CN106732206A - A kind of recoverying and utilizing method of intelligent reactor and hydrofluoric acid and hydrochloric acid nitration mixture - Google Patents
A kind of recoverying and utilizing method of intelligent reactor and hydrofluoric acid and hydrochloric acid nitration mixture Download PDFInfo
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- CN106732206A CN106732206A CN201611042746.4A CN201611042746A CN106732206A CN 106732206 A CN106732206 A CN 106732206A CN 201611042746 A CN201611042746 A CN 201611042746A CN 106732206 A CN106732206 A CN 106732206A
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- Prior art keywords
- nitration mixture
- magnetic valve
- feed pipe
- hydrochloric acid
- suction filtration
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 108
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000000203 mixture Substances 0.000 title claims abstract description 46
- 238000006396 nitration reaction Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 85
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 82
- 238000000967 suction filtration Methods 0.000 claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 35
- 239000000047 product Substances 0.000 claims abstract description 25
- 229910001632 barium fluoride Inorganic materials 0.000 claims abstract description 14
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 claims abstract description 13
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical group [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 230000001105 regulatory effect Effects 0.000 claims description 46
- 230000001276 controlling effect Effects 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 15
- 239000011229 interlayer Substances 0.000 claims description 14
- 239000010410 layer Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 9
- 239000000872 buffer Substances 0.000 claims description 9
- 239000000498 cooling water Substances 0.000 claims description 9
- 230000005611 electricity Effects 0.000 claims description 8
- 229910052731 fluorine Inorganic materials 0.000 claims description 7
- 239000012043 crude product Substances 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 5
- 230000001186 cumulative effect Effects 0.000 claims description 4
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000012935 Averaging Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 claims description 2
- 230000001360 synchronised effect Effects 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 229910052788 barium Inorganic materials 0.000 claims 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract 1
- 239000012265 solid product Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 239000002253 acid Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 210000004051 gastric juice Anatomy 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/01—Filters 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
- B01D29/03—Filters 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/01—Filters 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
- B01D29/075—Filters 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/22—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00212—Plates; Jackets; Cylinders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00592—Controlling the pH
Landscapes
- 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 a kind of intelligent reactor and the recoverying and utilizing method of hydrofluoric acid and hydrochloric acid nitration mixture, reactor is redesigned so that the reactor that the present invention is used is capable of the recycling of perfect cooperation nitration mixture, time saving and energy saving.Recovery method of the invention is, to witherite powder (barium carbonate) is continuously added in the reactor equipped with nitration mixture, controls pH value and reaction end, and reaction terminates rear suction filtration, and residue washing drying obtains barium fluoride product;It is barium chloride solution product after filtrate impurity removal and purification, the external direct marketing of fluid product can be made, it is also possible to be condensed into solid product for sale.Nitration mixture is processed into two products of barium fluoride and barium chloride by above-mentioned recoverying and utilizing method, is fully used nitration mixture, is turned waste into wealth, while again free from environmental pollution.
Description
Technical field
The present invention relates to chemical field, more particularly, to the recovery of a kind of intelligent reactor and hydrofluoric acid and hydrochloric acid nitration mixture
Application way.
Background technology
Hydrofluoric acid is the aqueous solution of hydrogen fluoride gas, limpid, colourless, smoke corrosive liquids, there is severe irritation gas
Taste.- 83.3 DEG C of fusing point, 112.2 DEG C of boiling point, density 0.888g/cm3.Soluble in water, ethanol, is slightly soluble in ether.Because hydrogen atom
The ability combined and between fluorine atom is relatively strong so that hydrofluoric acid can not be ionized completely in water, so low concentration in theory
Hydrofluoric acid is a kind of weak acid (actually belonging to middle strong acid by its dissociation constant).With extremely strong corrosivity, can consumingly corrode
Metal, glass and siliceous object.Such as suck steam or contact skin can cause to be difficult to cure burns.Due to hydrofluoric acid dissolution
The ability of oxide, it plays an important role in the purification of aluminium and uranium.Hydrofluoric acid is also used for etching glass, can carve figure
Case, mark scale and word;Semi-conductor industry uses it to remove the oxide of silicon face, and it can serve as different in oil plant
The catalyst of the alkylated reaction of butane and n-butene, can also use during " pickling " of the oxygenate impurity for removing stainless steel surfaces
To hydrofluoric acid.Hydrofluoric acid is also used for the synthesis of various organic fluorocompounds, such as Teflon (polytetrafluoroethylene (PTFE)) also has freon one
The refrigerant of class.
Hydrochloric acid, is the aqueous solution of hydrogen chloride, belongs to unitary inorganic strong acid, and industrial use is extensive.The proterties of hydrochloric acid is colourless
Transparent liquid, there is strong sharp aroma, with corrosivity higher.Concentrated hydrochloric acid (mass fraction is about 37%) is with extremely strong
Volatility, therefore fill concentrated hydrochloric acid container open afterchlorinate hydrogen can volatilize, combined generation with the vapor in air
Hydrochloric acid droplet, makes bottleneck top acid mist occur.Hydrochloric acid is the main component of hydrochloric acid in gastric juice, and it can promote food digestion, resist micro-
Biological infection.Hydrochloric acid is colourless liquid (industrial hydrochloric acid can show slightly yellow because there is impurity trivalent iron salt), is corrosive, and is chlorine
Change the aqueous solution of hydrogen, with penetrating odor, concentrated hydrochloric acid is dissolved in water has heat to release.It is dissolved in alkali lye and occurs to neutralize instead with alkali lye
Should.Because concentrated hydrochloric acid has volatility, the hydrogen chloride gas for volatilizing act on forming hydrochloric acid droplet with the vapor in air,
So can be appreciated that white haze.Hydrochloric acid is a kind of inorganic acid, is had a wide range of applications in industrial processes, the refining of such as metal.
Recently as continuing to develop for fluorine chemical industry, the yield of the fluorine product such as fluorinated refrigerant fluoroplastics is increasing.
In its production process, because technique needs, the mixed acid for generating substantial amounts of hydrofluoric acid containing and hydrochloric acid (hereinafter referred to as mixes
Acid).The composition of the mixed acid be hydrofluoric acid 10~40%, hydrochloric acid 3~20%, remaining be water, also a small amount of other impurities.Should
Mixed acid cannot direct marketing, need to by treatment.The current use producer of the nitration mixture is mostly without card underground factory, these producers
Gone to process metal surface with nitration mixture, acid-bearing wastewater is directly discharged in production process, and environmental pollution is extremely serious.Even accredited
Manufacturer discharges after can only also being neutralized to the hydrochloric acid in nitration mixture.
From from the point of view of recycling economy, mixed acid is recycled, with the Acid of Hydrofluoric Acid Production in mixed acid, other are fluorinated
Chemical product, so as to be separated with hydrochloric acid, makes Fluorine contained chemicals and each self-sales of Related product formed by hydrochloric acid.So can both reduce
Substantial amounts of fluorine-containing industrial waste, improves environment, and maximum resource utilization rate can be realized again, production cost is reduced, with obvious society
Can benefit and economic benefit.
The content of the invention
It is an object of the invention to provide a kind of intelligent reactor and the recoverying and utilizing method of hydrofluoric acid and hydrochloric acid nitration mixture,
Using witherite powder (barium carbonate) respectively with nitration mixture in hydrofluoric acid and hydrochloric acid reaction, so as to obtain barium fluoride product and barium chloride
Aqueous products, nitration mixture is utilized completely, is turned waste into wealth, and realizes no pollution, zero-emission.
In order to solve the above-mentioned technical problem, adopt the following technical scheme that:
A kind of intelligent reactor, including kettle, include conversion zone and suction filtration layer in kettle, the surface of kettle is provided with cold
But water leg, cooling water jecket is provided with water inlet and delivery port, it is characterised in that:The upper end of kettle be provided with first charging aperture with
Second charging aperture, the lower end of first charging aperture is connected with the first feed hopper, and the lower end of the first feed hopper is connected with the first feed pipe;
The lower end of second charging aperture is connected with the second feed hopper, and the lower end of the second feed hopper is connected with the second feed pipe, the second feed pipe
On feed surge device and the first magnetic valve are installed;The surface of kettle is provided with control panel, and control electricity is included in control panel
Road and single-chip microcomputer, single-chip microcomputer are mutually matched with control circuit, and the first magnetic valve is connected on control circuit;Conversion zone and suction filtration layer
Between be provided with filter plate assembly, filter plate assembly is connected on control circuit, and suction filter pump is connected with suction filtration layer, and suction filter pump is installed on kettle
The surface of body, suction filter pump is connected on control circuit.
Further, feed surge device includes suitable for reading, lower mouth, connecting rod and drive device, and the upper end of connecting rod is provided with plug suitable for reading, even
The lower end of bar is provided with lower mouth plug, and plug suitable for reading is mutually matched with suitable for reading, and lower mouth plug is mutually matched with lower mouth;The interposition of connecting rod is installed
There is driven gear, drive device includes buffer motor, output revolving shaft, area's shoulder, connecting plate, reciprocating gear and driving gear, delays
Device motor connection output revolving shaft is rushed, output revolving shaft bonding pad shoulder, area's shoulder connection connecting plate, connecting plate connects reciprocating gear, back and forth
Gear connects driving gear, touches gear and is intermeshed with driven gear.Feed surge device is buffered by plug suitable for reading and lower mouth plug
The feed rate of witherite powder, it is to avoid charging influences reaction rate very much soon;In the presence of feed surge device, witherite powder connects
It is continuous, stabilization to be delivered to conversion zone, reaction rate is dramatically speeded up, reactant is fully utilized.
Further, the upper end of conversion zone is provided with interlayer, and the first feed pipe and the second feed pipe run through interlayer, the first feed pipe
Lower end with the second feed pipe connects conversion zone.Interlayer completely cuts off conversion zone, prevents hydrochloric acid from volatilizing, it is to avoid waste.
Further, agitator is installed, agitator includes stirring motor and frame type agitating blade, and stirring motor is installed in kettle
In the upper end of interlayer, stirring motor has connected agitating shaft, and agitating shaft runs through interlayer, and agitating shaft connection frame type agitating blade, frame is stirred
Oar is mixed to be located in conversion zone.Agitator accelerates reaction rate, lifts the production rate of product.
Further, the first pH value regulating tank is provided with the left of kettle, the 3rd feed pipe is connected with the first pH value regulating tank,
The second magnetic valve, the 3rd feed pipe connection conversion zone are connected with 3rd feed pipe;The regulation of the second pH value is provided with the right side of kettle
Groove, is connected with the 4th feed pipe on the second pH value regulating tank, the 3rd magnetic valve is connected with the 4th feed pipe, and the 4th feed pipe connects
Logical conversion zone;Circuit for regulating and controlling is connected with control circuit, circuit for regulating and controlling includes regulating switch, the second magnetic valve and the 3rd electromagnetism
Valve, Single-chip Controlling regulating switch, regulating switch is mutually matched with the second magnetic valve, regulating switch and mutual of the 3rd magnetic valve
Match somebody with somebody;PH meters are installed, PH meters are mutually matched with single-chip microcomputer in conversion zone.
Further, filter plate assembly includes suction filtration plate and electric rotating disk, and suction filtration plate is provided with suction filtration area, and electric rotating disk is provided with envelope
Plate, shrouding is mutually matched with suction filtration area;Control circuit includes timing circuit, and time block, timing mould are provided with control panel
Block connects single-chip microcomputer, and timing circuit includes time switch and electric rotating disk, Single-chip Controlling time switch, time switch and electric rotating disk
It is mutually matched, electric rotating disk and suction filtration series connection of pumps.
The method that hydrofluoric acid and hydrochloric acid nitration mixture are recycled using intelligent reactor, it is characterised in that including following step
Suddenly:
(1) nitration mixture of hydrofluoric acid and hydrochloric acid is collected, appropriate nitration mixture sample is taken, hydrofluoric acid concentration and salt in sample is analyzed respectively
Acid concentration;
(2) according to hydrofluoric acid in step (1) and the cumulative volume of concentration of hydrochloric acid and nitration mixture, theoretical witherite powder consumption is calculated,
Actual witherite powder consumption is 1.05 times of theoretical witherite powder consumption;
(3) nitration mixture is added in conversion zone by first charging aperture, witherite powder is added to by second charging aperture
In two feed hoppers, sodium acid carbonate is filled in the first pH value regulating tank, low-concentration hcl is filled in the second pH value regulating tank;
(4) reaction time of 2-3h is set first in the time block of control panel, it is cold to being passed through in cold water water leg
But water, restarts reactor, and the first magnetic valve is opened, and witherite powder is continuously put into conversion zone, agitator synchronous averaging, by
Sodium acid carbonate adjusts the pH value of reaction solution with low-concentration hcl;After reaction terminates, electric rotating disk is opened, and suction filtration pump startup starts to take out
Filter, obtains filtrate and filter residue after suction filtration;
(5) filter residue is taken out, filter residue obtains barium fluoride product after treatment;
(6) barium chloride solution product is obtained after filtrate impurity removal and purification.
It is preferred that after, the stir speed (S.S.) that agitator is controlled in step (3) is 500-780r/min.
It is preferred that after, regulation pH value concretely comprises the following steps in step (3):PH meters measure pH value in reaction solution it is too low when,
Single-chip Controlling regulating switch opens the second magnetic valve, adds sodium acid carbonate, until PH meters measure reaction solution pH value normally,
Close the second magnetic valve;PH meters measure pH value in reaction solution it is too high when, Single-chip Controlling regulating switch opens the 3rd electromagnetism
Valve, adds low concentration watery hydrochloric acid, until PH meters measure reaction solution pH value normally, closes the 3rd magnetic valve.
It is preferred that after, post processing concretely comprises the following steps in step (5):A small amount of hydrochloric acid is added in filter residue first, is filtered again
After obtain barium fluoride crude product, obtain barium fluoride product after the scrubbed drying of crude product.
Due to using upper technical scheme, have the advantages that:
The present invention is a kind of intelligent reactor and the recoverying and utilizing method of hydrofluoric acid and hydrochloric acid nitration mixture, using witherite powder
(barium carbonate) respectively with nitration mixture in hydrofluoric acid and hydrochloric acid reaction, so as to obtain barium fluoride product and barium chloride solution product,
Nitration mixture is utilized completely, is turned waste into wealth, realize no pollution, zero-emission.Its specific beneficial effect show as it is following some:
1st, the second feed hopper, second charging aperture and the second feed pipe collocation is used, and the second feed hopper volume is big, can accommodate
Substantial amounts of witherite powder is time saving and energy saving without repeatedly addition;Continuous, uninterrupted addition witherite powder is realized, promotes reaction.
2nd, feed surge device buffers the feed rate of witherite powder by plug suitable for reading with lower mouth plug, and operation principle is as follows:It is slow
After rushing device electric motor starting, by each upper and lower reciprocating motion of drive disk assembly drivening rod, during moving downward, plug suitable for reading is de-
From suitable for reading, the lower lower mouth of mouth plug closure, witherite powder is by entrance feed surge device suitable for reading;It is suitable for reading in the upward motion process of connecting rod
Plug closure is suitable for reading, and lower mouth is opened, and witherite powder is passed through in conversion zone, and continuous buffering charging is realized in and so on motion.The device
Avoid charging too fast and influence reaction rate;In the presence of feed surge device, witherite powder is continuous, stabilization to conversion zone throwing
Put, dramatically speed up reaction rate, reactant is fully utilized.
3rd, the first magnetic valve is connected on control circuit, controls the first magnetic valve to open and close by controlling circuit, so as to control
Witherite powder feeds, and simple structure is practical.
4th, filter plate assembly includes suction filtration plate and electric rotating disk, and electric rotating disk is provided with shrouding, and shrouding is used to switch or close suction filtration
Area, concrete operating principle is as follows:During the course of the reaction, the shrouding closure suction filtration area of the electric rotating disk of control circuit control, prevents not anti-
The raw material answered is leaked into suction filtration layer;After reaction terminates, the electric rotating disk of time switch connection, electric rotating disk starts, door open structure suction filtration
Area, suction filtration pump startup starts suction filtration work.Filter plate assembly coordinates suction filter pump to complete suction filtration work under the control of time switch,
It is time saving and energy saving.
5th, the present invention recycles nitration mixture using witherite powder, and nitration mixture is processed into two products of barium fluoride and barium chloride,
Nitration mixture is utilized completely.Substantial amounts of fluorine-containing industrial waste so can be both reduced, had improved environment, can realize that maximum resource was utilized again
Rate, reduces production cost, with obvious Social benefit and economic benefit.
Brief description of the drawings
The invention will be further described below in conjunction with the accompanying drawings:
Fig. 1 is a kind of structural representation of intelligent reactor in the present invention;
Fig. 2 is the structural representation of feed surge device in the present invention;
Fig. 3 is the structural representation of control panel in the present invention;
Fig. 4 is the structural representation of filter plate assembly in the present invention;
Fig. 5 is electric operation control circuit figure in the present invention;
Fig. 6 is the timing circuit part in Fig. 5;
Fig. 7 is the circuit for regulating and controlling part in Fig. 5.
Wherein, T is transformer in Fig. 5, and K is master switch, and M1 is buffer motor, PV1 is the first magnetic valve, and M2 is stirring
Motor, U is relay, and C1, C2, C3 are protection electric capacity;K1 is time switch in Fig. 6, and PV2 is electric rotating disk, and PV3 is suction filtration
Pump;K2 is regulating switch in Fig. 7, and PV4 is the second magnetic valve, and PV5 is the 3rd magnetic valve, and L is backward dioded.
Specific embodiment
Invention describes a kind of intelligent reactor and the recoverying and utilizing method of hydrofluoric acid and hydrochloric acid nitration mixture, using poison weight
Stone flour (barium carbonate) respectively with nitration mixture in hydrofluoric acid and hydrochloric acid reaction, so as to obtain barium fluoride product and barium chloride solution produce
Product, nitration mixture is utilized completely.
Conversion zone 2 and suction filtration layer 3 are provided with a kind of intelligent reactor, including kettle 1, kettle 1, raw material is in conversion zone 2
In reacted, product suction filtration layer 3 in suction filtration.The surface of kettle 1 is provided with cooling water jecket 4, and nitration mixture reacts with witherite powder
During can produce substantial amounts of heat, generally cold water is continuously injected into cooling water jecket 4 to remove the big calorimetric in conversion zone 2
Amount.Cooling water jecket 4 is provided with water inlet 45 and delivery port 46, and the connection water inlet pipe of water inlet 45, delivery port 46 connects outlet pipe,
Realization is continuously injected into cooling water, is obviously improved the effect that cools.
The upper end of kettle 1 is provided with first charging aperture 5 and second charging aperture 8, and the lower end of first charging aperture 5 is connected with first and enters
Hopper 6, the lower end of the first feed hopper 6 is connected with the first feed pipe 7, and the connection conversion zone 2 of the first feed pipe 7, nitration mixture passes through first
In charging aperture 5, the first feed hopper 6 and the first feed pipe 7 input conversion zone 2.The lower end of second charging aperture 8 is connected with the second charging
Bucket 9, the lower end of the second feed hopper 9 is connected with the second feed pipe 10, and feed surge device 47 and the are provided with the second feed pipe 10
One magnetic valve 11, witherite powder is put into conversion zone 2 by second charging aperture 8, the second feed hopper 9 and the second feed pipe 10.The
Two feed hoppers 9, the collocation of 8 and second feed pipe of second charging aperture 10 are used, and the volume of the second feed hopper 9 is big, can accommodate substantial amounts of
Witherite powder is time saving and energy saving without repeatedly addition;Continuous, uninterrupted addition witherite powder is realized, promotes reaction.
Feed surge device 47 includes suitable for reading 34, lower mouth 36, connecting rod 32 and drive device, and the upper end of connecting rod 32 is provided with plug suitable for reading
33, the lower end of connecting rod 32 is provided with lower mouth plug 35, and plug 33 suitable for reading is mutually matched with suitable for reading 34, mutual of lower mouth plug 35 and lower mouth 36
Match somebody with somebody;The centre position of connecting rod 32 is provided with driven gear 31, drive device include buffer motor 25, output revolving shaft 26, area's shoulder 27,
Connecting plate 28, reciprocating gear 29 and driving gear 30, the connection output revolving shaft 26 of buffer motor 25, the bonding pad shoulder of output revolving shaft 26
27, the connection connecting plate 28 of area's shoulder 27, the connection reciprocating gear 29 of connecting plate 28, the connection driving gear 30 of reciprocating gear 29 touches tooth
Wheel is intermeshed with driven gear 31.Feed surge device 47 is fast with the charging of lower mouth plug 35 buffering witherite powder by plug 33 suitable for reading
Rate, operation principle is as follows:After buffer motor 25 starts, by each upper and lower reciprocating motion of drive disk assembly drivening rod 32, to
In lower motion process, plug 33 suitable for reading departs from suitable for reading 34, and the lower lower mouth 36 of the closure of mouth plug 35, witherite powder is slow into charging by suitable for reading 34
Rush in device 47;In the upward motion process of connecting rod 32, the closure of plug 33 suitable for reading 34 suitable for reading, lower mouth 36 is opened, and witherite powder is passed through reaction
In layer 2, continuous buffering charging is realized in and so on motion.The device avoids charging too fast and influences reaction rate;It is slow in charging
Rush in the presence of device 47, witherite powder is continuous, it is stabilization delivered to conversion zone 2, dramatically speed up reaction rate, reactant is abundant
Utilize.
The surface of kettle 1 is provided with control panel 12, and the surface of control panel 12 is provided with timing governor 38, master switch 39 and
Control circuit, single-chip microcomputer and time block are included in LCDs 37, control panel 12;Control circuit include transformer T,
Master switch 39, tie point, the second branch road, the 3rd branch road, the 4th branch road, relay U and protection electric capacity;The external electricity of transformer T
Source, and be operating voltage by photovoltaic conversion, master switch 39 is used to be turned on and off controlling circuit.Charging is connected with tie point
The magnetic valve 11 of buffer 47 and first, after master switch 39 is opened, feed surge device 47 works with the first magnetic valve 11.
Agitator is installed, agitator includes stirring motor 13 and frame type agitating blade 15, and stirring motor 13 is installed in kettle 1
In the upper end of interlayer 44, stirring motor 13 has connected agitating shaft 14, and agitating shaft 14 runs through interlayer 44, and the connection frame of agitating shaft 14 is stirred
Oar 15 is mixed, frame type agitating blade 15 is located in conversion zone 2.Agitator accelerates reaction rate, lifts the production rate of product.3rd branch road
Upper connection stirring motor 13, after master switch 39 is opened, stirring motor 13 starts, agitator work.
The left side of kettle 1 is provided with the first pH value regulating tank 17, and the 3rd feed pipe 18 is connected with the first pH value regulating tank 17,
The second magnetic valve 19, the connection conversion zone 2 of the 3rd feed pipe 18 are connected with 3rd feed pipe 18;The right side of kettle 1 is provided with second
PH value regulating tank 20, is connected with the 4th feed pipe 21 on the second pH value regulating tank 20, the 3rd electricity is connected with the 4th feed pipe 21
Magnet valve 22, the connection conversion zone 2 of the 4th feed pipe 21;Circuit for regulating and controlling is connected with 4th branch road, circuit for regulating and controlling includes regulating switch
K2, the second magnetic valve 19, the 3rd magnetic valve 22 and backward dioded L, Single-chip Controlling regulating switch K2, regulating switch K2 and
Two magnetic valves 19 are mutually matched, i.e. regulating switch K2 can connect the second magnetic valve 19, and now the second magnetic valve 19 is opened;Regulation and control are opened
Close K2 to be mutually matched with the 3rd magnetic valve 22, i.e., regulating switch K2 can connect the 3rd magnetic valve 22, now the 3rd magnetic valve 22 dozens
Open;Regulating switch K2 is mutually matched with backward dioded L, i.e., regulating switch K2 can connect backward dioded L, now the second electromagnetism
Valve 19 is turned off with the 3rd magnetic valve 22.PH meters are installed in conversion zone 2, PH meters are mutually matched with single-chip microcomputer, PH
Meter measures the pH value of reaction solution, and amount pH value fed back into single-chip microcomputer, single-chip microcomputer judge reaction solution whether peracid or mistake alkali,
Regulating switch K2 is controlled on this basis, so that the pH value of the regulation and control reaction solution of intelligence.
The upper end of conversion zone 2 is provided with interlayer 44, and the first feed pipe 7, the second feed pipe 10, the 3rd feed pipe 18 enter with the 4th
Expects pipe 21 runs through interlayer 44, and the lower end of the first feed pipe 7, the second feed pipe 10, the 3rd feed pipe 18 and the 4th feed pipe 21 connects
Logical conversion zone 2.Interlayer 44 completely cuts off conversion zone 2, prevents hydrochloric acid from volatilizing, it is to avoid waste.
Filter plate assembly 23 is provided between conversion zone 2 and suction filtration layer 3, filter plate assembly 23 includes suction filtration plate 40 and electric rotating disk 43,
Suction filtration plate 40 is provided with suction filtration area 41, and electric rotating disk 43 is provided with shrouding 42, and shrouding 42 is mutually matched with suction filtration area 41;Control circuit
Include and time block (not marked in figure) is provided with timing circuit, control panel 12, time block connection single-chip microcomputer, timing electricity
Road includes time switch K1 and electric rotating disk 43, and Single-chip Controlling time switch K1, time switch K1 are mutually matched with electric rotating disk 43,
I.e. time switch K1 can connect electric rotating disk 43, and now electric rotating disk 43 starts.Suction filter pump 48, suction filter pump 48 are connected with suction filtration layer 3
The surface of kettle 1 is installed on, electric rotating disk 43 is connected with suction filter pump 48.Filter plate assembly 23 includes suction filtration plate 40 and electric rotating disk 43, electricity
Rotating disk 43 is provided with shrouding 42, and shrouding 42 is used to switch or close suction filtration area 41, and concrete operating principle is as follows:In course of reaction
In, the closure suction filtration of shrouding 42 area 41 of the electric rotating disk 43 of control circuit control prevents unreacted raw material from leaking into suction filtration layer 3;
After reaction terminates, the electric rotating disk 43 of time switch K1 connections, electric rotating disk 43 starts, and shrouding 42 opens suction filtration area 41, and suction filter pump 48 is opened
It is dynamic, start suction filtration work.Filter plate assembly 23 coordinates suction filter pump 48 to complete suction filtration work under the control of time switch K1, time saving
It is laborsaving.
The method that hydrofluoric acid and hydrochloric acid nitration mixture are recycled using intelligent reactor, is comprised the following steps:
(1) nitration mixture of hydrofluoric acid and hydrochloric acid is collected, appropriate nitration mixture sample is taken, F ion and Cl in nitration mixture sample is detected respectively
The concentration of ion, and then hydrofluoric acid concentration and concentration of hydrochloric acid in sample are analyzed, according to hydrofluoric acid concentration in sample and concentration of hydrochloric acid
Determine the cumulative volume of hydrofluoric acid and hydrochloric acid in nitration mixture;
(2) according to hydrofluoric acid in step (1) and the cumulative volume of concentration of hydrochloric acid and nitration mixture, theoretical witherite powder consumption M is calculated,
And then determine actual witherite powder consumption 1.05M;
(3) nitration mixture is added in conversion zone 2 by first charging aperture 5, witherite powder is added to by second charging aperture 8
In second feed hopper 9, sodium acid carbonate is filled in the first pH value regulating tank 17, low concentration is filled in the second pH value regulating tank 20
Hydrochloric acid;
(4) reaction time of 2-3h is set first in the time block of control panel 12, to being passed through in cold water water leg
Cooling water, restarts reactor, and the first magnetic valve 11 is opened, and witherite powder is continuously put into conversion zone 2, and agitator is synchronously opened
Dynamic, the stir speed (S.S.) for controlling agitator is 500-780r/min;Its reaction equation is as follows:
BaCO3+ 2HCl=BaCl2+CO2↑+H2O (1)
BaCO3+ 2HF=BaF2↓+CO2↑+H2O (2)
The pH value of reaction solution is adjusted by sodium acid carbonate and low-concentration hcl:PH value is too low during PH meters measure reaction solution
When, Single-chip Controlling regulating switch K2 opens the second magnetic valve 19, sodium acid carbonate is added, until PH meters measure reaction solution PH
Value is normal, closes the second magnetic valve 19;PH meters measure pH value in reaction solution it is too high when, Single-chip Controlling regulating switch K2 beats
The 3rd magnetic valve 22 is driven, low concentration watery hydrochloric acid is added, until PH meters measure reaction solution pH value normally, the 3rd magnetic valve is closed
22。
After reaction terminates, electric rotating disk 43 is opened, and suction filter pump 48 starts, and starts suction filtration, and filtrate and filter residue are obtained after suction filtration;
(5) the first discharge port (not marked in figure) for opening the surface of kettle 1 takes out filter residue, is added first in filter residue a small amount of
Hydrochloric acid, barium fluoride crude product is obtained after filtering again, and barium fluoride product is obtained after the scrubbed drying of crude product;
(6) filtrate is taken out by second discharge port 24 of the lower end of kettle 1, barium chloride solution is obtained after filtrate impurity removal and purification
Product.
Specific embodiment of the invention is these are only, but technical characteristic of the invention is not limited thereto.It is any with this hair
It is to solve essentially identical technical problem based on bright, realizes essentially identical technique effect, done ground simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (10)
1. a kind of intelligent reactor, including kettle, includes conversion zone and suction filtration layer, the surface of the kettle in the kettle
Cooling water jecket is provided with, cooling water jecket is provided with water inlet and delivery port, it is characterised in that:The upper end of the kettle is provided with
One charging aperture and second charging aperture, the lower end of the first charging aperture are connected with the first feed hopper, under first feed hopper
End is connected with the first feed pipe;The lower end of the second charging aperture is connected with the second feed hopper, the lower end of second feed hopper
The second feed pipe is connected with, feed surge device and the first magnetic valve are installed on second feed pipe;The surface of the kettle
Control panel is provided with, control circuit and single-chip microcomputer, the single-chip microcomputer and the control circuit phase are included in the control panel
Mutually matching, first magnetic valve is connected on the control circuit;Filter plate is provided between the conversion zone and suction filtration layer
Component, the filter plate assembly is connected on the control circuit, and suction filter pump is connected with the suction filtration layer, and the suction filter pump is installed
In the surface of the kettle, the suction filter pump is connected on the control circuit.
2. a kind of intelligent reactor according to claim 1, it is characterised in that:The feed surge device include it is suitable for reading, under
Mouth, connecting rod and drive device, the upper end of the connecting rod are provided with plug suitable for reading, and the lower end of the connecting rod is provided with lower mouth plug, described suitable for reading
Plug with it is described it is suitable for reading be mutually matched, the lower mouth plug is mutually matched with the lower mouth;The centre position of the connecting rod is provided with driven
Gear, the drive device includes buffer motor, output revolving shaft, area's shoulder, connecting plate, reciprocating gear and driving gear, described
Output revolving shaft described in buffer motor connection, the output revolving shaft connects area's shoulder, and area's shoulder connects the connecting plate, institute
State connecting plate and connect the reciprocating gear, the reciprocating gear connects the driving gear, and the shake-up gear is driven with described
Gear is intermeshed.
3. a kind of intelligent reactor according to claim 1, it is characterised in that:The upper end of the conversion zone is provided with interlayer,
First feed pipe and second feed pipe run through the interlayer, under first feed pipe and second feed pipe
The end connection conversion zone.
4. a kind of intelligent reactor according to claim 3, it is characterised in that:Agitator, institute are installed in the kettle
Stating agitator includes stirring motor and frame type agitating blade, and the stirring motor is installed on the upper end of the interlayer, the stirring electricity
Machine has connected agitating shaft, and the agitating shaft runs through the interlayer, and the agitating shaft connects the frame type agitating blade, and the frame is stirred
Oar is mixed to be located in the conversion zone.
5. a kind of intelligent reactor according to claim 1, it is characterised in that:The first pH value is provided with the left of the kettle
Regulating tank, is connected with the 3rd feed pipe on the first pH value regulating tank, the second magnetic valve is connected with the 3rd feed pipe,
3rd feed pipe connects the conversion zone;The second pH value regulating tank is provided with the right side of the kettle, second pH value is adjusted
The 4th feed pipe is connected with section groove, the 3rd magnetic valve is connected with the 4th feed pipe, the 4th feed pipe connects institute
State conversion zone;Circuit for regulating and controlling is connected with the control circuit, the circuit for regulating and controlling includes regulating switch, second magnetic valve
With the 3rd magnetic valve, regulating switch described in the Single-chip Controlling, the regulating switch is mutual with second magnetic valve
Matching, the regulating switch is mutually matched with the 3rd magnetic valve;PH meters are installed, the PH is surveyed in the conversion zone
Gauge is mutually matched with the single-chip microcomputer.
6. a kind of intelligent reactor according to claim 1, it is characterised in that:The filter plate assembly includes suction filtration plate and electricity
Rotating disk, the suction filtration plate is provided with suction filtration area, and the electric rotating disk is provided with shrouding, mutual of the shrouding and the suction filtration area
Match somebody with somebody;The control circuit includes timing circuit, and time block is provided with the control panel, and the time block connection is described
Single-chip microcomputer, the timing circuit includes time switch, the electric rotating disk and the suction filter pump, timing described in the Single-chip Controlling
Switch, the time switch is mutually matched with the electric rotating disk, the electric rotating disk and the suction filtration series connection of pumps.
7. the method for hydrofluoric acid and hydrochloric acid nitration mixture being recycled using intelligent reactor as claimed in claim 1, its feature
It is to comprise the following steps:
(1) nitration mixture of hydrofluoric acid and hydrochloric acid is collected, appropriate nitration mixture sample is taken, hydrofluoric acid concentration is dense with hydrochloric acid in analyzing sample respectively
Degree;
(2) according to hydrofluoric acid in step (1) and the cumulative volume of concentration of hydrochloric acid and nitration mixture, theoretical witherite powder consumption is calculated, it is actual
Witherite powder consumption is 1.05 times of theoretical witherite powder consumption;
(3) nitration mixture is added in the conversion zone by the first charging aperture, witherite powder is by the second charging aperture
It is added in second feed hopper, sodium acid carbonate is filled in the first pH value regulating tank, is filled in the second pH value regulating tank
Low-concentration hcl;
(4) reaction time of 2-3h is set first in the time block of the control panel, to the cold water water leg
Cooling water is inside passed through, restarts reactor, first magnetic valve is opened, and witherite powder is continuously put into the conversion zone, institute
Agitator synchronous averaging is stated, the pH value of reaction solution is adjusted by sodium acid carbonate and low-concentration hcl;After reaction terminates, the electricity turns
Disk is opened, the suction filtration pump startup, starts suction filtration, and filtrate and filter residue are obtained after suction filtration;
(5) filter residue is taken out, barium fluoride product is obtained after filter residue is post-treated;
(6) barium chloride solution product is obtained after filtrate impurity removal and purification.
8. the method that intelligent reactor recycles hydrofluoric acid and hydrochloric acid nitration mixture according to claim 7, it is characterised in that:
The stir speed (S.S.) that the agitator is controlled in the step (4) is 500-780r/min.
9. the method that intelligent reactor recycles hydrofluoric acid and hydrochloric acid nitration mixture according to claim 7, it is characterised in that:
Regulation pH value concretely comprises the following steps in the step (4):The PH meters measure pH value in reaction solution it is too low when, the monolithic
Machine controls the regulating switch to open second magnetic valve, sodium acid carbonate is added, until PH meters measure reaction solution pH value
Normally, second magnetic valve is closed;The PH meters measure pH value in reaction solution it is too high when, described in the Single-chip Controlling
Regulating switch opens the 3rd magnetic valve, adds low concentration watery hydrochloric acid, until PH meters measure reaction solution pH value normally, closes
Close the 3rd magnetic valve.
10. the method that intelligent reactor recycles hydrofluoric acid and hydrochloric acid nitration mixture according to claim 7, its feature exists
In:Post processing concretely comprises the following steps in the step (5):A small amount of hydrochloric acid is added in filter residue first, fluorine is obtained after filtering again
Change barium crude product, barium fluoride product is obtained after the scrubbed drying of crude product.
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CN107020061A (en) * | 2017-06-02 | 2017-08-08 | 江苏中天科技股份有限公司 | A kind of mini-plant of silicium cathode material strong acid alkali process |
CN109179327A (en) * | 2018-09-25 | 2019-01-11 | 李晓垚 | A kind of food grade salt acid production process |
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CN205269612U (en) * | 2015-09-11 | 2016-06-01 | 福建紫荆环境工程技术有限公司 | A acidleach oxidation reation kettle for $discarding SCR denitration catalyst comprehensive recovery utilization |
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CN107020061A (en) * | 2017-06-02 | 2017-08-08 | 江苏中天科技股份有限公司 | A kind of mini-plant of silicium cathode material strong acid alkali process |
CN109179327A (en) * | 2018-09-25 | 2019-01-11 | 李晓垚 | A kind of food grade salt acid production process |
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