to disperse in rubber; the difference value between BET and CTAB of the white carbon black product prepared in the embodiment is smaller than that of common white carbon black, which shows that the surface roughness of the white carbon black of the embodiment is low, and the reinforcing property of rubber is better than that of the common white carbon black; the surface hydroxyl content of the white carbon black product in the embodiment is lower than that of the comparative example, which shows that the white carbon black prepared by the invention can reduce the surface silicon hydroxyl content, so that the compatibility of the white carbon black and rubber is improved, and the reinforcing performance of the rubber can be further promoted.
Comparing the above three examples, the best technical index is combined in example 3, which is the best example.
The above embodiments are not intended to limit the present invention, and those skilled in the art may still modify the technical solutions described in the above embodiments or substitute some technical features. 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-transparency high-dispersibility white carbon black is characterized by comprising the following steps: the preparation method of the high-transparency high-dispersity white carbon black product by adopting the in-situ synthesis of the aluminum magnesium silicate dispersion inducer comprises the following operation steps of:
A. in-situ synthesis of a magnesium aluminum silicate dispersion inducer:
a1, adding water into a reaction kettle, and adding water according to a volume ratio V: adding silicate with the modulus of 2.5-3.5 under the stirring condition, heating to 60-80 ℃, gradually adding a magnesium compound aqueous solution with the mass fraction of 10.0-30.0% under vigorous stirring, and reacting within 0.5-2.0 h to form a magnesium and silicon-containing base solution slurry;
a2, adding an aluminum compound aqueous solution with the mass fraction of 40.0-60.0% into the slurry prepared in the step A1, dropwise adding the aluminum compound aqueous solution within 0.5-2.0 h, adjusting the pH of the slurry to 10-14 with a saturated alkali solution, and continuously reacting for 0.5-2.0 h to obtain a dispersion inducer magnesium aluminum silicate suspension, wherein the suspension can be directly applied to the next reaction for synthesizing high-transparency high-dispersibility silicon dioxide;
the volume ratio of the magnesium compound to the aluminum compound is V magnesium compound: the V aluminum compound is 2: 3-7: 3, and the adding amount of the V aluminum compound and the V silicate is as follows according to the volume ratio: the total amount of the magnesium compound and the aluminum compound is 1: 3-6: 3;
B. synthesizing a high-transparency high-dispersity white carbon black covering layer by using a magnesium aluminum silicate dispersion inducer:
b1, adding the magnesium aluminum silicate suspension obtained from the step A2 and bottom water into a reaction kettle, adding silicate with the modulus of 2.5-3.5, and heating to 75-95 ℃ under the stirring condition to enable the pH of the bottom liquid in the reaction kettle to be 8-10; the adding amount of the aluminum magnesium silicate solution accounts for 0.5 to 5.0 percent of the mass fraction of the total components;
b2, adding silicate with the modulus of 2.5-3.5 and an acidifying agent with the mass fraction of 50% -98% into the reaction bottom material obtained in the step B1 simultaneously, so that the pH of the reaction medium is 8-10; the flow rate of the silicate is 10-20 m3The flow velocity of the acidifying agent is 0.5-2.0 m3The charging time of the silicate and the acidifying agent is 1-2 h;
b3, stopping adding the silicate, and continuously adding an acidifying agent into the reaction kettle, wherein the flow rate of the acidifying agent is 0.5-2.0 m3Feeding for 20-60 min, and stopping adding the acidifying agent until the pH value reaches 3.5-5.0 to obtain the high-transparency high-dispersity high-white carbon black slurry;
b4, filtering, washing and drying the slurry obtained in the step B3 to obtain a powdery or microbead-shaped white carbon black product, and briquetting to obtain a granular high-transparency high-dispersity white carbon black product, wherein the product comprises an aluminum magnesium silicate dispersion inducer and a silicon dioxide covering layer, and the aluminum magnesium silicate accounts for 0.5-5.0% of the total weight of the components; the aluminum magnesium silicate comprises the following components in percentage by mass: na (Na)2O 1.0％～10.0％、MgO 5.0％～15.0％、Al2O325.0％～35.0％、SiO230.0％～50.0％、H2O 5.0％～15.0％。
2. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1, which is characterized in that: the acidifying agent is any form of acid including sulfuric acid, nitric acid, oxalic acid.
3. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1 or 2, which is characterized in that: the acidifying agent is concentrated sulfuric acid.
4. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1, which is characterized in that: the silicate is any form of silicate including potassium silicate, sodium silicate, ethyl silicate.
5. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1 or 4, which is characterized in that: the silicate is sodium silicate.
6. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1, which is characterized in that: the aluminum compound is any form of water soluble aluminum including aluminum chloride, aluminum nitrate, potassium aluminum sulfate dodecahydrate, aluminum sulfate.
7. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1 or 6, which is characterized in that: the aluminum compound is aluminum sulfate.
8. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1, which is characterized in that: the magnesium compound is any form of water soluble magnesium including magnesium oxide, magnesium carbonate, magnesium chloride, magnesium sulfate.
9. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1 or 8, which is characterized in that: the magnesium compound is magnesium sulfate.
10. The method for preparing the white carbon black with high transparency and high dispersibility as claimed in claim 1, which is characterized in that: the alkali solution is any form of water soluble alkali including sodium hydroxide, potassium hydroxide, lithium hydroxide.
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| CN113027447A (en) * | 2021-03-11 | 2021-06-25 | 重庆工程职业技术学院 | Coal mining electromechanical device |
| 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 |
| CN114085553A (en) * | 2021-12-07 | 2022-02-25 | 无锡恒诚硅业有限公司 | Device and method for producing high-dispersion white carbon black |
| CN114604874A (en) * | 2022-04-01 | 2022-06-10 | 金三江(肇庆)硅材料股份有限公司 | High-refraction macroporous precipitated silica for high-transparency silicone rubber and preparation method thereof |
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