CN115340101B - Production method of silicon dioxide for green tire - Google Patents
Production method of silicon dioxide for green tire Download PDFInfo
- Publication number
- CN115340101B CN115340101B CN202210874423.0A CN202210874423A CN115340101B CN 115340101 B CN115340101 B CN 115340101B CN 202210874423 A CN202210874423 A CN 202210874423A CN 115340101 B CN115340101 B CN 115340101B
- Authority
- CN
- China
- Prior art keywords
- sulfuric acid
- reactor
- dilute sulfuric
- silica
- green tire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of silica production, and discloses a production method of silica for green tires, which comprises the following steps: s1, adding a dispersing agent containing soluble silicon dioxide into a base solution of a reactor; s2, stirring is started, and meanwhile, the reaction solution is heated, and seed crystal preparation is carried out; s3, continuously heating after the preparation of the seed crystal, and adding quantitative dilute sulfuric acid and dilute sodium silicate into a reactor to carry out a synthesis reaction while heating to obtain slurry; s4, continuously adding dilute sulfuric acid to acidify the slurry; and S5, adding quantitative sodium metaaluminate as a pulping aid in the pulping process, and then adding dilute sulfuric acid to adjust the PH. By adopting the method, the materials which are involved in the reaction in the reactor are more stable and uniform in the reaction process, so that the comprehensive properties of the silica in the tire, such as dispersibility, reinforcement and the like, are improved, and the physicochemical properties of the silica are ensured to meet the index requirements.
Description
Technical Field
The invention relates to the technical field of silicon dioxide production, in particular to a production method of silicon dioxide for green tires.
Background
Precipitation of hydrated silicon dioxide SiO 2 ·nH 2 O is a chemically synthesized amorphous silicic acid product, the appearance is white powder, the main component is silicon dioxide, the silicon dioxide is insoluble in water and acid, the silicon dioxide becomes aggregated fine particles after absorbing water, the silicon dioxide can be dissolved in sodium hydroxide and hydrofluoric acid when being heated, the silicon dioxide is stable to other chemicals, the silicon dioxide is high-temperature resistant and non-combustible, has good electrical insulation property, and is widely applied to the industries of rubber, plastics, papermaking, coating, pesticides, food, daily chemicals and the like.
In recent years, the quality requirements of tire enterprises on white carbon black are continuously improved, the quality of white carbon black products is required to be stable, the addition amount is required to be large, and the reinforcing performance and the dispersing performance are required to be good. The black cat company is the largest domestic carbon black producer, and is also the fourth carbon black producer in the world, and with the acceleration of the diversification and globalization development pace, the company is advancing to the third largest carbon black company in the world. Silica is one of the industrial directions of important development of companies, improves the dispersibility of silica in rubber, and develops the silica for the green tire with special performance, which is a technical key of industrial development, and is also a requirement of development in the field of rubber tire manufacturing, and has great significance for black cat companies to adjust product structures, improve economic benefits of enterprises and keep the advanced advantages of the black cat companies in the domestic carbon black industry.
At present, the brands of silica products at home and abroad are hundreds, the application field is very wide, and most white carbon black enterprises have small device scale, low automation degree and poor product quality, so that the prepared product has unsatisfactory dispersion performance, or the silica with excellent quality can be obtained only by prolonging the reaction time and greatly reducing the production efficiency, and is difficult to be utilized in actual production.
Disclosure of Invention
In view of the above, the invention provides a method for producing silicon dioxide for green tires, which aims to solve the problems of poor reinforcement, low production efficiency and poor uniformity of products caused by the difficulty in dispersing the existing precipitated hydrated silicon dioxide in rubber.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for producing silica for green tires, comprising the steps of:
s1, adding a dispersing agent containing soluble silicon dioxide into a base solution of a reactor;
s2, stirring is started, and meanwhile, the reaction solution is heated, and seed crystal preparation is carried out;
s3, continuously heating after the preparation of the seed crystal is finished, and simultaneously adding dilute sulfuric acid and dilute sodium silicate into a reactor for synthesis reaction to obtain slurry;
s4, continuously adding dilute sulfuric acid to acidify the slurry; .
S5, filtering, washing and preparing a filter cake from the acidified slurry, conveying the filter cake into a pulping system, adding a pulping auxiliary agent in the pulping process, adding dilute sulfuric acid to adjust the PH, and drying after pulping.
Preferably, in the above method for producing silica for green tire, the base solution is prepared from a diluted sodium silicate having a modulus m=3.4 to 3.6 in water, and the density of the diluted sodium silicate is 1.180 to 1.280kg/L.
Preferably, in the above-mentioned method for producing silica for green tire, the dispersant in step S1 is Na in a volume ratio of 100 (1-2) 2 SO 4 And soluble silica SiO 2 ·nH 2 Mixed solution of O and Na 2 SO 4 The mass percentage concentration of (2) is 4-6%, soluble silicon dioxide SiO 2 ·nH 2 The mass percentage concentration of O is 0.04-0.12%.
Preferably, in the above method for producing silica for green tire, the soluble silica SiO 2 ·nH 2 The iron content of O is not higher than 115ppm.
Preferably, in the above-mentioned production method of silica for green tire, the dispersant is added in an amount of 30 to 50% by mass of the total mass of the base liquid in step S1.
The beneficial effects of the technical scheme are as follows: the dispersing agent is added into the base solution, so that the uniformity of the particle size of the precipitated silica can be effectively improved.
Preferably, in the above-mentioned production method of silica for green tire, the stirring rate in step S2 is 75rpm; the temperature of the reaction solution was raised to 70.+ -. 1 ℃.
Further preferably, in step S2, the stirring device of the reactor is started, the stirring rotation speed is controlled at 75rpm, and meanwhile, the heating steam valve of the reactor is started to introduce steam into the reactor, the steam pressure is more than or equal to 6.0kg, and the temperature of the bottom solution in the reactor is raised to 70+/-1 ℃.
Preferably, in the above-mentioned production method of silica for green tire, the seed preparation in step S2 includes: dilute sulfuric acid is added into the reactor until the pH value is 7-8, and the seed crystal preparation is completed.
Further preferably, the seed crystal preparation in step S2 includes: adding dilute sulfuric acid with the concentration of 7-9% into a reactor, detecting the pH value in real time, stopping adding acid when the pH value of feed liquid in the reactor reaches 7-8, and finishing the preparation of the seed crystal.
Preferably, in the above production method of silica for green tire, the addition rate of the dilute sulfuric acid in the seed crystal preparation process is 2000-2300Kg/h, and the density of the dilute sulfuric acid is 1000-1010Kg/m 3 The definition of dilute sulfuric acid density is herein mainly to prevent local reaction to form gel upon addition, affecting product structure and performance.
Preferably, in the above-mentioned production method of silica for green tire, the temperature rise in step S3 is to raise the temperature from 70±1 ℃ to 86 to 96 ℃ at a rate of 3 to 5 ℃/min.
Further preferably, in the above-mentioned production method of silica for green tire, the temperature rise in step S3 is to raise the temperature of the feed liquid in the reactor from 70±1 ℃ to 86 to 96 ℃ at a rate of 3 to 5 ℃/min in a period of 10 to 20 minutes, and the whole temperature rise process is carried out simultaneously with the synthesis reaction.
The beneficial effects of the technical scheme are as follows: through controlling the stirring speed and the temperature, the materials which are involved in the reaction kettle are fully, softly and uniformly mixed and reacted, and the consistency of the internal and external structures of the silicon dioxide reaction product aggregate is improved, so that the dispersibility, the reinforcing property and the comprehensive performance of the silicon dioxide in the green tire are improved, and the physicochemical property of the silicon dioxide is ensured to meet the index requirements.
Preferably, in the above-mentioned production method of silica for green tire, the pH value of the synthesis reaction in step S3 is controlled to 7 to 8.
Preferably, in the above production method of silica for green tire, dilute sulfuric acid is added to a pH of 4 to 6 in step S4, and the acid addition time is controlled to be 5 to 10min.
Further preferably, when the pH value of the feed liquid in the step S4 reaches 4-6, stopping adding acid, continuing stirring for 3-5min, and ending the reaction to fix the aggregate structure.
Preferably, in the method for producing silica for green tire, in the step S5, the beating aid is sodium metaaluminate, and the addition amount of the beating aid is 4-6% of the total amount of the slurry, and dilute sulfuric acid is added to adjust the pH to 6.0±0.1.
The beneficial effects of the technical scheme are as follows: according to the invention, by adding proper amounts of sodium metaaluminate and sulfuric acid in the pulping process, the pulping effect is greatly improved, the dispersion performance and the reinforcing performance of the product are improved, and the vulcanizing time of the sizing material for producing the green tire is in a reasonable range by adjusting the stable pH value.
Preferably, the method for producing silica for green tire further comprises:
and S6, after the reaction is finished, opening an electric control discharge valve of the reactor, discharging materials in the reactor into a storage tank, and cleaning the inner wall of the reactor through a cleaning device.
Preferably, in the method for producing silica for green tires, the sodium silicate and the dispersant are both recycled after filtration and purification treatment of the reaction water.
The technical scheme has the beneficial effects that the inner wall of the reactor is cleaned, so that the accumulation of stock on the inner wall of the reactor is prevented from affecting feeding, and the corrosion of long-time accumulation to the reactor is avoided.
The invention provides a production method of silicon dioxide for green tires, which has the beneficial effects that compared with the prior art:
(1) The initial stage of the reaction is carried out in the environment of low temperature 70+/-1 ℃, because the aggregate particle structure in the initial stage of the reaction is simple, the surface of the particle is easier to form larger and relatively uniform holes by adopting low-temperature reaction, when the initial particle diameter of the silicon dioxide is increased to 10-30nm, the temperature is increased, the temperature increasing rate of the reaction is strictly controlled, the reaction temperature is continuously increased step by step, the reaction is promoted to be intensified along with the increase of the reaction temperature, the growth speed of the silicon dioxide particles is synchronously accelerated, the inner and outer structural compactness of the chain dendritic aggregate formed by the particle does not have inner and outer differences, so that the CTAB (specific surface area) of the product is close to the BET (specific surface area);
(2) By adopting the method, the reaction kettle can fully, softly and uniformly mix and react the reacted materials, and the consistency of the internal and external structures of the silicon dioxide reaction product aggregate is improved, so that the dispersibility, the reinforcing property and the comprehensive performance of the silicon dioxide in the green tire are improved, and the physicochemical property of the silicon dioxide is ensured to meet the index requirement.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method for producing silica for green tires, comprising the steps of:
(1) Raw material preparation: preparing dilute sodium silicate with the density of 1.180-1.280kg/L from liquid sodium silicate with the modulus of M=3.4-3.6 for later use;
(2) Mixing the raw materials: adding 12.5-16.5m into the reactor 3 The diluted sodium silicate is used as base solution, a dispersant feeding pump is started to add 10000-13000kg of dispersant into the reactor, and the dispersant is Na 2 SO 4 And soluble silica SiO 2 ·nH 2 O, the mixing ratio of which is 100 (1-2) and Na 2 SO 4 The mass percentage concentration of (2) is 4-6%, soluble silicon dioxide SiO 2 ·nH 2 The mass percentage concentration of O is 0.04-0.12%;
(3) Primary temperature rise: starting a reactor stirring device, controlling the stirring rotating speed at 75rpm, and simultaneously starting a reactor heating steam valve to introduce steam into the reactor, wherein the steam pressure is more than or equal to 6.0kg until the temperature of the bottom solution in the reactor is raised to 70+/-1 ℃;
(4) Seed crystal preparation: density of 1000-1010Kg/m 3 Adding dilute sulfuric acid with the addition amount of 1300-1800Kg into a reactor, and controlling the acid adding flow to be 2000-2300Kg/h; detecting the pH value in real time, stopping adding acid when the pH value of the feed liquid in the reactor reaches 7-8, and finishing the preparation of the seed crystal;
(5) And (3) secondary temperature rise: starting steam to continuously heat, and heating the feed liquid in the reactor from 70+/-1 ℃ to 86-96 ℃ at a speed of 3-5 ℃ per minute within 10-20 min;
(6) And (3) synthesis reaction: the synthesis reaction is carried out simultaneously in the whole secondary temperature rising process, namely dilute sulfuric acid and dilute sodium silicate are added into a reactor simultaneously, the total amount of the added dilute sodium silicate is controlled to be 3000-4000kg, and the pH value is strictly controlled to be stabilized to be 7-8 in the reaction process;
(7) Acidifying the slurry: stopping adding dilute sodium silicate after the pH value is stabilized at 7-8, continuously dropwise adding dilute sulfuric acid, controlling the acid adding time at 5-10min, controlling the total acid adding amount at 0.7-1.2L, and controlling the pH value at the acid adding end point at 4-6;
(8) Structural shaping: stopping adding acid when the pH value of the acid adding end point reaches 4-6, continuously stirring for 3-5min, and ending the reaction;
(9) Discharging materials: opening an electric control discharge valve of the reactor, discharging materials in the reactor into a storage tank, and cleaning the inner wall of the reactor through a cleaning device;
(10) The materials in the storage tank are filtered and washed by a filter press and then sent to a pulping system for pulping treatment, sodium metaaluminate is added as a pulping auxiliary agent in the pulping process, the addition amount of the pulping auxiliary agent is 4-6% of the total amount of the pulp, and then dilute sulfuric acid is added to adjust the PH to 6.0+/-0.1, so that the materials can be sent to the next working procedure for drying, and the product is obtained.
Comparative example 1
(1) Raw material preparation: preparing dilute sodium silicate with the density of 1.180-1.280kg/L from liquid sodium silicate with the modulus of M=3.4-3.6 for later use;
(2) Mixing the raw materials: adding 12.5-16.5m into the reactor 3 The diluted sodium silicate is used as base solution, a dispersant feeding pump is started to add 10000-13000kg of dispersant into the reactor, and the dispersant is Na 2 SO 4 And soluble silica SiO 2 ·nH 2 O, the mixing ratio of which is 100 (1-2) and Na 2 SO 4 The mass percentage concentration of (2) is 4-6%, soluble silicon dioxide SiO 2 ·nH 2 The mass percentage concentration of O is 0.04-0.12%;
(3) Primary temperature rise: starting a reactor stirring device, controlling the stirring rotating speed at 65rpm, and simultaneously starting a reactor heating steam valve to introduce steam into the reactor, wherein the steam pressure is more than or equal to 6.0kg until the temperature of the bottom solution in the reactor is raised to 65+/-1 ℃;
(4) Seed crystal preparation: adding dilute sulfuric acid with a certain concentration into a reactor, wherein the adding amount is 1300-1800Kg, and the acid adding flow is controlled to be 2000-2300Kg/h; detecting the pH value in real time, stopping adding acid when the pH value of the feed liquid in the reactor reaches 7-8, and finishing the preparation of the seed crystal;
(5) And (3) secondary temperature rise: starting steam to continuously heat, and directly heating the feed liquid in the reactor from 65+/-1 ℃ to 86-96 ℃ within 5-6 min;
(6) And (3) synthesis reaction: when the temperature of the feed liquid in the reactor reaches 86-96 ℃, starting the reaction, namely adding dilute sulfuric acid and dilute sodium silicate into the reactor, controlling the total amount of the added dilute sodium silicate to be 3000-4000kg, and strictly controlling the pH value to be stable to 7-8 in the reaction process;
(7) Acidifying the slurry: stopping adding dilute sodium silicate after the pH value is stabilized at 7-8, continuously dropwise adding dilute sulfuric acid, controlling the acid adding time at 5-10min, controlling the total acid adding amount at 0.7-1.2L, and controlling the pH value at the acid adding end point at 4-6;
(8) Structural shaping: stopping adding acid when the pH value of the acid adding end point reaches 4-6, continuously stirring for 3-5min, and ending the reaction;
(9) Discharging materials: opening an electric control discharge valve of the reactor, discharging materials in the reactor into a storage tank, and cleaning the inner wall of the reactor through a cleaning device;
(10) The materials in the storage tank are filtered and washed by a filter press and then sent to a pulping system for pulping treatment, sodium metaaluminate is added as a pulping auxiliary agent in the pulping process, the addition amount of the pulping auxiliary agent is 4-6% of the total amount of the pulp, and then dilute sulfuric acid is added to adjust the PH to 6.0+/-0.1, so that the products can be dried in the next working procedure.
The main differences between example 1 and comparative example 1 are as follows:
(1) the stirring speed of example 1 was controlled at 75rpm, and the stirring speed of comparative example 1 was controlled at 65rpm;
(2) the temperature of the reaction base solution in the example 1 is 7071 ℃ and the temperature of the reaction base solution in the comparative example 1 is 65+/-1 ℃;
(3) example 1 the synthesis reaction was carried out simultaneously throughout the entire elevated temperature of the synthesis reaction stage, and the synthesis reaction of comparative example 1 was initiated when the feed temperature in the reactor had increased to 86-96 c.
Comparative example 2
(1) Raw material preparation: preparing dilute sodium silicate with the density of 1.180-1.280kg/L from liquid sodium silicate with the modulus of M=3.4-3.6 for later use;
(2) Mixing the raw materials: adding diluted sodium silicate with a particle size of 12.5-16.5m into the reactor as base solution, starting a dispersing agent feeding pump, adding 10000-13000kg of dispersing agent which is Na into the reactor 2 SO 4 And soluble silica SiO 2 ·nH 2 O, the mixing ratio of which is 100 (1-2) and Na 2 SO 4 The mass percentage concentration of (2) is 4-6%, soluble silicon dioxide SiO 2 ·nH 2 The mass percentage concentration of O is 0.04-0.12%;
(3) Primary temperature rise: starting a reactor stirring device, controlling the stirring rotating speed at 75rpm, and simultaneously starting a reactor heating steam valve to introduce steam into the reactor, wherein the steam pressure is more than or equal to 6.0kg until the temperature of the bottom solution in the reactor is raised to 70+/-1 ℃;
(4) Seed crystal preparation: adding dilute sulfuric acid with a certain concentration into a reactor, wherein the adding amount is 1300-1800Kg, and the acid adding flow is controlled to be 2000-2300Kg/h; detecting the pH value in real time, stopping adding acid when the pH value of the feed liquid in the reactor reaches 7-8, and finishing the preparation of the seed crystal;
(5) And (3) secondary temperature rise: starting steam to continuously heat, and raising the temperature of the feed liquid in the reactor from 70+/-1 ℃ to 86-96 ℃ within 5-6 min;
(6) And (3) synthesis reaction: when the temperature of the feed liquid in the reactor reaches 86-96 ℃, starting the reaction, namely adding dilute sulfuric acid and dilute sodium silicate into the reactor, controlling the total amount of the added dilute sodium silicate to be 3000-4000kg, and strictly controlling the pH value to be stable to 7-8 in the reaction process;
(7) Acidifying the slurry: stopping adding dilute sodium silicate after the pH value is stabilized at 7-8, continuing adding dilute sulfuric acid, controlling the acid adding time at 5-10min, controlling the total acid adding amount at 0.7-1.2L, and controlling the pH value at the acid adding end point at 4-6;
(8) Structural shaping: stopping adding acid when the pH value of the acid adding end point reaches 4-6, continuously stirring for 3-5min, and ending the reaction;
(9) Discharging materials: opening an electric control discharge valve of the reactor, discharging materials in the reactor into a storage tank, and cleaning the inner wall of the reactor through a cleaning device.
(10) The materials in the storage tank are filtered and washed by a filter press and then sent to a pulping system for pulping treatment, sodium metaaluminate is added as a pulping auxiliary agent in the pulping process, the addition amount of the pulping auxiliary agent is 4-6% of the total amount of the pulp, and then dilute sulfuric acid is added to adjust the PH to 6.0+/-0.1, so that the products can be dried in the next working procedure.
The main difference between example 1 and comparative example 2 is that:
(1) example 1 the entire temperature rise from 70 + 1 c to 86-96 c during the synthesis reaction stage was carried out simultaneously with the synthesis reaction, and the synthesis reaction of comparative example 2 was started after the feed temperature in the reactor had risen to 86-96 c.
The invention detects various performance indexes of the silicon dioxide prepared by the methods of the embodiment 1 and the comparative example-2, wherein the detection method is based on HG/T3061-2009 and GB/T23656-2009; see table 1 for test results:
remarks: description of typical index CTAB and BET meaning in Table 1 (1) CTAB is the "reinforcing specific surface area", which is the sum of the outer surface area that can be brought into contact with rubber and the large pore area into which rubber molecules can permeate, and the height of this index characterizes the reinforcing ability of precipitated silica, and is also called "useful specific surface area"; (2) the BET specific surface area characterizes the physical specific surface area of precipitated silica, including the sum of the outer surface area that can be contacted with rubber and the inner surface area of the large pores and the inner surface area of the small pores that cannot be contacted with rubber; (3) CTAB-BET meaning: since the rubber polymer cannot penetrate into pores or micropores, the surface of the pores cannot be bonded to the rubber, and is a useless surface area, so that a smaller BET-CTAB indicates a larger "useful specific surface area", a smaller number of micropores, and better dispersibility in the tire rubber, and if bet=ctab indicates that the silica particle aggregate is all macropores, the dispersibility is the best.
From the results of the performance test in Table 1, it can be seen that BET-CTAB.ltoreq.5 in example 1, BET-CTAB.apprxeq.30 in comparative example 1, and BET-CTAB.apprxeq.10 in comparative example 2, and therefore the product dispersibility, reinforcement property, etc. in example 1 are superior in combination to those in comparative examples 1 and 2.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the solution disclosed in the embodiments, since it corresponds to the method disclosed in the embodiments, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for producing silica for green tires, comprising the steps of:
s1, adding a dispersing agent containing soluble silicon dioxide into a base solution of a reactor;
s2, stirring is started, the stirring speed is 75rpm, and meanwhile, the temperature of the reaction solution is raised to 70+/-1 ℃ for seed crystal preparation;
s3, raising the temperature from 70+/-1 ℃ to 86-96 ℃ at a speed of 3-5 ℃/min after the seed crystal preparation is finished, and simultaneously adding dilute sulfuric acid and dilute sodium silicate into a reactor for synthesis reaction to obtain slurry, wherein the whole temperature raising process and the synthesis reaction are carried out simultaneously;
s4, continuously adding dilute sulfuric acid to acidify the slurry;
s5, filtering, washing and preparing a filter cake from the acidified slurry, conveying the filter cake into a pulping system, adding a pulping auxiliary agent in the pulping process, adding dilute sulfuric acid to adjust the PH, and drying after pulping.
2. The method for producing silica for green tire according to claim 1, wherein the base liquid is prepared from a diluted sodium silicate having a modulus m=3.4 to 3.6 in water, and the density of the diluted sodium silicate is 1.180 to 1.280kg/L.
3. The method for producing silica for green tire according to claim 1, wherein the dispersant in step S1 is Na in a volume ratio of 100 (1-2) 2 SO 4 And soluble silica SiO 2 ·nH 2 Mixed solution of O and Na 2 SO 4 The mass percentage concentration of (2) is 4-6%, soluble silicon dioxide SiO 2 ·nH 2 The mass percentage concentration of O is 0.04-0.12%.
4. A method for producing silica for green tires as claimed in any one of claims 1 to 3, wherein the dispersant is added in an amount of 30 to 50% by mass of the total mass of the base liquid in step S1.
5. The method for producing silica for green tire according to claim 1, wherein the seed preparation in step S2 comprises: dilute sulfuric acid is added into the reactor until the pH value is 7-8, and the seed crystal preparation is completed.
6. The method for producing silica for green tire according to claim 5, wherein the addition rate of dilute sulfuric acid in the seed crystal production process is 2000-2300Kg/h, and the density of dilute sulfuric acid is 1000-1010Kg/m 3 。
7. The method for producing silica for green tire according to claim 1, wherein the pH value of the synthesis reaction is controlled to 7 to 8.
8. The method for producing silica for green tire according to claim 1, wherein dilute sulfuric acid is added to a pH of 4 to 6 in step S4, and the acid addition time is controlled to be 5 to 10min.
9. The method according to claim 1, wherein in the step S5, the beating aid is sodium metaaluminate, and the addition amount of the beating aid is 4-6% of the total amount of the slurry, and dilute sulfuric acid is added to adjust the pH to 6.0±0.1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210874423.0A CN115340101B (en) | 2022-07-22 | 2022-07-22 | Production method of silicon dioxide for green tire |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210874423.0A CN115340101B (en) | 2022-07-22 | 2022-07-22 | Production method of silicon dioxide for green tire |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115340101A CN115340101A (en) | 2022-11-15 |
| CN115340101B true CN115340101B (en) | 2023-09-26 |
Family
ID=83949221
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210874423.0A Active CN115340101B (en) | 2022-07-22 | 2022-07-22 | Production method of silicon dioxide for green tire |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115340101B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019038728A (en) * | 2017-08-28 | 2019-03-14 | 味の素株式会社 | Method for producing precipitated silica |
| CN110255572A (en) * | 2019-07-26 | 2019-09-20 | 江西黑猫炭黑股份有限公司 | Utilize the method for the by-product production precipitated silica in fumed silica production process |
| 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060182681A1 (en) * | 2004-12-28 | 2006-08-17 | Fortum Oyj | Catalytic materials and method for the preparation thereof |
| JP5137521B2 (en) * | 2006-10-12 | 2013-02-06 | 日揮触媒化成株式会社 | Konpira sugar-like sol and process for producing the same |
-
2022
- 2022-07-22 CN CN202210874423.0A patent/CN115340101B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019038728A (en) * | 2017-08-28 | 2019-03-14 | 味の素株式会社 | Method for producing precipitated silica |
| CN110255572A (en) * | 2019-07-26 | 2019-09-20 | 江西黑猫炭黑股份有限公司 | Utilize the method for the by-product production precipitated silica in fumed silica production process |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115340101A (en) | 2022-11-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109705402B (en) | Preparation method of aerogel film opening agent | |
| CN101774623B (en) | Industrial preparation method of rice-shaped ultra-fine activated calcium carbonate | |
| CN111017932B (en) | Large-aperture white carbon black and preparation method and application thereof | |
| US20090169456A1 (en) | Apparatus for Manufacturing Nanoporous Silica Method Thereof | |
| CN107055557B (en) | Preparation method of white carbon black with adjustable CTAB specific surface area | |
| WO2020034745A1 (en) | High-adsorption and high-dispersion silicon dioxide and preparation method therefor | |
| CN105236429A (en) | Ultrahighly-dispersed white carbon black preparation method | |
| WO2010078821A1 (en) | Method for preparing subsphaeroidal barium sulfate by sulfuric acid process and its use in copper foil substrate | |
| CN111393172B (en) | Inorganic green body reinforcing agent based on silicate system | |
| CN111547730B (en) | Preparation method of ultrafine precipitated silica anticaking agent for powder coating | |
| CN1128199C (en) | Preparation process of magnesium hydroxide fire-retarding nanomaterial | |
| CN112811456A (en) | Nano calcium carbonate with high specific surface area and preparation method thereof | |
| CN108033453A (en) | A kind of preparation method of modified precipitated silica | |
| CN115340101B (en) | Production method of silicon dioxide for green tire | |
| CN110562991A (en) | Production method of white carbon black for high-oil-absorption carrier | |
| CN112626915A (en) | Preparation method and application of high-whiteness paper surface sizing agent | |
| CN110835110A (en) | Preparation method of precipitated hydrated silicon dioxide | |
| CN111573683B (en) | Preparation method of silica with high specific surface area and low oil absorption value and product thereof | |
| CN109337290A (en) | A kind of preparation method of conducting ceramic fibers paper | |
| CN110643206A (en) | Production method of high-dispersion white carbon black | |
| CN107324350A (en) | A kind of method for preparing nanoprecipitation silica using low-grade diatomite | |
| CN116002743B (en) | Hollow tubular nano barium sulfate and preparation method and application thereof | |
| CN113830773A (en) | Preparation method of white carbon black by large pore volume precipitation method | |
| CN111017939A (en) | Preparation method of high-dispersion silicon dioxide | |
| CN111137901A (en) | Preparation method of high-performance silicon dioxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |