Double-circulation double-effect carbonization device for preparing white carbon black

Abstract

The utility model relates to a double-circulation double-effect carbonization device for preparing white carbon black, which comprises a carbonization tank, the top of the carbonization tank is provided with a carbon dioxide inlet, a carbon dioxide outlet and a feed port, and the bottom of the carbonization tank is provided with a discharge port; the feed port is respectively connected with a water glass feed pipe and an outlet end of a Venturi ejector through a first three-way pipe, a main inlet of the Venturi ejector is connected with the discharge port through a slurry circulating pipe, a side inlet of the Venturi ejector is connected with a carbon dioxide gas outlet through a carbon dioxide circulating pipe, the slurry circulating pipe is provided with a slurry circulating pump, and the carbon dioxide gas outlet is provided with a carbon dioxide gas outlet. A carbon dioxide circulating pump is arranged on the carbon dioxide circulating pipe; and a plurality of ultrasonic vibrators and microwave radiation heads are arranged on the side part in the carbonization tank. According to the utility model, the reaction efficiency of carbon dioxide and water glass is greatly improved, the reaction time is shortened and high-quality nanoscale white carbon black products meeting requirements can be produced through the dual effects of high-energy microwave radiation and ultrasonic molecular oscillation on slurry in the tank in combination with double circulation.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical production, in particular to a carbonization device for double-cycle and double-effect preparation of silica white. Background Art

[0002] At present, in China, most of the silica white is still produced by the traditional precipitation method using strong acids (mainly sulfuric acid and hydrochloric acid). However, strong acids seriously corrode equipment, and a large amount of sulfates are discharged during production, resulting in serious pollution and great environmental protection pressure. The carbonization method using carbon dioxide and water glass as raw materials is a method between the gas phase method and the precipitation method, which eliminates the corrosion of strong acids to equipment and the emission of sulfates, and overcomes many disadvantages of the strong acid precipitation method for producing silica white. However, the existing carbonization method is usually carried out in a hydrothermal carbonization tank or a bubbling carbonization tower. The carbonization method belongs to a gas-liquid-solid three-phase reaction system controlled by liquid film. Due to the dual properties of water glass as a solution and a colloid, the mass transfer resistance between carbon dioxide and water glass in the gas-liquid two phases is large, which to a certain extent limits the progress of the reaction. Different reactors, different gas injection methods, and even different stirring methods will all affect the silica white product. It is necessary to fully carry out gas-liquid contact to improve the reaction efficiency. However, in addition to its solution properties, water glass also has colloidal properties. During the production process, carbon dioxide gas is difficult to penetrate deep into the interior of water glass for contact, resulting in low reaction efficiency and long time consumption. Content of the Utility Model

[0003] In view of this, the purpose of the utility model is to provide a carbonization device for double-cycle and double-effect preparation of silica white, which can improve the reaction efficiency, shorten the reaction time, and improve the quality of the silica white product.

[0004] The utility model adopts the following scheme: A carbonization device for double-cycle and double-effect preparation of silica white includes a carbonization tank. The top of the carbonization tank is provided with a carbon dioxide inlet, a carbon dioxide outlet, and a feed inlet. The bottom of the carbonization tank is provided with a discharge outlet. The feed inlet is respectively connected with a water glass feed pipe and the outlet end of a venturi injector through a first three-way pipe. The main inlet of the venturi injector is connected with the discharge outlet through a slurry circulation pipe, and the side inlet of the venturi injector is connected with the carbon dioxide outlet through a carbon dioxide circulation pipe. A slurry circulation pump is arranged on the slurry circulation pipe, and a carbon dioxide circulation pump is arranged on the carbon dioxide circulation pipe. A plurality of ultrasonic vibrators and microwave radiation heads are arranged on the inner side of the carbonization tank.

[0005] Further, the discharge outlet is also connected with a discharge pump through a discharge pipe, and the discharge outlet is connected with the discharge pipe and the slurry circulation pipe through a second three-way pipe.

[0006] Further, a carbon dioxide concentration sensor, a pressure sensor, a pressure relief valve, a liquid level sensor, and a temperature measuring sensor are also installed on the top of the carbonization tank. An on-line pH sensor is connected to one end of the slurry circulation pipe close to the second three-way pipe.

[0007] Furthermore, an intake electromagnetic valve is installed at the carbon dioxide intake port, an extraction electromagnetic valve is installed at the carbon dioxide outlet port, a feed electromagnetic valve is installed at the connection end of the first three-way pipe and the sodium silicate feed pipe, and a circulating feed electromagnetic valve is installed at the connection end of the first three-way pipe and the Venturi injector; a discharge electromagnetic valve is installed at the connection end of the second three-way pipe and the discharge pipe, and a circulating discharge electromagnetic valve is installed at the connection end of the second three-way pipe and the slurry circulation pipe.

[0008] Furthermore, the ultrasonic vibrators and the microwave radiation heads are distributed in an alternating hierarchical manner in the vertical direction, and there are several ultrasonic vibrators and microwave radiation heads in each layer, which are evenly distributed along the circumferential direction; all the ultrasonic vibrators are electrically connected in parallel with the ultrasonic generator outside the carbonization tank, and all the microwave radiation heads are electrically connected in parallel with the microwave generator outside the carbonization tank.

[0009] Compared with the prior art, the present utility model has the following beneficial effects: In the carbonization device for preparing silica by double-cycle and double-effect of the present utility model, the slurry and carbon dioxide form a double-cycle and violently mix and contact. Inside and outside the carbonization tank, the carbon dioxide gas fully contacts with the slurry and reacts efficiently; and through the dual effects of high-energy microwave radiation and ultrasonic molecular oscillation on the slurry in the tank, combined with the double-cycle, the reaction efficiency of carbon dioxide and sodium silicate is greatly improved, the reaction time is shortened, and the quality of the silica product is improved.

[0010] In order to make the purpose, technical solution and advantages of the present utility model clearer, the following will further describe the present utility model in detail through specific embodiments and related drawings. Description of the Drawings

[0011] Figure 1 is a schematic diagram of the overall structure of the carbonization device in the embodiment of the present utility model;

[0012] Figure 2 is a schematic diagram of the dual effect of the combination of microwave radiation energy and ultrasonic energy for high-strength molecular oscillation of the carbonization device in the embodiment of the present utility model;

[0013] Figure 3 is a schematic diagram of the production state of the carbonization device in the embodiment of the present utility model;

[0014] Figure 4 is a schematic diagram of the ultrasonic vibrator emitting ultrasonic waves in the embodiment of the present utility model;

[0015] Figure 5 is a schematic diagram of the microwave radiation head emitting microwave radiation energy in the embodiment of the present utility model;

[0016] Figure 6 is a schematic block diagram of the control principle of the carbonization device in the embodiment of the present utility model;

[0017] Description of reference numerals in the figure: 1 - carbonization tank; 2 - ultrasonic oscillator; 3 - microwave radiation head; 4 - carbon dioxide concentration sensor; 5 - pressure sensor; 6 - intake solenoid valve; 7 - pressure relief valve; 8 - exhaust solenoid valve; 9 - liquid level sensor; 10 - first three-way pipe; 11 - feed solenoid valve; 12 - temperature measuring sensor; 13 - reaction slurry; 14 - second three-way pipe; 15 - circulating discharge solenoid valve; 16 - online pH sensor; 17 - discharge solenoid valve; 18 - discharge pump; 19 - circulating feed solenoid valve; 20 - Venturi ejector; 21 - carbon dioxide circulation pump; 22 - slurry circulation pump; 23 - ultrasonic wave; 24 - microwave; 25 - ultrasonic generator; 26 - microwave generator. Detailed implementation manners

[0018] It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the present application. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which the present application belongs.

[0019] It should be noted that the terms used herein are only for describing specific implementation manners and are not intended to limit the exemplary implementation manners according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0020] As Figures 1 - 6 shown, a double-cycle and double-effect white carbon black carbonization device includes a carbonization tank 1. The top of the carbonization tank is provided with a carbon dioxide inlet, a carbon dioxide outlet, and a feed inlet, and the bottom of the carbonization tank is provided with a discharge outlet; the feed inlet is respectively connected to a water glass feed pipe and the outlet end of a Venturi ejector 20 through a first three-way pipe 10. The main inlet of the Venturi ejector 20 is connected to the discharge outlet through a slurry circulation pipe, and the side inlet of the Venturi ejector is connected to the carbon dioxide outlet through a carbon dioxide circulation pipe. A slurry circulation pump 22 is provided on the slurry circulation pipe, and a carbon dioxide circulation pump 21 is provided on the carbon dioxide circulation pipe. The carbon dioxide circulation pump 21 is used to extract the unreacted completely carbon dioxide mixed gas overflowing from the upper part of the liquid in the carbonization tank, and then strongly suck it in by the side inlet negative pressure generated by the high-speed flowing slurry inside through the Venturi ejector, and after being violently mixed with the slurry, they are sprayed into the tank together to continue the carbonization reaction; several ultrasonic oscillators 2 and microwave radiation heads 3 are provided on the inner side of the carbonization tank. The microwave radiation head emits microwave radiation energy to the solution in the tank to keep the solution within a certain reaction temperature range. The high-intensity ultrasonic waves generated by the ultrasonic oscillator perform violent molecular oscillation on the inside of the liquid in the tank, greatly improving the reaction efficiency of carbon dioxide and water glass.

[0021] In a sealed carbonization tank, at a set pressure and temperature, carbon dioxide gas undergoes intense ultrasonic vibration and bubbling contact with refined water glass, resulting in a chemical reaction that gradually produces silica slurry. Many of the gases overflowing during the reaction are carbon dioxide gases that have not fully participated in the reaction. These incompletely reacted mixed carbon dioxide gases are extracted, and after being vigorously mixed with the slurry circulating outside the tank, they are then sprayed back into the tank. Through continuous circulation, they enter the carbonization tank and vigorously bubble in the water glass solution. Similarly, the slurry also circulates inside and outside the carbonization tank, forming a double-circulation intense mixing contact with carbon dioxide. Outside the carbonization tank, carbon dioxide gas and the slurry are efficiently mixed and sprayed into the tank through a Venturi device. Inside and outside the carbonization tank, carbon dioxide gas is in full contact with the slurry for efficient reaction. A number of microwave radiation heads and ultrasonic vibrators are evenly installed and inlaid on the inner wall of the carbonization tank. Through the dual effects of high-energy microwave radiation and ultrasonic molecular oscillation on the slurry in the tank, combined with the double circulation, the reaction efficiency of carbon dioxide and water glass is greatly improved, the reaction time is shortened, high-quality nano-level white carbon black products meeting the requirements can be produced, and the yield of silica produced is over 95%. The double circulation refers to the circulation of carbon dioxide gas inside and outside the carbonization tank and the circulation of incompletely reacted silica slurry inside and outside the tank. The dual effects refer to the microwave radiation energy effect and the high-strength molecular oscillation effect of ultrasonic energy.

[0022] In this embodiment, the discharge port is also connected to a discharge pump 18 through a discharge pipe. The discharge port is connected to the discharge pipe and the slurry circulation pipe through a second three-way pipe 14. The discharge pump pumps the white carbon black slurry generated after the reaction to the next pressure filtration, washing, and sodium carbonate recovery processes.

[0023] In this embodiment, the carbonization tank is made of high-quality stainless steel into a cylindrical tank with upper and lower semi-elliptical heads according to the requirements of a pressure vessel. The inner wall of the tank is lined with a tetrafluoro inner wall, ensuring that the microwave radiation energy is absorbed by the slurry in the tank, while the inner wall of the tank does not absorb microwave radiation energy.

[0024] In this embodiment, a carbon dioxide concentration sensor 4, a pressure sensor 5, a pressure relief valve 7, a liquid level sensor 9, and a temperature measurement sensor 12 are also installed on the top of the carbonization tank; an on-line pH sensor 16 is connected to one end of the slurry circulation pipe near the second three-way pipe 14. The liquid level sensor 9 uses a radar wave non-contact liquid level sensor, and the temperature measurement sensor 12 uses an infrared non-contact temperature measurement sensor, which are respectively used to monitor the temperature and liquid level in the tank. The relief valve is used to maintain the pressure in the tank within a certain set range. When the carbon dioxide concentration sensor 4 detects that the carbon dioxide gas concentration is lower than the lower limit of the set value, high-purity carbon dioxide is supplemented through the air inlet to the upper limit value. When the pressure sensor detects that the pressure in the tank exceeds the upper pressure limit value, it is depressurized to the set pressure value through the pressure relief valve 7. The on-line pH sensor 16 is used to monitor the pH value of the circulating slurry.

[0025] In this embodiment, an intake electromagnetic valve 6 is installed at the carbon dioxide intake port, an extraction electromagnetic valve 8 is installed at the carbon dioxide outlet port, a feed electromagnetic valve 11 is installed at the connection end of the first three-way pipe and the sodium silicate feed pipe, and a circulating feed electromagnetic valve 19 is installed at the connection end of the first three-way pipe and the Venturi injector; a discharge electromagnetic valve 17 is installed at the connection end of the second three-way pipe and the discharge pipe, and a circulating discharge electromagnetic valve 15 is installed at the connection end of the second three-way pipe and the slurry circulating pipe.

[0026] In this embodiment, the ultrasonic vibrators 2 and the microwave radiation heads 3 are distributed in an alternating hierarchical manner in the vertical direction. There are several ultrasonic vibrators 2 and microwave radiation heads 3 in each layer and they are evenly distributed along the circumferential direction; all the ultrasonic vibrators are electrically connected in parallel with an ultrasonic generator 25 outside the carbonization tank, and all the microwave radiation heads are electrically connected in parallel with a microwave generator 26 outside the carbonization tank.

[0027] It further includes a control module for controlling the operation of the carbonization device. The control module pre-sets an operation program, including: temperature, pressure, liquid level, pH value at the end point of the slurry reaction, static aging time, etc. The input end of the control module is electrically connected to the output ends of a temperature measuring sensor, a carbon dioxide concentration sensor, a pressure sensor, a liquid level sensor, an on-line pH sensor, a time relay, etc. The output end of the control module is electrically connected to the input ends of an intake electromagnetic valve, an extraction electromagnetic valve, a carbon dioxide circulating pump, a feed electromagnetic valve, a circulating feed electromagnetic valve, a pressure relief valve, a slurry circulating pump, a discharge pump, a discharge electromagnetic valve, a circulating discharge electromagnetic valve, a microwave generator, an ultrasonic generator, etc. Among them, the operation program of the control module belongs to conventional technology, and those skilled in the art can easily figure out how to program and set the operation program according to the structure and working process of the carbonization device of this application.

[0028] A method for preparing white carbon black by double-cycle double-effect. First, prepare a refined sodium silicate solution with a certain Baume degree in the previous process and add 4%-8% additives (the additive is an EDTA mixed depolymerizer) to configure the raw material sodium silicate; the following production process combined with this additive can produce higher-quality nano-level white carbon black products that meet the requirements. Using the double-cycle double-effect white carbon black carbonization device as described above, it includes the following steps:

[0029] (1) Open the feed electromagnetic valve 11 and add the raw material sodium silicate into the carbonization tank 1. When the liquid level sensor 9 detects that the set liquid level value is reached, close the sodium silicate inlet electromagnetic valve 11;

[0030] (2) Turn on the ultrasonic generator 25 and the microwave generator 26;

[0031] (3) When the temperature sensor 12 detects that the temperature in the carbonization tank 1 reaches the set value, open the carbon dioxide gas inlet solenoid valve 6 to add high-purity carbon dioxide gas into the carbonization tank 1. When the pressure sensor 5 detects that the set pressure value is reached, close the inlet solenoid valve 6;

[0032] (4) Open the circulating feed solenoid valve 19, the circulating discharge solenoid valve 15, and the slurry circulating pump 22 in sequence to perform the in-tank and out-of-tank circulation of the slurry; then open the air extraction solenoid valve 8 and the carbon dioxide circulating pump 21 in sequence to perform the in-tank and out-of-tank circulation of the carbon dioxide gas; the mixed gas continuously overflowing in the carbonization tank 1 is pumped out by the carbon dioxide circulating pump 21, and after being violently mixed with the circulating slurry through the Venturi injector 20, it is sprayed into the carbonization tank 1 and circulated continuously; whether in the carbonization tank or outside the carbonization tank, the carbon dioxide gas is continuously and fully contacted with the slurry, and the reaction is efficient;

[0033] (5) When the carbon dioxide concentration sensor 4 monitors that the carbon dioxide concentration in the tank drops to the lower limit set value, open the inlet solenoid valve 6 to supplement high-purity carbon dioxide gas, and close the inlet solenoid valve 6 when it reaches the upper limit set value of the carbon dioxide concentration, so as to always keep the carbon dioxide gas concentration in the tank within the set range;

[0034] (6) When the pressure sensor 5 monitors that the pressure in the tank reaches the upper limit of the set value, open the pressure relief valve 7, and close the pressure relief valve 7 when the pressure is relieved to the lower limit of the pressure setting, so as to always keep the pressure in the tank within the set range;

[0035] (7) When the temperature sensor 12 detects that the temperature in the tank reaches the upper limit set value, turn off the microwave generator 26, and when the temperature is lower than the lower limit set value, turn on the microwave generator 26 again, so as to always keep the temperature within the set range;

[0036] (8) When the on-line pH sensor 16 detects that the pH value of the slurry reaches the set value and remains unchanged within the set time, turn off the carbon dioxide circulating pump 21, the air extraction solenoid valve 8, the circulating discharge solenoid valve 15, the slurry circulating pump 22, the circulating feed solenoid valve 19, the microwave generator 26, and the ultrasonic generator 25 in sequence;

[0037] (9) Open the discharge solenoid valve 17 and the discharge pump 18 to pump the slurry that has completed the reaction in the carbonization tank to the next process for slurry pressure filtration washing and sodium carbonate recovery; after the discharge is completed, close the discharge solenoid valve 17 and the discharge pump 18 in sequence to prepare for the production of the next production cycle.

[0038] In the method for preparing silica by double-loop double-effect, double-loop of carbon dioxide gas and reaction slurry is realized inside and outside the tank. Whether inside or outside the carbonization tank, the carbon dioxide gas is continuously and sufficiently contacted with the slurry for efficient reaction. At the same time, the dual effects of microwave energy radiation and ultrasonic strong molecular oscillation are combined, and fresh high-purity carbon dioxide gas is automatically supplemented to always maintain the stability of the temperature, pressure and carbon dioxide concentration inside the carbonization tank, overcoming the disadvantage that the existing carbonization method or carbonization equipment cannot effectively improve the full and in-depth contact reaction between carbon dioxide gas and water glass with dual properties of liquid and colloid.

[0039] For any of the technical solutions disclosed by the present utility model as described above, unless otherwise stated, if it discloses a numerical range, the disclosed numerical range is a preferred numerical range. Any person skilled in the art should understand that the preferred numerical range is only the numerical values with obvious technical effects or representativeness among many feasible numerical values. Since there are too many numerical values to enumerate, the present utility model only discloses some numerical values to illustrate the technical solutions of the present utility model. Moreover, the above-listed numerical values should not constitute a limitation to the protection scope of the present invention.

[0040] If the present utility model discloses or involves components or structural parts that are fixedly connected to each other, then, unless otherwise stated, the fixed connection can be understood as: a detachable fixed connection (for example, connected by bolts or screws), or can also be understood as: a non-detachable fixed connection (for example, riveting, welding). Of course, the mutual fixed connection can also be replaced by an integral structure (for example, manufactured by integral forming using casting technology) (except when it is obviously impossible to adopt the integral forming process).

[0041] In addition, for the terms used to represent the positional relationship or shape in any of the technical solutions disclosed by the present utility model as described above, unless otherwise stated, their meanings include states or shapes that are approximate, similar or close to them.

[0042] Any component provided by the present utility model can either be assembled from multiple separate components or be a single component manufactured by integral forming technology.

[0043] The above is only a preferred embodiment of the present utility model, and it is not a limitation to the present utility model in other forms. Any person skilled in the art may use the disclosed technical content to make changes or modifications into equivalent embodiments with equivalent changes. However, any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present utility model without departing from the technical solution content of the present utility model still belong to the protection scope of the technical solution of the present utility model.

Claims

1. A double-circulation double-effect carbonization device for preparing white carbon black, characterized in that: It includes a carbonization tank, wherein a carbon dioxide inlet, a carbon dioxide outlet and a feed port are arranged on the top of the carbonization tank, and a discharge port is arranged on the bottom of the carbonization tank; the feed port is respectively connected to a water glass feed pipe and an outlet end of a venturi ejector through a first three-way pipe, the main inlet of the venturi ejector is connected to the discharge port through a slurry circulation pipe, the side inlet of the venturi ejector is connected to the carbon dioxide outlet through a carbon dioxide circulation pipe, a slurry circulation pump is arranged on the slurry circulation pipe, and a carbon dioxide circulation pump is arranged on the carbon dioxide circulation pipe; a plurality of ultrasonic vibrators and microwave radiation heads are arranged on the inner side of the carbonization tank.

2. The double-circulation double-effect carbonization device for preparing white carbon black according to claim 1, characterized in that: The discharge port is also connected to a discharge pump via a discharge pipe, and the discharge port is connected to the discharge pipe and the slurry circulation pipe via a second three-way pipe.

3. The double-circulation double-effect carbonization device for preparing white carbon black according to claim 2, characterized in that: A carbon dioxide concentration sensor, a pressure sensor, a pressure relief valve, a liquid level sensor, and a temperature sensor are also installed on the top of the carbonization tank; an online pH sensor is connected to one end of the slurry circulation pipe close to the second three-way pipe.

4. The double-circulation double-effect carbonization device for preparing white carbon black according to claim 3, characterized in that: The carbon dioxide inlet is equipped with an air intake solenoid valve, the carbon dioxide outlet is equipped with an exhaust solenoid valve, the end of the first three-way pipe connected to the water glass feed pipe is equipped with a feed solenoid valve, and the end of the first three-way pipe connected to the venturi injector is equipped with a circulation feed solenoid valve; the end of the second three-way pipe connected to the discharge pipe is equipped with a discharge solenoid valve, and the end of the second three-way pipe connected to the slurry circulation pipe is equipped with a circulation discharge solenoid valve.

5. The double-circulation double-effect carbonization device for preparing white carbon black according to claim 1, characterized in that: The ultrasonic vibrators and microwave radiation heads are distributed in staggered layers in the vertical direction, and each layer has a plurality of ultrasonic vibrators and microwave radiation heads that are evenly distributed along the circumference; all ultrasonic vibrators are electrically connected in parallel with the ultrasonic generator outside the carbonization tank, and all microwave radiation heads are electrically connected in parallel with the microwave generator outside the carbonization tank.

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