High-efficiency short-process production method and production system for carbonization-process white carbon black

Abstract

The invention discloses a high-efficiency short-process production method and production system for carbonization-process white carbon black, an absorption reaction is completed in a normal-pressure gas-liquid small-sized carbonization reaction kettle, and rapid continuous reaction of CO2 gas and liquid sodium silicate in the carbonization reaction kettle is realized through high-strength stirring and gas-liquid interface contact enhanced absorption; and high-efficiency absorption of carbon dioxide is realized under normal-pressure reaction conditions. The carbonization reaction is carried out in a small-sized carbonization reaction kettle, the precipitation reaction can be carried out in a large-sized precipitation reaction kettle according to the scale, the solid-liquid reaction is carried out in the precipitation reaction kettle, and the silicon dioxide micro particles generated by the absorption reaction are subjected to uniform mixing by controlling the reaction time, the reaction temperature and the reaction pH value. The particles are further aggregated and grown to form the silicon dioxide particles with stable structure and reliable performance, the structure is stable, the performance is reliable, and the utilization efficiency of raw materials is improved.

Description

Technical Field

[0001] The invention relates to the field of white carbon black production, and in particular to a high-efficiency short-process production method and a production system for white carbon black produced by a carbonization process. Background Art

[0002] White carbon black is a general name for amorphous silicic acid and silicate products. It is called white carbon black because of its reinforcing effect in the rubber industry, which is similar to carbon black. It has a molecular formula of SiO2·nH2O and a white appearance. It is an amorphous silicon dioxide. White carbon black is mainly divided into fumed white carbon black and precipitated white carbon black. Precipitated white carbon black is mainly obtained by synthesis reaction of sodium silicate and sulfuric acid. With the improvement of environmental protection requirements and the concern about carbon dioxide emission reduction, the continuous upgrading and improvement of carbon dioxide acidification technology has made carbon dioxide replace sulfuric acid as a new acidifier, which not only helps to reduce environmental pollution, but also achieve the goal of carbon emission reduction. The use of carbon dioxide acidification technology not only meets the current global requirements for environmental protection and sustainable development, but also helps to promote technological progress and environmental protection upgrades in the white carbon black production industry. In this way, carbon dioxide can be recycled and utilized with high added value, reducing carbon dioxide emissions and reducing the carbon footprint of white carbon black products, while also producing white carbon black products that meet environmental standards.

[0003] The application number CN202010384373.9 is a kind of nano-silicon dioxide for rubber reinforcement and its preparation method, and the application number CN201910318339.9 is a method for preparing spherical silicon dioxide. The carbonization synthesis reaction is carried out by a membrane dispersion reaction tower or a microreactor to increase the reaction efficiency of CO2, and the production equipment is relatively complex. The application number CN202311127112.9 is a method for preparing highly dispersed white carbon black by pressurized carbonization of multiple kettles in series, and the application number CN202310969463.8 is a method for preparing precipitated white carbon black by coupling carbonization of sodium silicate. The carbon dioxide absorption reaction of multiple kettles in series is pressurized to prepare white carbon black, and the production equipment and control process are relatively complex. Summary of the invention

[0004] In view of this, the object of the present invention is to provide a highly efficient short-process production method and production system for carbonization-processed silica.

[0005] In order to achieve the above technical objectives, the technical solution adopted by the present invention is:

[0006] In a first aspect, the present invention provides an efficient short-process production system for carbonization-process white carbon black, comprising a carbonization component, a precipitation component, a cooling component, a filtering component and a drying component; the carbonization component comprises a carbonization reactor, a first feed pipe, a second feed pipe, a third feed pipe and a first discharge pipe, the first feed pipe, the second feed pipe, the third feed pipe and the first discharge pipe are all connected to the carbonization reactor, the first discharge pipe, the second feed pipe and the third feed pipe are respectively connected to the bottom of the carbonization reactor, the first feed pipe is used to introduce liquid sodium silicate, the second feed pipe is used to introduce steam, the third feed pipe is used to introduce carbon dioxide gas, the carbonization reactor is filled with an aqueous solution, liquid silicon Sodium hydroxide and carbon dioxide form a first slurry in an aqueous solution, and a first discharge pipe is used to output the first slurry; the precipitation component includes a precipitation reactor, a fourth feed pipe, a second discharge pipe and a third discharge pipe, the precipitation reactor is filled with an aqueous solution, the first discharge pipe is connected to the top of the precipitation reactor, the fourth feed pipe, the second discharge pipe and the third discharge pipe are respectively connected to the bottom of the precipitation reactor, the fourth feed pipe is used to pass steam, and the other end of the second discharge pipe is also connected to the carbonization reactor. The first slurry forms a second slurry in the precipitation reactor, the second discharge pipe is used to repeatedly pass the second slurry into the carbonization reactor, and the third discharge pipe is used to output the second slurry after the precipitation process is completed;

[0007] The cooling component includes a cooling reactor, a fifth feed pipe, a fourth discharge pipe and a fifth discharge pipe. The fifth discharge pipe and the fourth discharge pipe are both arranged at the bottom of the cooling reactor. The third discharge pipe is connected to the cooling reactor. The fifth feed pipe is used to introduce circulating cooling water. The fifth discharge pipe is used to output the circulating cooling water in the cooling reactor. After the second slurry is cooled in the cooling reactor, a third slurry is formed. The fourth discharge pipe is used to output the third slurry. The filtering component includes a plate and frame filter, a sixth feed pipe and a belt conveyor. The plate and frame filter is connected to the fourth discharge pipe. The sixth feed pipe is connected to the plate and frame filter. The sixth feed pipe is used to introduce hot water. The belt conveyor is arranged at the output end of the plate and frame filter. The third slurry is repeatedly washed and filtered by hot water in the plate and frame filter to form a filter cake. The belt conveyor is used to receive the filtered filter cake. The drying component includes a stirring and mixing tank, a stirring transition tank and a drying tower. The stirring and mixing tank is connected to the output end of the belt conveyor, the output end of the stirring and mixing tank is connected to the stirring transition tank, the drying tower is connected to the output end of the stirring transition tank, the stirring and mixing tank is used to stir and mix the filter cake with the aqueous solution to form a fourth slurry, the stirring transition tank is used to transport the fourth slurry to the drying tower, and the drying tower dries the fourth slurry to form a white carbon black product.

[0008] In some embodiments, the carbonization assembly further includes a first connecting tube, one end of which is connected to the top of the carbonization reactor, and the other end of the first connecting tube is connected to the precipitation reactor, and the connecting end of the first connecting tube and the precipitation reactor is 10 to 30 mm lower than the liquid level of the precipitation reactor.

[0009] In some embodiments, the precipitation component also includes a second connecting pipe, which is connected to the top of the precipitation reactor and is also connected to the spray tower; the cooling component also includes a third connecting pipe, which is connected to the top of the cooling reactor and is also connected to the spray tower.

[0010] In some embodiments, a first agitator, a first thermometer, a first material level meter, and a first pH meter are provided in the carbonization reactor, a first flow meter is provided on the first feed pipe, a second flow meter is provided on the second feed pipe, and a third flow meter is provided on the third feed pipe; and / or, a second agitator, a second thermometer, a second material level meter, and a second pH meter are provided in the precipitation reactor, and a fourth flow meter is provided on the fourth feed pipe; and / or, a third agitator, a third thermometer, a third material level meter, and a third pH meter are provided in the precipitation reactor, and a fifth flow meter is provided on the fifth feed pipe; and / or, a fourth agitator, a third thermometer, a third material level meter, and a third pH meter are provided in the precipitation reactor, and a fifth flow meter is provided on the fifth feed pipe; and / or, a fourth agitator, a third thermometer, a third material level meter, and a third pH meter are provided in the stirring and slurry mixing tank. an agitator, a fourth thermometer, a fourth material level meter, a fourth pH meter; and / or, a fifth agitator, a fifth thermometer, a fifth material level meter, and a fifth pH meter are provided in the stirring transition tank; and / or, a sixth flowmeter is provided on the first discharge pipe, a seventh flowmeter and a first delivery pump are provided on the second discharge pipe, an eighth flowmeter and a second delivery pump are provided on the third discharge pipe, a ninth flowmeter and a third delivery pump are provided on the fourth discharge pipe, a tenth flowmeter is provided on the fifth discharge pipe, a fourth delivery pump is provided at the connection between the stirring slurry mixing tank and the stirring transition tank, and a fifth delivery pump is provided at the connection between the stirring transition tank and the drying tower.

[0011] In some embodiments, the ratio of the height to the diameter of the carbonization reactor is not less than 3.

[0012] In some embodiments, the first agitator and / or the second agitator and / or the third agitator and / or the fourth agitator and / or the fifth agitator are self-priming stainless steel high-speed agitators.

[0013] In a second aspect, the present invention further provides a highly efficient short-process production method of carbonization-processed white carbon black, which is applicable to the production system described in the first aspect, and the method comprises:

[0014] Liquid sodium silicate is continuously added into the carbonization reactor, and carbon dioxide is continuously added from the bottom of the carbonization reactor, and steam is introduced into the carbonization reactor to maintain the temperature of the carbonization reactor, wherein the mass concentration of the liquid sodium silicate is 15-30% and the modulus is 3.3-3.5;

[0015] Liquid sodium silicate reacts with carbon dioxide and aqueous solution to obtain a first slurry;

[0016] The first slurry is transported to a precipitation reactor, and steam is added to the precipitation reactor to maintain the temperature of the precipitation reactor, and the first slurry in the precipitation reactor is repeatedly pumped to the carbonization reactor to maintain the liquid levels of the carbonization reactor and the precipitation reactor;

[0017] The first slurry precipitates a carbonized product in a precipitation reactor to form a second slurry;

[0018] The second slurry is transported to a cooling reactor, and circulating cooling water is added to the cooling reactor, and the second slurry is cooled to form a third slurry;

[0019] The third slurry is transported to a plate-and-frame filter, and hot water is introduced into the plate-and-frame filter to wash the third slurry to form a filter cake;

[0020] The filter cake is unloaded onto a belt conveyor and conveyed by the belt conveyor into a mixing and slurry mixing tank, where the filter cake is mixed with an aqueous solution to form a white carbon black slurry;

[0021] The white carbon black slurry is transported to a drying tower via a stirring transition tank, and the drying tower dries the white carbon black slurry to obtain a white carbon black product.

[0022] In some embodiments, the stirring frequency of the carbonization reactor is not less than 100 r / min, the temperature of the first slurry in the carbonization reactor is 70-95° C., the pH value of the first slurry is 9-12, and the residence time of the first slurry in the carbonization reactor is 3-10 min.

[0023] In some embodiments, the temperature of the second slurry in the precipitation reactor is 70-95°C, the pH value of the second slurry is 9.5-11, the residence time of the second slurry in the precipitation reactor is 60-180min, the pH value of the second slurry when entering the next process is 8.5-9.5, and the dissolved silicon content of the second slurry is less than 100PPm.

[0024] In some embodiments, the temperature of the third slurry in the cooling reactor is not higher than 85°C.

[0025] By adopting the above technical solution, the present invention has the following beneficial effects compared with the prior art:

[0026] (1) The absorption reaction of the present invention is completed in a small gas-liquid carbonization reactor at normal pressure. The absorption is enhanced by high-intensity stirring and gas-liquid interface contact, so that the CO2 gas and liquid sodium silicate react rapidly and continuously in the carbonization reactor, and the efficient absorption of carbon dioxide is achieved under normal pressure reaction conditions. The carbonization reaction is carried out in a small absorption reactor, and the precipitation reaction can be carried out in a large precipitation reactor according to the scale. The solid-liquid reaction is carried out in the precipitation reactor, and the silicon dioxide microparticles generated by the absorption reaction are further aggregated and grown to form silicon dioxide particles with stable structure and reliable performance by controlling the reaction time, reaction temperature and reaction pH. Then, the absorption reaction is continued by reflux, and the pH value of the solution is further reduced, and the content of dissolved silicon dioxide precipitation in the solution is reduced to absorb carbon dioxide, so that the particle structure is stable and the performance is reliable, thereby improving the utilization efficiency of raw materials.

[0027] The carbon dioxide carbonization process for producing white carbon black of the present invention decomposes the synthesis reaction into two reaction processes, namely, a carbonization reaction and a precipitation reaction. The production can be continuous, and the problems that a relatively high pressure and temperature are required when a traditional integrated synthesis reactor is scaled up, or a multi-stage series forced gas-liquid reaction is required to improve the carbon dioxide absorption rate, the production lacks continuity, and the traditional gas-liquid contact is insufficient, resulting in a low carbon dioxide absorption rate in the reaction process.

[0028] (2) The present invention can simultaneously and continuously add liquid sodium silicate and CO2 into the carbonization reactor to carry out carbonization reaction of carbon dioxide, and continuously carry out precipitation reaction and cooling reaction. At the same time, the carbonization reactor is equipped with a slurry circulation to initiate a carbonization chain reaction of CO2, which can achieve efficient carbonization conversion of carbon dioxide and increase the carbonization reaction rate of CO2. Then, the carbon dioxide enters the precipitation reactor to continue the reaction. At the same time, when entering the cooling reactor, the silicon dioxide continues to condense and grow at variable temperature.

[0029] (3) Liquid sodium silicate with high mass concentration can be used as raw material, and the mass concentration of liquid sodium silicate reaches 20-30%, thereby improving the reaction efficiency and yield per unit volume during the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0031] Figure 1 This is a schematic diagram of the efficient short-process production system of carbonization-based silica;

[0032] Figure 2 It is a highly efficient and short-process production flow chart of carbonization-based silica.

[0033] Reference numerals:

[0034] 101, carbonization reactor; 102, first feed pipe; 103, second feed pipe; 104, third feed pipe; 105, first discharge pipe; 106, first connecting pipe; 107, first flow meter; 108, second flow meter; 109, third flow meter; 110, sixth flow meter;

[0035] 201, precipitation reaction kettle; 202, fourth feed pipe; 203, second discharge pipe; 204, third discharge pipe; 205, second connecting pipe; 206, fourth flow meter; 207, seventh flow meter; 208, eighth flow meter; 209, first delivery pump; 210, second delivery pump;

[0036] 301, cooling reactor; 302, fourth discharge pipe; 303, fifth feed pipe; 304, fifth discharge pipe; 305, third connecting pipe; 306, fifth flow meter; 307, ninth flow meter; 308, tenth flow meter; 309, third delivery pump;

[0037] 401, plate and frame filter; 402, belt conveyor; 403, sixth feed pipe;

[0038] 501, stirring and mixing tank; 502, stirring transition tank; 503, drying tower; 504, fourth delivery pump; 505, fifth delivery pump. DETAILED DESCRIPTION

[0039] The present invention will be further described in detail below in conjunction with the accompanying drawings and examples. It is particularly noted that the following examples are only used to illustrate the present invention, but are not intended to limit the scope of the present invention. Similarly, the following examples are only partial embodiments of the present invention rather than all embodiments, and all other embodiments obtained by those of ordinary skill in the art without creative work are within the scope of protection of the present invention.

[0040] See also Figure 1 and Figure 2In the first aspect, the present embodiment provides an efficient short-process production system for carbonization-process white carbon black, including a carbonization component, a precipitation component, a cooling component, a filtering component and a drying component; the carbonization component includes a carbonization reactor 101, a first feed pipe 102, a second feed pipe 103, a third feed pipe 104 and a first discharge pipe 105, the first feed pipe 102, the second feed pipe 103, the third feed pipe 104 and the first discharge pipe 105 are all connected to the carbonization reactor 101, the first discharge pipe 105, the second feed pipe 103 and the third feed pipe 104 are respectively connected to the bottom of the carbonization reactor 101, the first feed pipe 102 is used to introduce liquid sodium silicate, the second feed pipe 103 is used to introduce steam, and the third feed pipe 104 is used to introduce carbon dioxide gas. The carbonization reactor 101 is filled with an aqueous solution, liquid silicate Sodium and carbon dioxide form a first slurry in an aqueous solution, and a first discharge pipe 105 is used to output the first slurry; the precipitation assembly includes a precipitation reactor 201, a fourth feed pipe 202, a second discharge pipe 203 and a third discharge pipe 204, the precipitation reactor 201 is filled with an aqueous solution, the first discharge pipe 105 is connected to the top of the precipitation reactor 201, the fourth feed pipe 202, the second discharge pipe 203 and the third discharge pipe 204 are respectively connected to the bottom of the precipitation reactor 201, the fourth feed pipe 202 is used to pass steam, and the other end of the second discharge pipe 203 is also connected to the carbonization reactor 101, the first slurry forms a second slurry in the precipitation reactor 201, the second discharge pipe 203 is used to repeatedly pass the second slurry into the carbonization reactor 101, and the third discharge pipe 204 is used to output the second slurry after the precipitation process is completed;

[0041] The cooling component includes a cooling reactor 301, a fifth feed pipe 303, a fourth discharge pipe 302 and a fifth discharge pipe 304. The fifth discharge pipe 304 and the fourth discharge pipe 302 are both arranged at the bottom of the cooling reactor 301. The third discharge pipe 204 is connected to the cooling reactor 301. The fifth feed pipe 303 is used to introduce circulating cooling water. The fifth discharge pipe 304 is used to output the circulating cooling water in the cooling reactor 301. The second slurry is cooled in the cooling reactor 301 to form a third slurry. The fourth discharge pipe 302 is used to output the third slurry. The filtering component includes a plate and frame filter 401, a sixth feed pipe 403 and a belt conveyor 402. The plate and frame filter 401 is connected to the fourth discharge pipe 302, the sixth feed pipe 403 is connected to the plate and frame filter 401, and the sixth feed pipe 404 is connected to the plate and frame filter 401. 03 is used to introduce hot water, and the belt conveyor 402 is arranged at the output end of the plate and frame filter 401. The third slurry is repeatedly washed and filtered with hot water in the plate and frame filter 401 to form a filter cake, and the belt conveyor 402 is used to receive the filtered filter cake; the drying component includes a stirring and slurry mixing tank 501, a stirring transition tank 502 and a drying tower 503. The stirring and slurry mixing tank 501 is connected to the output end of the belt conveyor 402, the output end of the stirring and slurry mixing tank 501 is connected to the stirring transition tank 502, and the drying tower 503 is connected to the output end of the stirring transition tank 502. The stirring and slurry mixing tank 501 is used to stir and slurry the filter cake with the aqueous solution to form a fourth slurry, and the stirring transition tank 502 is used to transport the fourth slurry to the drying tower 503. The drying tower 503 dries the fourth slurry to obtain a white carbon black product.

[0042] It should be noted that this embodiment is adapted to the production process of carbonized white carbon black. The entire production process of white carbon black includes the steps of carbonization, precipitation, cooling, filtering and washing, slurry preparation and drying. The carbonization reaction is a chemical reaction between sodium silicate and carbon dioxide in an aqueous solution. Specifically, CO2 completes the carbonization reaction in the carbonization reactor 101. Due to the addition of sodium silicate, the carbonization reactor 101 is an alkaline environment as a whole. In this environment, carbon dioxide (CO2) reacts with water and continuously hydrolyzes to form carbonic acid (H2CO3). Carbonic acid is a weak acid, which further ionizes to form bicarbonate ions (HCO3 - ) and hydrogen ions (H + ), which can be further ionized to form carbonate ions (CO3 2- ) and two hydrogen ions (2H + ).

[0043] The chemical equation for the hydrolysis of carbon dioxide is as follows:

[0044]

[0045] Under alkaline conditions, carbonic acid further ionizes:

[0046]

[0047] In the absorption reaction, sodium silicate (Na2OTnSiO2) reacts with hydrogen ions ionized by carbonic acid to produce silicic acid, which is further precipitated to form white carbon black (SiO2) particles. The reaction equation is as follows:

[0048] Na2OTnSiO2+2nH + +2HCO3 - =2NaHCO3+nH2SiO3

[0049] Na2OTnSiO2+2nH + +CO3 2- =Na2CO3+nH2SiO3

[0050]

[0051] During the entire absorption and precipitation reaction, the carbonate and bicarbonate ions converted into ionic form of carbon dioxide will all participate in the absorption reaction, and the carbon dioxide that escapes and does not participate in the absorption reaction accounts for less than 10% of the total consumption, which means that the absorption reaction efficiency of carbon dioxide is not less than 90%.

[0052] The carbonized product (i.e., the slurry containing white carbon black) is subjected to a precipitation treatment to precipitate the white carbon black from the reaction solution. Afterwards, the precipitated slurry containing white carbon black is cooled to reach a suitable temperature. The cooled slurry containing white carbon black is passed through a filtering device to remove impurities and excess liquid therein. The filtered white carbon black product is then mixed with an appropriate amount of liquid (such as water, solvent, etc.) to form a white carbon black slurry, which does not contain impurities and other solid particles before filtration. This step is usually performed in a stirring and slurry mixing tank 501, and the purpose of stirring is to evenly disperse the white carbon black in the liquid. The white carbon black slurry is smoothly transported from the stirring and slurry mixing tank 501 to the next processing equipment, such as a filter, a dryer, etc., for drying to obtain the final white carbon black product.

[0053] Based on the above process flow, the production system shown in this embodiment includes a carbonization component, a precipitation component, a cooling component, a filtering component and a drying component. Among them, the carbonization component includes a carbonization reactor 101, and the carbonization reactor 101 can be a small carbonization reactor 101, and this embodiment does not limit this. The carbonization reactor 101 is filled with an aqueous solution, and the aqueous solution is pure water. While liquid sodium silicate is passed into the pure water, carbon dioxide and steam are passed into the pure water, wherein the steam is used to maintain the temperature in the aqueous solution of pure water, and carbon dioxide and liquid sodium silicate produce the chemical reaction shown above in the water, thereby forming a slurry containing white carbon black, which is recorded as the first slurry for ease of understanding.

[0054] Further, a precipitation reactor 201 is provided in the precipitation assembly, and the precipitation reactor 201 and the carbonization reactor 101 are two independent reactors, and an aqueous solution can be introduced into the precipitation reactor 201, and the aqueous solution is pure water, and the first slurry is introduced into the precipitation reactor 201 for precipitation. It should be noted that, in this embodiment, the precipitation reactor 201 is also provided with a second discharge pipe 203, and the second discharge pipe 203 can re-introduce the solution in the precipitation reactor 201 and the first slurry into the carbonization reactor 101. It can be understood that the use time of the second discharge pipe 203 and the third discharge pipe 204 can be adjusted in sequence to achieve different use effects. For example, when the first slurry is still in the reaction process, the second discharge pipe 203 and the first discharge pipe 105 can be opened to realize the liquid circulation between the precipitation reactor 201 and the carbonization reactor 101; after the precipitation is completed, the third discharge pipe 204 is opened, and the second discharge pipe 203 and the first discharge pipe 105 are closed to output the second slurry formed after the precipitation of the first slurry to the precipitation reactor 201; optionally, after the second slurry in the precipitation reactor 201 is output, the third discharge pipe 204 is closed and the second discharge pipe 203 is opened to re-introduce the solution of the residual first slurry that has not yet precipitated in the precipitation reactor 201 into the carbonization reactor 101 to realize the recycling of the liquid.

[0055] In this embodiment, the second slurry is introduced into the cooling reactor 301, and the temperature of the second slurry is reduced in the cooling reactor 301. It should be noted that the cooling reactor 301 realizes the replenishment and output of circulating cooling water through the fifth feeding pipe 303 and the fifth discharging pipe 304, so that the cooling reactor 301 maintains the required cooling temperature and uses water to maintain heat exchange with the second slurry. For the convenience of description, the cooled second slurry is recorded as the third slurry.

[0056] Furthermore, the present embodiment is provided with a plate-and-frame filter 401, and the third slurry is introduced into the plate-and-frame filter 401. Meanwhile, hot water is introduced into the sixth feed pipe 403, and the hot water can wash the third slurry to remove the residual liquid, ions, etc. in the third slurry, and finally obtain a white carbon black product. For the convenience of description, the white carbon black product is described as a filter cake. The filter cake is output from the output end of the plate-and-frame filter 401 to the belt conveyor 402, and is transported to the stirring and slurry mixing tank 501 by the belt conveyor 402. For example, the stirring and slurry mixing tank 501 can be equipped with pure water, and the filter cake is slurried with pure water, so that the white carbon black product is fully slurried in the water. The stirring transition tank 502 can be understood as a conveying tank body that maintains the stirring intensity, which can keep the white carbon black solution formed after the white carbon black product is slurried in water in a turbid state, and prevent the white carbon black product from precipitating in the tank body. Finally, the stirring transition tank 502 passes the white carbon black solution into the drying tower 503, and the drying tower 503 takes away the water molecules in the white carbon black solution, thereby obtaining a white carbon black product.

[0057] It should be noted that the precipitation reactor 201, carbonization reactor 101 and cooling reactor 301 described in this embodiment are all independent devices. Under this condition, the size and quantity of the precipitation reactor 201, carbonization reactor 101 and cooling reactor 301 can be adjusted according to actual needs, and the entire production system has greater flexibility in modification. At the same time, the absorption reaction of this embodiment is completed in the atmospheric pressure gas-liquid small carbonization reactor 101, and the absorption is enhanced by high-intensity stirring and gas-liquid interface contact, so as to realize the rapid and continuous reaction of CO2 gas and liquid sodium silicate in the carbonization reactor 101, and realize the efficient absorption of carbon dioxide under atmospheric pressure reaction conditions. The carbonization reaction is carried out in a small carbonization reactor 101, and the precipitation reaction can be carried out in a large precipitation reactor 201 according to the scale. A solid-liquid reaction is carried out in the precipitation reactor 201, and the silica particles generated by the absorption reaction are further aggregated and grown to form silica particles with stable structure and reliable performance by controlling the reaction time, reaction temperature, and reaction pH, and then refluxed to continue the absorption reaction, further reducing the pH value of the solution, reducing the content of dissolved silica precipitation in the solution, absorbing carbon dioxide, making the particle structure stable, reliable, and improving the utilization efficiency of raw materials. The carbon dioxide carbonization method white carbon black production process shown in this embodiment decomposes the synthesis reaction into two reaction processes, carbonization reaction and precipitation reaction, and the production can achieve continuity, which solves the problem that the traditional integrated synthesis reactor needs to be scaled up by relatively high pressure and temperature, or requires multi-stage series forced gas-liquid reaction to improve the carbon dioxide absorption rate, and the production lacks continuity, and the traditional gas-liquid contact is insufficient, and the carbon dioxide absorption rate in the reaction process is low. In this embodiment, liquid sodium silicate and CO2 can be added to the carbonization reactor 101 simultaneously and continuously to carry out carbonization reaction of carbon dioxide, and precipitation reaction and cooling reaction are continuously carried out. At the same time, the carbonization reactor 101 is equipped with a slurry circulation to trigger the carbonization chain reaction of CO2, which can achieve efficient carbonization conversion of carbon dioxide and increase the carbonization reaction speed of CO2. Then, it enters the precipitation reactor 201 to continue the reaction, and at the same time, silicon dioxide continues to condense and grow at variable temperature when entering the cooling reactor 301. Liquid sodium silicate with high mass concentration can be used as raw material, and the mass concentration of liquid sodium silicate reaches 20-30%, which improves the reaction efficiency and yield per unit volume during the reaction.

[0058] In some embodiments, the carbonization component also includes a first connecting tube 106, one end of the first connecting tube 106 is connected to the top of the carbonization reactor 101, and the other end of the first connecting tube 106 is connected to the precipitation reactor 201, and the connecting end of the first connecting tube 106 and the precipitation reactor 201 is 10 to 30 mm lower than the liquid level of the precipitation reactor 201.

[0059] The first connecting pipe 106 is connected to the upper part of the carbonization reactor 101 , and the connecting end of the first connecting pipe 106 and the precipitation reactor 201 is 10 to 30 mm lower than the liquid level in the precipitation reactor 201 to recover the remaining carbon dioxide gas. At the same time, the first connecting pipe 106 is also used to buffer the gas pressure in the precipitation reactor 201 .

[0060] In some embodiments, the precipitation component also includes a second connecting pipe 205, which is connected to the top of the precipitation reactor 201 and is also connected to the spray tower; the cooling component also includes a third connecting pipe 305, which is connected to the top of the cooling reactor 301 and is also connected to the spray tower.

[0061] The second connecting pipe 205 and the third connecting pipe 305 can recover the heat in the precipitation reactor 201 and the cooling reactor 301, and realize the gas pressure balance in the cooling reactor 301 and the precipitation reactor 201. It should be noted that the spray tower is a circulating spray tower, and the spray tower can be set according to actual needs. The spray tower of other equipment in the area where the entire production system is located can also be used to fully save the production cost and realize the diversified utilization of energy.

[0062] In some embodiments, the carbonization reactor 101 is provided with a first agitator, a first thermometer, a first material level meter, and a first pH meter, the first feed pipe 102 is provided with a first flowmeter 107, the second feed pipe 103 is provided with a second flowmeter 108, and the third feed pipe 104 is provided with a third flowmeter 109; and / or, the precipitation reactor 201 is provided with a second agitator, a second thermometer, a second material level meter, and a second pH meter, and the fourth feed pipe 202 is provided with a fourth flowmeter 206; and / or, the precipitation reactor 201 is provided with a third agitator, a third thermometer, a third material level meter, and a third pH meter, and the fifth feed pipe 303 is provided with a fifth flowmeter 306; and / or, the stirring and mixing tank 501 is provided with a fourth agitator, a fourth thermometer, a third material level meter, and a third pH meter. , a fourth material level meter, a fourth pH meter; and / or, a fifth agitator, a fifth thermometer, a fifth material level meter, and a fifth pH meter are provided in the stirring transition tank 502; and / or, a sixth flowmeter 110 is provided on the first discharge pipe 105, a seventh flowmeter 207 and a first delivery pump 209 are provided on the second discharge pipe 203, an eighth flowmeter 208 and a second delivery pump 210 are provided on the third discharge pipe 204, a ninth flowmeter 307 and a third delivery pump 309 are provided on the fourth discharge pipe 302, a tenth flowmeter 308 is provided on the fifth discharge pipe 304, a fourth delivery pump 504 is provided at the connection between the stirring and slurry mixing tank 501 and the stirring transition tank 502, and a fifth delivery pump 505 is provided at the connection between the stirring transition tank 502 and the drying tower 503.

[0063] In some embodiments, the ratio of the height to the diameter of the carbonization reactor 101 is not less than 3.

[0064] In some embodiments, the first agitator and / or the second agitator and / or the third agitator and / or the fourth agitator and / or the fifth agitator are self-priming stainless steel high-speed agitators.

[0065] By setting the first agitator, the second agitator, the third agitator, the fourth agitator and the fifth agitator, the production efficiency of the entire white carbon black can be improved. By equipping each device with a thermometer, a level meter and a pH meter, the temperature, level and pH of multiple devices can be monitored and adjusted. At the same time, flow meters are set on multiple pipelines to achieve accurate transportation and adjustment of various materials.

[0066] See also Figure 2 In the second aspect, this embodiment further provides a highly efficient short-process production method of carbonization-processed white carbon black, which is applicable to the production system described in the first aspect, and the method comprises:

[0067] Liquid sodium silicate is continuously added into the carbonization reactor, and carbon dioxide is continuously added from the bottom of the carbonization reactor, and steam is introduced into the carbonization reactor to maintain the temperature of the carbonization reactor, wherein the mass concentration of the liquid sodium silicate is 15-30% and the modulus is 3.3-3.5;

[0068] Liquid sodium silicate reacts with carbon dioxide and aqueous solution to obtain a first slurry;

[0069] The first slurry is transported to a precipitation reactor, and steam is added to the precipitation reactor to maintain the temperature of the precipitation reactor, and the first slurry in the precipitation reactor is repeatedly pumped to the carbonization reactor to maintain the liquid levels of the carbonization reactor and the precipitation reactor;

[0070] The first slurry precipitates a carbonized product in a precipitation reactor to form a second slurry;

[0071] The second slurry is transported to a cooling reactor, and circulating cooling water is added to the cooling reactor, and the second slurry is cooled to form a third slurry;

[0072] The third slurry is transported to a plate-and-frame filter, and hot water is introduced into the plate-and-frame filter to wash the third slurry to form a filter cake;

[0073] The filter cake is unloaded onto a belt conveyor and conveyed by the belt conveyor into a mixing and slurry mixing tank, where the filter cake is mixed with an aqueous solution to form a white carbon black slurry;

[0074] The white carbon black slurry is transported to a drying tower via a stirring transition tank, and the drying tower dries the white carbon black slurry to obtain a white carbon black product.

[0075] In some embodiments, the stirring frequency of the carbonization reactor is not less than 100 r / min, the temperature of the first slurry in the carbonization reactor is 70-95° C., the pH value of the first slurry is 9-12, and the residence time of the first slurry in the carbonization reactor is 3-10 min.

[0076] In some embodiments, the temperature of the second slurry in the precipitation reactor is 70-95°C, the pH value of the second slurry is 9.5-11, the residence time of the second slurry in the precipitation reactor is 60-180min, the pH value of the second slurry when entering the next process is 8.5-9.5, and the dissolved silicon content of the second slurry is less than 100PPm.

[0077] In some embodiments, the temperature of the third slurry in the cooling reactor is not higher than 85°C.

[0078] By adopting the above technical solution, the present invention has the following beneficial effects:

[0079] (1) The absorption reaction of the present invention is completed in a small gas-liquid carbonization reactor at normal pressure. The absorption is enhanced by high-intensity stirring and gas-liquid interface contact, so that the CO2 gas and liquid sodium silicate react rapidly and continuously in the carbonization reactor, and the efficient absorption of carbon dioxide is achieved under normal pressure reaction conditions. The carbonization reaction is carried out in a small absorption reactor, and the precipitation reaction can be carried out in a large precipitation reactor according to the scale. The solid-liquid reaction is carried out in the precipitation reactor, and the silicon dioxide microparticles generated by the absorption reaction are further aggregated and grown to form silicon dioxide particles with stable structure and reliable performance by controlling the reaction time, reaction temperature and reaction pH. Then, the absorption reaction is continued by reflux, and the pH value of the solution is further reduced, and the content of dissolved silicon dioxide precipitation in the solution is reduced to absorb carbon dioxide, so that the particle structure is stable and the performance is reliable, thereby improving the utilization efficiency of raw materials.

[0080] The carbon dioxide carbonization process for producing white carbon black of the present invention decomposes the synthesis reaction into two reaction processes, namely, a carbonization reaction and a precipitation reaction. The production can be continuous, and the problems that a relatively high pressure and temperature are required when a traditional integrated synthesis reactor is scaled up, or a multi-stage series forced gas-liquid reaction is required to improve the carbon dioxide absorption rate, the production lacks continuity, and the traditional gas-liquid contact is insufficient, resulting in a low carbon dioxide absorption rate in the reaction process.

[0081] (2) The present invention can simultaneously and continuously add liquid sodium silicate and CO2 into the carbonization reactor to carry out carbonization reaction of carbon dioxide, and continuously carry out precipitation reaction and cooling reaction. At the same time, the carbonization reactor is equipped with a slurry circulation to initiate a carbonization chain reaction of CO2, which can achieve efficient carbonization conversion of carbon dioxide and increase the carbonization reaction rate of CO2. Then, the carbon dioxide enters the precipitation reactor to continue the reaction. At the same time, when entering the cooling reactor, the silicon dioxide continues to condense and grow at variable temperature.

[0082] (3) Liquid sodium silicate with high mass concentration can be used as raw material, and the mass concentration of liquid sodium silicate reaches 20-30%, thereby improving the reaction efficiency and yield per unit volume during the reaction.

[0083] In addition, each functional unit in each embodiment of the present invention may be integrated into one processing unit, or each unit may exist physically separately, or two or more units may be integrated into one unit. The above-mentioned integrated unit may be implemented in the form of hardware or in the form of software functional units.

[0084] If the integrated unit is implemented in the form of a software functional unit and sold or used as an independent product, it can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of the present invention, in essence, or the part that contributes to the prior art, or all or part of the technical solution can be embodied in the form of a software product, and the computer software product is stored in a storage medium, including a number of instructions for a computer device (which can be a personal computer, server, or network device, etc.) or a processor (processor) to perform all or part of the steps of each embodiment of the present invention. The aforementioned storage medium includes: U disk, mobile hard disk, read-only memory (ROM, Read-Only Memory), random access memory (RAM, Random Access Memory), disk or optical disk and other media that can store program codes.

[0085] The above descriptions are only some embodiments of the present invention, and are not intended to limit the protection scope of the present invention. Any equivalent device or equivalent process transformation made using the contents of the present invention specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. An efficient short-process production system for carbonization-process white carbon black, characterized in that: include: A carbonization assembly, comprising a carbonization reactor, a first feed pipe, a second feed pipe, a third feed pipe and a first discharge pipe, wherein the first feed pipe, the second feed pipe, the third feed pipe and the first discharge pipe are all connected to the carbonization reactor, the first discharge pipe, the second feed pipe and the third feed pipe are respectively connected to the bottom of the carbonization reactor, the first feed pipe is used to introduce liquid sodium silicate, the second feed pipe is used to introduce steam, the third feed pipe is used to introduce carbon dioxide gas, the carbonization reactor is filled with an aqueous solution, the liquid sodium silicate and the carbon dioxide form a first slurry in the aqueous solution, and the first discharge pipe is used to output the first slurry; A precipitation assembly, comprising a precipitation reactor, a fourth feed pipe, a second discharge pipe and a third discharge pipe, wherein the precipitation reactor is filled with an aqueous solution, the first discharge pipe is connected to the top of the precipitation reactor, the fourth feed pipe, the second discharge pipe and the third discharge pipe are respectively connected to the bottom of the precipitation reactor, the fourth feed pipe is used to pass steam, the other end of the second discharge pipe is also connected to the carbonization reactor, the first slurry forms a second slurry in the precipitation reactor, the second discharge pipe is used to repeatedly pass the second slurry into the carbonization reactor, and the third discharge pipe is used to output the second slurry after the precipitation process is completed; A cooling assembly, comprising a cooling reactor, a fifth feed pipe, a fourth discharge pipe and a fifth discharge pipe, wherein the fifth discharge pipe and the fourth discharge pipe are both arranged at the bottom of the cooling reactor, the third discharge pipe is connected to the cooling reactor, the fifth feed pipe is used to introduce circulating cooling water, the fifth discharge pipe is used to output the circulating cooling water in the cooling reactor, the second slurry is cooled in the cooling reactor to form a third slurry, and the fourth discharge pipe is used to output the third slurry; A filter assembly, comprising a plate-frame filter, a sixth feed pipe and a belt conveyor, wherein the plate-frame filter is connected to the fourth discharge pipe, the sixth feed pipe is connected to the plate-frame filter, the sixth feed pipe is used to pass hot water, the belt conveyor is arranged at the output end of the plate-frame filter, the third slurry is repeatedly washed and filtered by hot water in the plate-frame filter to form a filter cake, and the belt conveyor is used to receive the filter cake after filtration; The drying component includes a stirring and slurry mixing tank, a stirring transition tank and a drying tower. The stirring and slurry mixing tank is connected to the output end of the belt conveyor, the output end of the stirring and slurry mixing tank is connected to the stirring transition tank, and the drying tower is connected to the output end of the stirring transition tank. The stirring and slurry mixing tank is used to stir the filter cake and the aqueous solution to form a fourth slurry, the stirring transition tank is used to transport the fourth slurry to the drying tower, and the drying tower dries the fourth slurry to form a white carbon black product.

2. The efficient short-process production system of carbonization-process silica according to claim 1, characterized in that: The carbonization assembly also includes a first connecting pipe, one end of which is connected to the top of the carbonization reactor, and the other end of which is connected to the precipitation reactor, and the connecting end of the first connecting pipe and the precipitation reactor is 10 to 30 mm lower than the liquid level of the precipitation reactor.

3. The efficient short-process production system of carbonization-process silica according to claim 2, characterized in that: The precipitation assembly further includes a second connecting pipe, the second connecting pipe is connected to the top of the precipitation reactor, and the second connecting pipe is also connected to the spray tower; The cooling assembly further includes a third connecting pipe, which is connected to the top of the cooling reactor and is also connected to the spray tower.

4. The efficient short-process production system of carbonization-process silica according to claim 3, characterized in that: The carbonization reactor is provided with a first agitator, a first thermometer, a first material level meter, and a first pH meter; the first feed pipe is provided with a first flow meter; the second feed pipe is provided with a second flow meter; and the third feed pipe is provided with a third flow meter; And / or, a second agitator, a second thermometer, a second material level meter, and a second pH meter are provided in the precipitation reactor, and a fourth flow meter is provided on the fourth feed pipe; And / or, a third agitator, a third thermometer, a third material level meter, and a third pH meter are provided in the precipitation reactor, and a fifth flow meter is provided on the fifth feed pipe; And / or, a fourth agitator, a fourth thermometer, a fourth material level meter, and a fourth pH meter are provided in the stirring and slurry mixing tank; And / or, a fifth agitator, a fifth thermometer, a fifth material level meter, and a fifth pH meter are provided in the stirring transition tank; And / or, a sixth flow meter is provided on the first discharge pipe, a seventh flow meter and a first delivery pump are provided on the second discharge pipe, an eighth flow meter and a second delivery pump are provided on the third discharge pipe, a ninth flow meter and a third delivery pump are provided on the fourth discharge pipe, a tenth flow meter is provided on the fifth discharge pipe, a fourth delivery pump is provided at the connection between the stirring and slurry mixing tank and the stirring transition tank, and a fifth delivery pump is provided at the connection between the stirring transition tank and the drying tower.

5. The efficient short-process production system of carbonization-process silica according to claim 4, characterized in that: The ratio of the height to the diameter of the carbonization reactor is not less than 3.

6. The efficient short-process production system of carbonization-process silica according to claim 4, characterized in that: The first agitator and / or the second agitator and / or the third agitator and / or the fourth agitator and / or the fifth agitator are self-priming stainless steel high-speed agitators.

7. An efficient short-process production method for carbonization white carbon black, characterized in that: Applicable to the production system according to any one of claims 1 to 6, the method comprising: Continuously adding liquid sodium silicate into the carbonization reactor, while continuously adding carbon dioxide from the bottom of the carbonization reactor, and introducing steam into the carbonization reactor to maintain the temperature of the carbonization reactor, wherein the mass concentration of the liquid sodium silicate is 15-30% and the modulus is 3.3-3.5; The liquid sodium silicate reacts with the carbon dioxide and the aqueous solution to produce the first slurry; The first slurry is transported to a precipitation reactor, and steam is added to the precipitation reactor to maintain the temperature of the precipitation reactor, and the first slurry in the precipitation reactor is repeatedly pumped to the carbonization reactor to maintain the liquid levels of the carbonization reactor and the precipitation reactor; The first slurry precipitates a carbonized product in the precipitation reactor to form the second slurry; The second slurry is transported to a cooling reactor, and circulating cooling water is added to the cooling reactor, and the second slurry is cooled to form a third slurry; The third slurry is transported to a plate-frame filter, and hot water is introduced into the plate-frame filter to wash the third slurry to form a filter cake; The filter cake is unloaded onto a belt conveyor, and is conveyed by the belt conveyor into a stirring and slurry mixing tank, where the filter cake is mixed with an aqueous solution to form a white carbon black slurry; The white carbon black slurry is transported to a drying tower via the stirring transition tank, and the drying tower dries the white carbon black slurry to obtain the white carbon black product.

8. The efficient short-process production method of carbonization-process white carbon black according to claim 7, characterized in that: The stirring frequency of the carbonization reactor is not less than 100 r / min, the temperature of the first slurry in the carbonization reactor is 70-95° C., the pH value of the first slurry is 9-12, and the residence time of the first slurry in the carbonization reactor is 3-10 min.

9. The efficient short-process production method of carbonization-process silica according to claim 8, characterized in that: The temperature of the second slurry in the precipitation reactor is 70-95°C, the pH value of the second slurry is 9.5-11, the residence time of the second slurry in the precipitation reactor is 60-180min, the pH value of the second slurry when entering the next process is 8.5-9.5, and the dissolved silicon content of the second slurry is less than 100PPm.

10. The efficient short-process production method of carbonization-process white carbon black according to claim 9, characterized in that: The temperature of the third slurry in the cooling reactor is not higher than 85°C.

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