CN106732206B - Intelligent reaction kettle and recycling method of hydrofluoric acid and hydrochloric acid mixed acid - Google Patents

Intelligent reaction kettle and recycling method of hydrofluoric acid and hydrochloric acid mixed acid Download PDF

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CN106732206B
CN106732206B CN201611042746.4A CN201611042746A CN106732206B CN 106732206 B CN106732206 B CN 106732206B CN 201611042746 A CN201611042746 A CN 201611042746A CN 106732206 B CN106732206 B CN 106732206B
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reaction
electromagnetic valve
acid
hydrochloric acid
feeding
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CN106732206A (en
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严招春
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Quzhou Xinbu Chemical Technology Co ltd
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Quzhou Xinbu Chemical Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B01D29/03Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B01D29/075Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements located in a closed housing and comprising scrapers or agitators on the cake side of the filtering elements, e.g. Nutsche- or Rosenmund-type filters for performing multiple step operations such as chemical reactions, filtering and cake treatment
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/20Halides
    • C01F11/22Fluorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/20Halides
    • C01F11/24Chlorides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • B01J2208/00168Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
    • B01J2208/00212Plates; Jackets; Cylinders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00592Controlling the pH

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses an intelligent reaction kettle and a method for recycling hydrofluoric acid and hydrochloric acid mixed acid, wherein the reaction kettle is redesigned, so that the reaction kettle used in the invention can perfectly match with the recycling of the mixed acid, and is time-saving and labor-saving. Continuously adding witherite powder (barium carbonate) into a reaction kettle filled with mixed acid, controlling the pH value and the reaction end point, performing suction filtration after the reaction is finished, and washing and drying filter residues to obtain a barium fluoride product; the filtrate is purified and refined to be a barium chloride aqueous solution product, which can be directly sold as a liquid product for the outside and can also be concentrated into a solid product for the outside. The recycling method processes the mixed acid into two products of barium fluoride and barium chloride, so that the mixed acid is completely utilized, waste is turned into wealth, and the environment is not polluted.

Description

Intelligent reaction kettle and recycling method of hydrofluoric acid and hydrochloric acid mixed acid
Technical Field
The invention relates to the field of chemistry, in particular to an intelligent reaction kettle and a method for recycling hydrofluoric acid and hydrochloric acid mixed acid.
Background
Hydrofluoric acid is an aqueous solution of hydrogen fluoride gas, clear, colorless, fuming, corrosive liquid, with a severe pungent odor. Melting point-83.3 deg.C, boiling point 112.2 deg.C, and density 0.888g/cm3. Is easily soluble in water and ethanol, and slightly soluble in diethyl ether. Because the bonding capacity between hydrogen and fluorine atoms is relatively strong, such that hydrofluoric acid cannot be completely ionized in water, it is theorized that low concentrations of hydrofluoric acid are weak acids (actually medium strong acids in terms of their ionization constants). Has extremely strong corrosivity, and can strongly corrode metal, glass and objects containing silicon. Such as inhalation of vapor or contact with the skin, can cause difficult to heal burns. Hydrofluoric acid plays an important role in the purification of aluminum and uranium due to its ability to dissolve oxides. Hydrofluoric acid is also used for etching glass, and patterns, scales and characters can be engraved; it is used by the semiconductor industry to remove oxides from silicon surfaces, it can be used as a catalyst in the alkylation of isobutane with n-butenes in refineries, and hydrofluoric acid is also used in "pickling" processes to remove oxygen-containing impurities from stainless steel surfaces. Hydrofluoric acid is also used in the synthesis of many fluorine-containing organic compounds, such as Teflon (polytetrafluoroethylene) and refrigerants such as freon.
Hydrochloric acid is an aqueous solution of hydrogen chloride, belongs to strong inorganic acid, and has wide industrial application. The hydrochloric acid is colorless and transparent liquid, has strong pungent smell, and has high corrosivity. The concentrated hydrochloric acid (mass fraction is about 37%) has extremely strong volatility, so that hydrogen chloride gas can volatilize after a container containing the concentrated hydrochloric acid is opened, and the hydrogen chloride gas is combined with water vapor in the air to generate small drops of hydrochloric acid, so that acid mist appears above a bottle mouth. Hydrochloric acid is the main component of gastric acid and it promotes digestion of food and protects against microbial infections. Hydrochloric acid is a colorless liquid (industrial hydrochloric acid is slightly yellow due to impurities of trivalent iron salt), corrosive, aqueous solution of hydrogen chloride and pungent smell, and concentrated hydrochloric acid is dissolved in water and releases heat. Dissolving in alkali liquor and performing neutralization reaction with the alkali liquor. Since concentrated hydrochloric acid is volatile, the volatilized hydrogen chloride gas reacts with water vapor in the air to form small drops of hydrochloric acid, so that white mist is seen. Hydrochloric acid is a strong inorganic acid and has wide application in industrial processes, such as metal refining.
In recent years, with the continuous development of fluorine chemical industry, the yield of fluorine products such as fluorine refrigerant fluoroplastics is increasing. In the production process thereof, a large amount of mixed acid containing hydrofluoric acid and hydrochloric acid (hereinafter referred to as mixed acid) is generated due to process requirements. The mixed acid comprises 10-40% of hydrofluoric acid, 3-20% of hydrochloric acid, the balance of water and a small amount of other impurities. The mixed acid cannot be directly sold and needs to be treated. Most of the current use factories of the mixed acid are unlicensed underground factories, the factories use the mixed acid to treat metal surfaces, acid-containing wastewater is directly discharged in the production process, and the environmental pollution is very serious. Even if the certified manufacturers can only discharge the hydrochloric acid in the mixed acid after neutralizing.
From the viewpoint of recycling economy, the mixed acid is recycled, and other fluorine chemical products are produced by using hydrofluoric acid in the mixed acid, so that the fluorine chemical products are separated from hydrochloric acid, and the fluorine chemical products and related products formed by the hydrochloric acid are sold respectively. Therefore, the method can reduce a large amount of fluorine-containing industrial waste, improve the environment, realize the maximum resource utilization rate, reduce the production cost and have obvious social and economic benefits.
Disclosure of Invention
The invention aims to provide an intelligent reaction kettle and a method for recycling hydrofluoric acid and hydrochloric acid mixed acid, which utilize witherite powder (barium carbonate) to respectively react with hydrofluoric acid and hydrochloric acid in the mixed acid so as to obtain a barium fluoride product and a barium chloride aqueous solution product, completely utilize the mixed acid, change waste into valuable and realize zero pollution and zero emission.
In order to solve the technical problems, the following technical scheme is adopted:
the utility model provides an intelligent reation kettle, includes the cauldron body, the internal reaction layer and the suction filtration layer of including of cauldron, the surface of the cauldron body is equipped with the cooling water jacket, is equipped with water inlet and delivery port, its characterized in that on the cooling water jacket: the upper end of the kettle body is provided with a first feed inlet and a second feed inlet, the lower end of the first feed inlet is connected with a first feed hopper, and the lower end of the first feed hopper is connected with a first feed pipe; the lower end of the second feed inlet is connected with a second feed hopper, the lower end of the second feed hopper is connected with a second feed pipe, and a feed buffer and a first electromagnetic valve are mounted on the second feed pipe; the surface of the kettle body is provided with a control panel, a control circuit and a single chip microcomputer are arranged in the control panel, the single chip microcomputer is matched with the control circuit, and a first electromagnetic valve is connected to the control circuit; be equipped with the filter plate subassembly between reaction layer and the suction filtration layer, the filter plate subassembly is connected on control circuit, is connected with the suction filtration pump on the suction filtration layer, and the suction filtration pump is installed in the surface of the cauldron body, and the suction filtration pump is connected on control circuit.
Further, the feeding buffer comprises an upper opening, a lower opening, a connecting rod and a driving device, wherein an upper opening plug is arranged at the upper end of the connecting rod, a lower opening plug is arranged at the lower end of the connecting rod, the upper opening plug is matched with the upper opening, and the lower opening plug is matched with the lower opening; the middle position of connecting rod is equipped with driven gear, and drive arrangement includes buffer motor, output pivot, district shoulder, connecting plate, reciprocating gear and driving gear, and the output pivot is connected to the buffer motor, and output pivot joining region shoulder, district shoulder connection connecting plate, and reciprocating gear is connected to the connecting plate, and reciprocating gear connects the driving gear, driving gear and driven gear intermeshing. The feeding buffer buffers the feeding rate of the withered and heavy stone powder by means of the upper opening plug and the lower opening plug, so that the reaction rate is prevented from being influenced by too fast feeding; under the action of the feeding buffer, the witherite powder is continuously and stably put into the reaction layer, so that the reaction rate is remarkably accelerated, and reactants are fully utilized.
Further, the upper end on reaction layer is equipped with the interlayer, and first inlet pipe runs through the interlayer with the second inlet pipe, the lower extreme intercommunication reaction layer of first inlet pipe and second inlet pipe. The interlayer isolates the reaction layer, thereby preventing the volatilization of hydrochloric acid and avoiding waste.
Further, the internal agitator that installs of cauldron, agitator include agitator motor and frame stirring rake, and agitator motor installs in the upper end of interlayer, and agitator motor even goes out to have the (mixing) shaft, and the (mixing) shaft runs through the interlayer, and the agitator shaft is connected frame stirring rake, and frame stirring rake is located the reaction layer. The stirrer accelerates the reaction rate and improves the generation rate of products.
Further, a first PH value adjusting groove is formed in the left side of the kettle body, a third feeding pipe is connected to the first PH value adjusting groove, a second electromagnetic valve is connected to the third feeding pipe, and the third feeding pipe is communicated with the reaction layer; a second PH value adjusting groove is formed in the right side of the kettle body, a fourth feeding pipe is connected to the second PH value adjusting groove, a third electromagnetic valve is connected to the fourth feeding pipe, and the fourth feeding pipe is communicated with the reaction layer; the control circuit is connected with a regulating circuit, the regulating circuit comprises a regulating switch, a second electromagnetic valve and a third electromagnetic valve, the single chip microcomputer controls the regulating switch, the regulating switch is matched with the second electromagnetic valve, and the regulating switch is matched with the third electromagnetic valve; and a PH measuring meter is arranged in the reaction layer, and the PH measuring meter is matched with the single chip microcomputer.
Further, the filter plate assembly comprises a filter plate and an electric rotary disc, wherein the filter plate is provided with a filter area, the electric rotary disc is provided with a sealing plate, and the sealing plate is matched with the filter area; the control circuit comprises a timing circuit, a timing module is arranged in the control panel and connected with the single chip microcomputer, the timing circuit comprises a timing switch and an electric turntable, the single chip microcomputer controls the timing switch, the timing switch is matched with the electric turntable, and the electric turntable is connected with the suction filtration pump in series.
The method for recycling the mixed acid of hydrofluoric acid and hydrochloric acid by adopting the intelligent reaction kettle is characterized by comprising the following steps:
(1) collecting mixed acid of hydrofluoric acid and hydrochloric acid, taking a proper amount of mixed acid samples, and respectively analyzing the concentration of the hydrofluoric acid and the concentration of the hydrochloric acid in the samples;
(2) calculating the theoretical usage amount of the witherite powder according to the concentration of the hydrofluoric acid and the hydrochloric acid and the total volume of the mixed acid in the step (1), wherein the actual usage amount of the witherite powder is 1.05 times of the theoretical usage amount of the witherite powder;
(3) adding mixed acid into the reaction layer through a first feed inlet, adding witherite powder into a second feed hopper through a second feed inlet, filling sodium bicarbonate into the first pH value adjusting groove, and filling low-concentration hydrochloric acid into the second pH value adjusting groove;
(4) firstly, setting a reaction time of 2-3h in a timing module of a control panel, introducing cooling water into a cooling water jacket, starting a reaction kettle, opening a first electromagnetic valve, continuously putting witherite powder into a reaction layer, synchronously starting a stirrer, and adjusting the pH value of a reaction solution by means of sodium bicarbonate and low-concentration hydrochloric acid; after the reaction is finished, opening the electric turntable, starting a suction filtration pump, starting suction filtration, and obtaining filtrate and filter residues after suction filtration;
(5) taking out filter residues, and treating the filter residues to obtain a barium fluoride product;
(6) and removing impurities from the filtrate and refining to obtain a barium chloride aqueous solution product.
Preferably, the stirring speed of the stirrer in the step (3) is controlled to be 500-780 r/min.
Preferably, the specific steps of adjusting the PH value in step (3) are: when the PH value in the reaction solution measured by the PH meter is too low, the singlechip controls the regulation switch to open the second electromagnetic valve, sodium bicarbonate is added until the PH value of the reaction solution measured by the PH meter is normal, and the second electromagnetic valve is closed; when the PH value in the reaction liquid measured by the PH meter is too high, the singlechip controls the regulation switch to open the third electromagnetic valve, low-concentration dilute hydrochloric acid is added until the PH value of the reaction liquid measured by the PH meter is normal, and the third electromagnetic valve is closed.
Preferably, the post-treatment in the step (5) comprises the following specific steps: firstly, adding a small amount of hydrochloric acid into filter residue, filtering again to obtain a crude product of barium fluoride, and washing and drying the crude product to obtain a barium fluoride product.
Due to the adoption of the technical scheme, the method has the following beneficial effects:
the invention relates to an intelligent reaction kettle and a recycling method of hydrofluoric acid and hydrochloric acid mixed acid, which utilize witherite powder (barium carbonate) to respectively react with hydrofluoric acid and hydrochloric acid in the mixed acid, thereby obtaining a barium fluoride product and a barium chloride aqueous solution product, completely utilizing the mixed acid, changing waste into valuable, and realizing zero pollution and zero emission. The concrete beneficial effects are as follows:
1. the second feed hopper, the second feed inlet and the second feed pipe are matched for use, the second feed hopper is large in size, can accommodate a large amount of toxic heavy stone powder, does not need to be added for multiple times, and is time-saving and labor-saving; realize continuous and uninterrupted adding of witherite powder and promote reaction.
2. The feeding buffer buffers the feeding speed of the withered and heavy stone powder by means of an upper opening plug and a lower opening plug, and the working principle is as follows: after the buffer motor is started, the connecting rod is driven by each transmission part to reciprocate up and down, in the downward movement process, the upper opening plug is separated from the upper opening, the lower opening plug is used for plugging the lower opening, and the witherite powder enters the feeding buffer from the upper opening; in the upward movement process of the connecting rod, the upper opening plug blocks the upper opening, the lower opening is opened, and the witherite powder is introduced into the reaction layer, so that the reciprocating movement realizes continuous buffer feeding. The device avoids the influence on the reaction rate caused by too fast feeding; under the action of the feeding buffer, the witherite powder is continuously and stably put into the reaction layer, so that the reaction rate is remarkably accelerated, and reactants are fully utilized.
3. First solenoid valve is connected on control circuit, opens and close through control circuit control first solenoid valve to control poison heavy mountain flour feeding, simple structure, the practicality is strong.
4. The filter plate subassembly is equipped with the shrouding including taking out filter plate and electric carousel on the electric carousel, and the shrouding is used for the switch or closes the suction filtration district, and specific theory of operation is as follows: in the reaction process, the control circuit controls a sealing plate of the electric turntable to seal the suction filtration area, so that unreacted raw materials are prevented from leaking into the suction filtration layer; after the reaction is finished, the timing switch is connected with the electric rotating disc, the electric rotating disc is started, the sealing plate opens the suction filtration area, the suction filtration pump is started, and suction filtration work is started. The filter plate component is matched with a suction filter pump to complete suction filtration under the control of a timing switch, so that time and labor are saved.
5. The invention adopts witherite powder to recycle mixed acid, and the mixed acid is processed into two products of barium fluoride and barium chloride, and the mixed acid is completely utilized. Therefore, the method can reduce a large amount of fluorine-containing industrial waste, improve the environment, realize the maximum resource utilization rate, reduce the production cost and have obvious social and economic benefits.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a schematic structural diagram of an intelligent reaction vessel according to the present invention;
FIG. 2 is a schematic view of the structure of a feed buffer according to the present invention;
FIG. 3 is a schematic structural diagram of a control panel according to the present invention;
FIG. 4 is a schematic illustration of the construction of a filter plate assembly according to the present invention;
FIG. 5 is a control circuit diagram of the present invention;
FIG. 6 is a portion of the timing circuit of FIG. 5;
fig. 7 is a portion of the conditioning circuit of fig. 5.
In the diagram of fig. 5, T is a transformer, K is a main switch, M1 is a buffer motor, PV1 is a first electromagnetic valve, M2 is a stirring motor, U is a relay, C1, C2 and C3 are all protection capacitors, K1 is a timing switch, PV2 is an electric turntable, PV3 is a suction pump, K2 is a regulation switch, PV4 is a second electromagnetic valve, PV5 is a third electromagnetic valve, and L is a reverse diode.
Detailed Description
The invention discloses an intelligent reaction kettle and a method for recycling hydrofluoric acid and hydrochloric acid mixed acid, wherein witherite powder (barium carbonate) is used for respectively reacting with hydrofluoric acid and hydrochloric acid in the mixed acid, so that a barium fluoride product and a barium chloride aqueous solution product are obtained, and the mixed acid is completely utilized.
An intelligent reaction kettle comprises a kettle body 1, wherein a reaction layer 2 and a suction filtration layer 3 are arranged in the kettle body 1, raw materials react in the reaction layer 2, and a product is subjected to suction filtration in the suction filtration layer 3. The surface of the kettle body 1 is provided with a cooling water jacket 4, a large amount of heat can be generated in the reaction process of the mixed acid and the witherite powder, and cold water is usually continuously injected into the cooling water jacket 4 to remove a large amount of heat in the reaction layer 2. The cooling water jacket 4 is provided with a water inlet 45 and a water outlet 46, the water inlet 45 is connected with a water inlet pipe, the water outlet 46 is connected with a water outlet pipe, cooling water is injected continuously, and the cooling effect is improved remarkably.
The upper end of the kettle body 1 is provided with a first feeding hole 5 and a second feeding hole 8, the lower end of the first feeding hole 5 is connected with a first feeding hopper 6, the lower end of the first feeding hopper 6 is connected with a first feeding pipe 7, the first feeding pipe 7 is communicated with the reaction layer 2, and mixed acid is fed into the reaction layer 2 through the first feeding hole 5, the first feeding hopper 6 and the first feeding pipe 7. The lower extreme of second feed inlet 8 is connected with second feeder hopper 9, and the lower extreme of second feeder hopper 9 is connected with second inlet pipe 10, installs feeding buffer 47 and first solenoid valve 11 on the second inlet pipe 10, and the witherite powder drops into in the reaction layer 2 through second feed inlet 8, second feeder hopper 9 and second inlet pipe 10. The second feed hopper 9, the second feed inlet 8 and the second feed pipe 10 are matched for use, the second feed hopper 9 is large in size, can contain a large amount of withered stone powder, does not need to be added for multiple times, and is time-saving and labor-saving; realize continuous and uninterrupted adding of witherite powder and promote reaction.
The feeding buffer 47 comprises an upper port 34, a lower port 36, a connecting rod 32 and a driving device, wherein the upper end of the connecting rod 32 is provided with an upper port plug 33, the lower end of the connecting rod 32 is provided with a lower port plug 35, the upper port plug 33 is matched with the upper port 34, and the lower port plug 35 is matched with the lower port 36; the middle position of the connecting rod 32 is provided with a driven gear 31, the driving device comprises a buffer motor 25, an output rotating shaft 26, a region shoulder 27, a connecting plate 28, a reciprocating gear 29 and a driving gear 30, the buffer motor 25 is connected with the output rotating shaft 26, the output rotating shaft 26 is connected with the region shoulder 27, the region shoulder 27 is connected with the connecting plate 28, the connecting plate 28 is connected with the reciprocating gear 29, the reciprocating gear 29 is connected with the driving gear 30, and the driving gear is meshed with the driven gear 31. The feeding buffer 47 buffers the feeding rate of the witherite powder by the upper opening plug 33 and the lower opening plug 35, and the working principle is as follows: after the buffer motor 25 is started, the connecting rod 32 is driven by each transmission component to reciprocate up and down, in the downward movement process, the upper opening plug 33 is separated from the upper opening 34, the lower opening plug 35 plugs the lower opening 36, and the witherite powder enters the feeding buffer 47 from the upper opening 34; in the upward movement process of the connecting rod 32, the upper opening plug 33 blocks the upper opening 34, the lower opening 36 is opened, and the witherite powder is introduced into the reaction layer 2, so that the reciprocating movement realizes continuous buffer feeding. The device avoids the influence on the reaction rate caused by too fast feeding; under the action of the feeding buffer 47, the witherite powder is continuously and stably fed into the reaction layer 2, so that the reaction rate is remarkably accelerated, and reactants are fully utilized.
The surface of the kettle body 1 is provided with a control panel 12, the surface of the control panel 12 is provided with a timing regulator 38, a main switch 39 and a liquid crystal display screen 37, and the control panel 12 internally comprises a control circuit, a singlechip and a timing module; the control circuit comprises a transformer T, a main switch 39, a first branch circuit, a second branch circuit, a third branch circuit, a fourth branch circuit, a relay U and a protective capacitor; the transformer T is externally connected to a power supply and converts the voltage into a working voltage, and the main switch 39 is used to turn on or off the control circuit. The first branch is connected with a feeding buffer 47 and a first electromagnetic valve 11, and after the main switch 39 is opened, the feeding buffer 47 and the first electromagnetic valve 11 work.
Install the agitator in the cauldron body 1, the agitator includes agitator motor 13 and frame stirring rake 15, and agitator motor 13 installs in the upper end of interlayer 44, and agitator motor 13 even goes out has (mixing) shaft 14, and (mixing) shaft 14 runs through interlayer 44, and (mixing) shaft 14 connects frame stirring rake 15, and frame stirring rake 15 is located reaction layer 2. The stirrer accelerates the reaction rate and improves the generation rate of products. The third branch is connected with a stirring motor 13, and after the main switch 39 is turned on, the stirring motor 13 is started, and the stirrer works.
The method comprises the steps that a first PH value adjusting groove 17 is formed in the left side of a kettle body 1, a third feeding pipe 18 is connected to the first PH value adjusting groove 17, a second electromagnetic valve 19 is connected to the third feeding pipe 18, the third feeding pipe 18 is communicated with a reaction layer 2, a second PH value adjusting groove 20 is formed in the right side of the kettle body 1, a fourth feeding pipe 21 is connected to the second PH value adjusting groove 20, a third electromagnetic valve 22 is connected to the fourth feeding pipe 21, the fourth feeding pipe 21 is communicated with the reaction layer 2, a regulating circuit is connected to a fourth branch and comprises a regulating switch 2, a second electromagnetic valve 19, a third electromagnetic valve 22 and a reverse diode L, the single chip microcomputer controls a regulating switch K2, a regulating switch K2 and the second electromagnetic valve 19 are matched with each other, namely the regulating switch K2 is connected with the second electromagnetic valve 19, the second electromagnetic valve 19 is opened at the moment, the regulating switch K2 and the third electromagnetic valve 22 are matched with each other, namely the regulating switch K2 is connected with the third electromagnetic valve 22, the third electromagnetic valve 22 is opened, the reverse regulating switch K8295 is matched with the reverse diode 8295, namely the pH value of an alkaline solution is connected with the single chip microcomputer, the single chip microcomputer controls the pH value of an alkaline reaction meter to measure the pH value of the alkaline solution, and the alkaline meter is fed back to the pH meter.
The upper end of the reaction layer 2 is provided with an interlayer 44, the first feeding pipe 7, the second feeding pipe 10, the third feeding pipe 18 and the fourth feeding pipe 21 penetrate through the interlayer 44, and the lower ends of the first feeding pipe 7, the second feeding pipe 10, the third feeding pipe 18 and the fourth feeding pipe 21 are communicated with the reaction layer 2. The interlayer 44 isolates the reaction layer 2, thereby preventing the volatilization of hydrochloric acid and avoiding waste.
A filter plate assembly 23 is arranged between the reaction layer 2 and the suction filtration layer 3, the filter plate assembly 23 comprises a suction filter plate 40 and an electric rotary table 43, a suction filtration area 41 is arranged on the suction filter plate 40, a sealing plate 42 is arranged on the electric rotary table 43, and the sealing plate 42 is matched with the suction filtration area 41; the control circuit comprises a timing circuit, a timing module (not marked in the figure) is arranged in the control panel 12, the timing module is connected with the single chip microcomputer, the timing circuit comprises a timing switch K1 and an electric turntable 43, the single chip microcomputer controls the timing switch K1, the timing switch K1 is matched with the electric turntable 43, namely the timing switch K1 can be connected with the electric turntable 43, and the electric turntable 43 is started at the moment. The suction filtration layer 3 is connected with a suction filtration pump 48, the suction filtration pump 48 is arranged on the surface of the kettle body 1, and the electric turntable 43 is connected with the suction filtration pump 48 in series. The filter plate assembly 23 includes a filter plate 40 and an electric turntable 43, a sealing plate 42 is provided on the electric turntable 43, the sealing plate 42 is used for opening and closing the filter area 41, and the specific working principle is as follows: in the reaction process, the control circuit controls the closing plate 42 of the electric turntable 43 to close the pumping region 41, so as to prevent unreacted raw materials from leaking into the pumping layer 3; after the reaction is finished, the timing switch K1 is connected with the electric rotating disc 43, the electric rotating disc 43 is started, the sealing plate 42 opens the suction filtration area 41, the suction filtration pump 48 is started, and suction filtration work is started. The filter plate assembly 23 is matched with the suction pump 48 to complete suction filtration under the control of the timing switch K1, so that the time and labor are saved.
The method for recycling the mixed acid of hydrofluoric acid and hydrochloric acid by adopting the intelligent reaction kettle comprises the following steps:
(1) collecting mixed acid of hydrofluoric acid and hydrochloric acid, taking a proper amount of mixed acid samples, respectively detecting the concentrations of F ions and Cl ions in the mixed acid samples, further analyzing the concentration of the hydrofluoric acid and the concentration of the hydrochloric acid in the samples, and determining the total volume of the hydrofluoric acid and the hydrochloric acid in the mixed acid according to the concentration of the hydrofluoric acid and the concentration of the hydrochloric acid in the samples;
(2) calculating the theoretical usage amount M of the witherite powder according to the concentration of the hydrofluoric acid and the hydrochloric acid and the total volume of the mixed acid in the step (1), and further determining the actual usage amount of the witherite powder to be 1.05M;
(3) adding mixed acid into the reaction layer 2 through a first feeding hole 5, adding witherite powder into a second feeding hopper 9 through a second feeding hole 8, filling sodium bicarbonate into a first pH value adjusting groove 17, and filling low-concentration hydrochloric acid into a second pH value adjusting groove 20;
(4) firstly, setting a reaction time of 2-3h in a timing module of a control panel 12, introducing cooling water into a cooling water jacket, starting a reaction kettle, opening a first electromagnetic valve 11, continuously putting witherite powder into a reaction layer 2, synchronously starting a stirrer, and controlling the stirring speed of the stirrer to be 780 r/min; the reaction equation is as follows:
BaCO3+2HCl=BaCl2+CO2↑+H2O (1)
BaCO3+2HF=BaF2↓+CO2↑+H2O (2)
the pH of the reaction solution was adjusted with sodium bicarbonate and low-concentration hydrochloric acid: when the PH value in the reaction solution measured by the PH meter is too low, the singlechip controls a regulation switch K2 to open the second electromagnetic valve 19, sodium bicarbonate is added until the PH value of the reaction solution measured by the PH meter is normal, and the second electromagnetic valve 19 is closed; when the PH value in the reaction liquid measured by the PH meter is too high, the singlechip controls the regulating switch K2 to open the third electromagnetic valve 22, low-concentration dilute hydrochloric acid is added until the PH value of the reaction liquid measured by the PH meter is normal, and the third electromagnetic valve 22 is closed.
After the reaction is finished, the electric turntable 43 is opened, the suction filtration pump 48 is started to start suction filtration, and filtrate and filter residues are obtained after suction filtration;
(5) opening a first discharge port (not shown in the figure) on the surface of the kettle body 1 to take out filter residues, firstly adding a small amount of hydrochloric acid into the filter residues, filtering again to obtain a crude barium fluoride product, and washing and drying the crude barium fluoride product to obtain a barium fluoride product;
(6) and taking out the filtrate through a second discharge opening 24 at the lower end of the kettle body 1, and removing impurities from the filtrate and refining to obtain a barium chloride aqueous solution product.
The above is only a specific embodiment of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions or modifications made on the basis of the present invention to solve the same technical problems and achieve the same technical effects are all covered in the protection scope of the present invention.

Claims (7)

1. The utility model provides an intelligent reation kettle, includes the cauldron body, the internal reaction layer and the suction filtration layer of including of cauldron, the surface of the cauldron body is equipped with the cooling water jacket, is equipped with water inlet and delivery port, its characterized in that on the cooling water jacket: the upper end of the kettle body is provided with a first feed inlet and a second feed inlet, the lower end of the first feed inlet is connected with a first feed hopper, and the lower end of the first feed hopper is connected with a first feed pipe; the lower end of the second feeding hole is connected with a second feeding hopper, the lower end of the second feeding hopper is connected with a second feeding pipe, and a feeding buffer and a first electromagnetic valve are mounted on the second feeding pipe; the surface of the kettle body is provided with a control panel, a control circuit and a single chip microcomputer are arranged in the control panel, the single chip microcomputer is matched with the control circuit, and the first electromagnetic valve is connected to the control circuit; a filter plate component is arranged between the reaction layer and the suction filtration layer, the filter plate component is connected to the control circuit, a suction filtration pump is connected to the suction filtration layer, the suction filtration pump is mounted on the surface of the kettle body and connected to the control circuit, the feeding buffer comprises an upper opening, a lower opening, a connecting rod and a driving device, an upper opening plug is arranged at the upper end of the connecting rod, a lower opening plug is arranged at the lower end of the connecting rod, the upper opening plug is matched with the upper opening, and the lower opening plug is matched with the lower opening; a driven gear is arranged in the middle of the connecting rod, the driving device comprises a buffer motor, an output rotating shaft, a zone shoulder, a connecting plate, a reciprocating gear and a driving gear, the buffer motor is connected with the output rotating shaft, the output rotating shaft is connected with the zone shoulder, the zone shoulder is connected with the connecting plate, the connecting plate is connected with the reciprocating gear, the reciprocating gear is connected with the driving gear, the driving gear and the driven gear are meshed with each other, a first pH value adjusting groove is formed in the left side of the kettle body, a third feeding pipe is connected to the first pH value adjusting groove, a second electromagnetic valve is connected to the third feeding pipe, and the third feeding pipe is communicated with the reaction layer; a second pH value adjusting groove is formed in the right side of the kettle body, a fourth feeding pipe is connected to the second pH value adjusting groove, a third electromagnetic valve is connected to the fourth feeding pipe, and the fourth feeding pipe is communicated with the reaction layer; the control circuit is connected with a regulating circuit, the regulating circuit comprises a regulating switch, the second electromagnetic valve and the third electromagnetic valve, the single chip microcomputer controls the regulating switch, the regulating switch is matched with the second electromagnetic valve, and the regulating switch is matched with the third electromagnetic valve; and a pH meter is arranged in the reaction layer, and the pH meter is matched with the single chip microcomputer.
2. The intelligent reaction kettle according to claim 1, wherein: the upper end on reaction layer is equipped with the interlayer, first inlet pipe with the second inlet pipe runs through the interlayer, first inlet pipe with the lower extreme intercommunication of second inlet pipe the reaction layer.
3. The intelligent reaction kettle according to claim 2, wherein: the internal agitator of installing of cauldron, the agitator includes agitator motor and frame stirring rake, agitator motor install in the upper end of interlayer, agitator motor even goes out there is the (mixing) shaft, the (mixing) shaft runs through the interlayer, agitator shaft connection the frame stirring rake, the frame stirring rake is located in the reaction layer.
4. The intelligent reaction kettle according to claim 3, wherein: the filter plate assembly comprises a filter plate and an electric turntable, wherein the filter plate is provided with a filter area, the electric turntable is provided with a sealing plate, and the sealing plate is matched with the filter area; the control circuit comprises a timing circuit, a timing module is arranged in the control panel and connected with the single chip microcomputer, the timing circuit comprises a timing switch, the electric turntable and the suction pump, the single chip microcomputer controls the timing switch, the timing switch is matched with the electric turntable, and the electric turntable is connected with the suction pump in series.
5. The method for recycling the mixed acid of hydrofluoric acid and hydrochloric acid by using the intelligent reaction kettle as claimed in claim 4, characterized by comprising the following steps:
(1) collecting mixed acid of hydrofluoric acid and hydrochloric acid, taking a proper amount of mixed acid samples, and respectively analyzing the concentration of the hydrofluoric acid and the concentration of the hydrochloric acid in the samples;
(2) calculating the theoretical usage amount of the witherite powder according to the concentration of the hydrofluoric acid and the hydrochloric acid and the total volume of the mixed acid in the step (1), wherein the actual usage amount of the witherite powder is 1.05 times of the theoretical usage amount of the witherite powder;
(3) adding mixed acid into the reaction layer through the first feed inlet, adding witherite powder into the second feed hopper through the second feed inlet, filling sodium bicarbonate into the first pH value adjusting groove, and filling low-concentration hydrochloric acid into the second pH value adjusting groove;
(4) setting a reaction time of 2-3h in the timing module of the control panel, introducing cooling water into the cooling water jacket, starting the reaction kettle, opening the first electromagnetic valve, continuously feeding witherite powder into the reaction layer, synchronously starting the stirrer, adjusting the pH value of the reaction liquid by using sodium bicarbonate and low-concentration hydrochloric acid, controlling the regulation switch to open the second electromagnetic valve by the singlechip when the pH value in the reaction liquid is too low as measured by the pH meter, adding the sodium bicarbonate until the pH value of the reaction liquid is normal as measured by the pH meter, and closing the second electromagnetic valve; when the pH meter detects that the pH value in the reaction liquid is too high, the singlechip controls the regulating switch to open the third electromagnetic valve, low-concentration dilute hydrochloric acid is added until the pH value of the reaction liquid detected by the pH meter is normal, and the third electromagnetic valve is closed; after the reaction is finished, opening the electric turntable, starting the suction filtration pump, starting suction filtration, and obtaining filtrate and filter residue after suction filtration;
(5) taking out filter residues, and carrying out post-treatment on the filter residues to obtain a barium fluoride product;
(6) and removing impurities from the filtrate and refining to obtain a barium chloride aqueous solution product.
6. The method for recycling mixed hydrofluoric acid and hydrochloric acid in the intelligent reaction kettle according to claim 5, wherein the method comprises the following steps: and (4) controlling the stirring speed of the stirrer to be 500-780 r/min.
7. The method for recycling mixed hydrofluoric acid and hydrochloric acid in the intelligent reaction kettle according to claim 5, wherein the method comprises the following steps: the post-treatment in the step (5) comprises the following specific steps: firstly, adding a small amount of hydrochloric acid into filter residue, filtering again to obtain a crude product of barium fluoride, and washing and drying the crude product to obtain a barium fluoride product.
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