CN215667169U - High-purity octahydrate barium hydroxide purification production system - Google Patents
High-purity octahydrate barium hydroxide purification production system Download PDFInfo
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- CN215667169U CN215667169U CN202122433086.5U CN202122433086U CN215667169U CN 215667169 U CN215667169 U CN 215667169U CN 202122433086 U CN202122433086 U CN 202122433086U CN 215667169 U CN215667169 U CN 215667169U
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- ZUDYPQRUOYEARG-UHFFFAOYSA-L barium(2+);dihydroxide;octahydrate Chemical compound O.O.O.O.O.O.O.O.[OH-].[OH-].[Ba+2] ZUDYPQRUOYEARG-UHFFFAOYSA-L 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 238000000746 purification Methods 0.000 title claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 42
- 230000008025 crystallization Effects 0.000 claims abstract description 42
- 239000012452 mother liquor Substances 0.000 claims abstract description 23
- 238000004806 packaging method and process Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000012546 transfer Methods 0.000 claims abstract description 14
- 239000002562 thickening agent Substances 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 239000013078 crystal Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 16
- 239000011229 interlayer Substances 0.000 claims description 15
- 229910052712 strontium Inorganic materials 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 13
- 238000011010 flushing procedure Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 10
- 239000000428 dust Substances 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 8
- 238000011001 backwashing Methods 0.000 claims description 6
- 239000007790 solid phase Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 11
- 238000010924 continuous production Methods 0.000 abstract 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 22
- 229910001863 barium hydroxide Inorganic materials 0.000 description 22
- 239000000243 solution Substances 0.000 description 18
- 239000012535 impurity Substances 0.000 description 16
- 239000007787 solid Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 10
- IVZJIPHAJINUAE-UHFFFAOYSA-N barium;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Ba] IVZJIPHAJINUAE-UHFFFAOYSA-N 0.000 description 9
- 238000001953 recrystallisation Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 6
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 6
- 229910001424 calcium ion Inorganic materials 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 229910001427 strontium ion Inorganic materials 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- -1 fluoride ions Chemical class 0.000 description 5
- 239000010413 mother solution Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000032258 transport Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- SKDCSNGKKUNRQJ-UHFFFAOYSA-M O.O.O.O.O.O.O.O.[OH-].[Li+] Chemical compound O.O.O.O.O.O.O.O.[OH-].[Li+] SKDCSNGKKUNRQJ-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 159000000009 barium salts Chemical class 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 150000004689 octahydrates Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 description 1
- 229910001637 strontium fluoride Inorganic materials 0.000 description 1
- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The utility model discloses a high-purity barium hydroxide octahydrate purification production system, which belongs to the technical field of barium hydroxide octahydrate purification, and comprises a raw material bin, a mother liquor tank, a dissolving tank, a precision filter, a transfer tank, a DTB (draw texturing yarn) crystallization system, a thickener, a centrifugal separator, a dryer, an airflow crusher and an automatic packaging machine which are sequentially communicated, wherein the whole processing continuous process is completed in a closed system, the production process is completed in the closed system, the efficiency is improved, and the whole operation process is safer.
Description
Technical Field
The utility model relates to the technical field of barium hydroxide octahydrate purification, in particular to a high-purity barium hydroxide octahydrate purification production system.
Background
Ba (OH)2.8H2O octahydrate is an important raw material for chemical industry, and is used as multi-effect additive in petroleum industry, barium-base grease and stabilizer for refining oil and producing plastics. Wherein the high-quality barium hydroxide octahydrate is mainly used for the production of high-purity barium titanate by a hydrothermal method and experimental application.
The conventional production process of high-quality pure barium hydroxide octahydrate usually adopts physical filtration, lacks a soluble ion removal means and has low product purity. The single-tank intermittent operation is adopted, the operation frequency is high, and the relative labor intensity of workers is high. Barium hydroxide is toxic, leakage in the device and steam entrainment, and is extremely easy to harm the health of workers.
Based on solving the problems, technical research and experiments are carried out, and the high-purity barium hydroxide octahydrate purification production system and method are developed.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a high-purity octahydrate barium hydroxide purification production system which has the advantages of improving purification efficiency and being safer to operate.
In order to achieve the purpose, the utility model adopts the technical scheme that:
a high-purity barium hydroxide octahydrate purification production system comprises a raw material bin, a mother liquor tank, a dissolving tank, a precision filter, a transfer tank, a DTB crystallization system, a thickener, a centrifugal separator, a dryer, a pneumatic crusher and an automatic packaging machine which are sequentially communicated,
wherein the raw material bin is communicated with the welding tank through a metering belt, the mother liquid tank, the dissolving tank, the precision filter, the transit tank, the DTB crystallization system, the thickener, the centrifugal separator, the dryer, the airflow crusher and the automatic packaging machine are sequentially communicated through pipelines,
the top end of the dissolving tank is provided with a feed inlet for receiving materials output by a metering belt, the top end of the dissolving tank is connected with a strontium removal agent storage tank through a pipeline, the top end of the dissolving tank is also communicated with a mother liquor tank through a pipeline for conveying mother liquor into the dissolving tank to dissolve raw materials in the dissolving tank, and the pipeline is provided with a pump body and a valve for controlling normal transportation of the materials;
the dissolving tank comprises a first-stage dissolving tank and a second-stage dissolving tank, a feed inlet is formed in the top end of the first-stage dissolving tank, a strontium removal agent storage tank is communicated with the first-stage dissolving tank, the output end of the first-stage dissolving tank and the output end of the second-stage dissolving tank are connected with the input end of a precision filter through a pipeline, an overflow outlet is formed in the side wall of the first-stage dissolving tank, an overflow inlet is formed in the side wall of the second-stage dissolving tank, the overflow outlet is communicated with the overflow inlet, and the height of the overflow inlet is not higher than that of the overflow outlet.
Preferably, the lateral walls of the first-stage dissolving tank and the second-stage dissolving tank are provided with interlayers, and the lateral walls of the first-stage dissolving tank and the second-stage dissolving tank are provided with a steam inlet for introducing steam into the interlayers and a condensed water outlet for allowing condensed water in the interlayers to flow out.
Preferably, the side wall of the precision filter is provided with an interlayer, and the side wall of the precision filter is provided with a steam inlet for introducing steam into the interlayer and a condensate outlet for allowing condensate in the interlayer to flow out.
Preferably, a coiled pipe is arranged in the transfer tank, one end of the coiled pipe is used for steam to enter, and the other end of the coiled pipe is used for condensed water to discharge.
Preferably, the side wall of the precision filter is communicated with a back flushing pipeline and a positive flushing pipeline;
a back washing water inlet pipe and a back blowing nitrogen inlet pipe are communicated with the back washing pipeline, and valves are arranged on the back washing water inlet pipe and the back blowing nitrogen inlet pipe;
the positive flushing pipeline is communicated with a positive flushing water inlet pipe and a positive nitrogen-blowing gas inlet pipe, and valves are arranged on the positive flushing water inlet pipe and the positive nitrogen-blowing gas inlet pipe.
Preferably, the DTB crystallization system comprises a DTB crystallizer, a crystallization cooler, a crystallization circulating pump, a crystal extraction pump and a liquid outlet pump;
the bottom of the DTB crystallizer is connected with a crystallization circulating pump through a pipeline, the output end of the crystallization circulating pump is communicated with the input end of a crystallization cooler, the output end of a transit tank is communicated with the input end of the crystallization cooler through a pipeline, the output end of the crystallization cooler is communicated with the input end of the DTB crystallizer through a pipeline, the bottom of the DTB crystallizer is communicated with a thickener through a pipeline, and a crystal extraction pump is arranged on the pipeline.
Preferably, a clear liquid overflow pipe is communicated with the side wall of the thickener, the other end of the clear liquid overflow pipe is communicated with the mother liquid tank, the liquid phase output end of the centrifugal separator is communicated with the mother liquid tank through a pipeline, and the solid phase output end of the centrifugal separator is communicated with the dryer through a pipeline.
Preferably, the air current breaker includes feeding storehouse, nitrogen breaker, cyclone collector and pulse bag collector, the input in feeding storehouse passes through the output intercommunication of pipeline with the desiccator, and the output in feeding storehouse and the input intercommunication of nitrogen breaker, and the output of nitrogen breaker passes through the input intercommunication of pipeline with cyclone collector, and cyclone collector's discharge gate passes through pipeline and automatic packaging machine's input intercommunication, and cyclone collector's air-out end passes through the input intercommunication of pipeline and pulse bag collector, and pulse bag collector's output passes through pipeline and automatic packaging machine intercommunication.
Preferably, the feed end of the raw material bin is provided with a gas collecting hood.
Compared with the prior art, the utility model has the advantages that:
the method comprises the following steps of firstly, utilizing DTB recrystallization as a means for separating soluble ions, increasing soluble impurities in mother liquor by tens of times after repeated recrystallization, and achieving the thousandth level of certain control indexes in products, wherein in the case, large particles are crystallized to form the minimum ratio of the area to the volume of crystals, reducing impurities carried on the surfaces of the crystals, and in the process of crystal growth, stably forming the crystals to avoid the carrying of internal impurities;
secondly, the process of generating impurity barium carbonate is mainly a drying and crushing link of the material in a solid state, namely after centrifugal separation, wherein the solid drying adopts closed vacuum drying and adopts nitrogen airflow for crushing, so that the contact with carbon dioxide in the air is avoided, and the generation of barium carbonate is prevented;
thirdly, because of the difference of the grain size of the crystal, the water content on the surface of the crystal and the water content in the crystal, and the characteristic of easy caking of the crystal, the water content of the dried barium hydroxide octahydrate has slight differences, and the differences can influence the formulation precision of certain downstream of a client;
fourthly, in the traditional technology, the conditions of pipe blockage and equipment blockage often occur, particularly in the filtering link, the reason is that the saturated concentration and the heat preservation are not well controlled, in the dissolving link, the technology controls the 80 ℃ saturated concentration for proportioning, the temperature is raised to 90 ℃ and then the mixture is sent backwards, the related equipment and pipelines adopt steam heat tracing, so that the materials are ensured not to be separated out before entering a DTB (draw textured boron) crystallization kettle, and the problem of pipe blockage of the traditional device is solved;
fifthly, barium hydroxide is a toxic medium, the solid production process is completed in a closed system, and a gas collecting hood is arranged in the feeding link, so that dust is prevented from flying, and the safety coefficient is improved;
and sixthly, a temperature rise link is provided, the temperature is controlled to be 90 ℃ instead of boiling the solution, and a tail gas exhaust pipe is arranged to prevent toxic steam from escaping and improve the safety coefficient.
Drawings
FIG. 1 is a schematic view of the structure of this embodiment;
FIG. 2 is a schematic view showing the structure of a dissolving tank of the present embodiment;
FIG. 3 is a schematic view of the construction of a precision filter according to the present embodiment;
FIG. 4 is a schematic view showing the structure of a DTB crystallization system of this example;
FIG. 5 is a schematic diagram of the thickener according to the embodiment;
FIG. 6 is a schematic view showing the structure of the centrifugal separator of the embodiment;
FIG. 7 is a schematic view showing the structure of the dryer of the present embodiment;
fig. 8 is a schematic view of the structure of the airflow crusher of the present embodiment.
Detailed Description
The present invention will be further explained below.
Example (b):
as shown in figure 1, the high-purity barium hydroxide octahydrate purification production system comprises a raw material bin, a mother liquor tank, a dissolving tank, a precision filter, a transfer tank, a DTB crystallization system, a thickener, a centrifugal separator, a dryer, an airflow crusher and an automatic packaging machine which are sequentially communicated. Wherein, communicate through the measurement belt between former feed bin and dissolving tank, mother liquor groove, dissolving tank, precision filter, transfer tank, DTB crystal system, stiff ware, centrifugal separator, desiccator, air current breaker and automatic packaging machine communicate through the pipeline in proper order, all are provided with the pump body and the valve that are used for controlling the normal transportation of material on the pipeline. The pipeline outside all is provided with the heat preservation in this embodiment in order to advance the heat preservation to the thick liquid of carrying, prevents that the crystal from appearing in the pipeline.
The output of former feed bin is provided with the butterfly valve, and the measurement belt is located former feed bin output under, and the output of measurement belt is located, and the feed inlet department on dissolving tank top to transport the material to dissolving in the dissolving tank, should throw the material link in this embodiment and be provided with the gas collecting channel, fly upward in order to prevent the dust, harm operating personnel healthy.
The top of dissolving tank passes through pipeline and mother liquor tank intercommunication, and the pump body on the pipeline of this department takes the measurement function to with control center signal connection, reach the control to the mother liquor input, thereby cooperate with the industrial grade barium hydroxide octahydrate of input and dissolve.
In this embodiment, in order to achieve the precise control of the concentration of the solution in the dissolving tank, the control center is used to control the metering belt and the pump body with the metering function at the position of the mother liquor conveying pipeline, the metering belt is interlocked with the on-line mother liquor flow meter, and the control center adjusts the running speed of the metering belt according to the flow of the mother liquor, so as to achieve the purpose of controlling the amount of the material added to the dissolving tank, and calculate the ratio.
As shown in fig. 1 and 2, in order to remove strontium and calcium ions in the dissolving tank, a strontium removal agent storage tank is connected to the top end of the dissolving tank through a pipeline, a valve body with a flow meter function and a flow rate adjusting function is arranged at the pipeline to regulate and control the adding amount of the strontium removal agent, and a quantitative strontium removal agent is dropwise added in the dissolving process to form precipitates with strontium and calcium in the solution. In this embodiment, the valve body on the pipeline is in signal connection with the control center, the control center calculates and controls the adding rate and the total amount of the strontium removal agent according to the obtained information, the strontium removal agent is selected from an ammonium fluoride solution, and due to the combination of cations and fluoride ions and the difference of solubility, fluoride ions preferentially combine with strontium ions and calcium ions to form a precipitate, thereby completing the removal of the strontium ions and the calcium ions from the solution. In order to achieve better dissolving and reaction effects, a stirring paddle is arranged in the dissolving tank to stir the solution, an interlayer is arranged on the side wall of the dissolving tank, steam is supplied to a steam inlet of the interlayer, and condensed water in the interlayer flows out from a condensed water outlet, so that the dissolving and the reaction are sufficient.
Because the temperature is higher, barium hydroxide solubility is bigger, nevertheless heaies up, dissolves and need the certain time, dissolving tank includes one-level dissolving tank and second grade dissolving tank in this application, and the feed inlet setting is on the top of one-level dissolving tank, and strontium removal agent storage jar and one-level dissolving tank intercommunication, the output of one-level dissolving tank and second grade dissolving tank pass through the pipeline and are connected with precision filter's input, and the overflow export has been seted up to the lateral wall of one-level dissolving tank, the overflow entry has been seted up to the lateral wall of second grade dissolving tank, overflow export and overflow entry intercommunication, the height that highly is not higher than the overflow export of overflow entry, the lateral wall of one-level dissolving tank and second grade dissolving tank all is provided with the intermediate layer, and the lateral wall of one-level dissolving tank and second grade dissolving tank all is provided with the condensate outlet that supplies steam to let in intermediate layer and supply the outflow of condensate water in the intermediate layer. The setting of second grade dissolving tank has increased heat transfer area, also can control solid content simultaneously, in this embodiment, sets up thermometer and control system signal connection in one-level dissolving tank and second grade dissolving tank, the temperature in real-time supervision one-level dissolving tank and the second grade dissolving tank, and the temperature is about 80 ℃, guarantees under the condition that the solid just dissolves completely, is less than the material boiling point.
As shown in fig. 1 and 3, the solution after the dissolution reaction is heated to 90 ℃ again, and then is conveyed into a precision filter by a pump body to filter insoluble impurities, wherein the insoluble impurities mainly comprise silicon dioxide, dust impurities, calcium strontium precipitate and the like. Since the content of insoluble impurities is originally small and the purity requirement of the product is high, the common filtering means can not meet the requirement. Adopt an advanced microporous filter in this embodiment, the filter fineness is 2 mu m, simultaneously in order to prevent that the crystal from appearing and blockking up the micropore at the filtration in-process, cause the unable normal clear operation of filtration work, precision filter's lateral wall is provided with the intermediate layer, and precision filter's lateral wall is provided with the steam inlet that supplies steam to let in the intermediate layer and supplies the comdenstion water export that the comdenstion water flows out in the intermediate layer, keeps warm to whole precision filter's inside, prevents that the crystal from appearing after the cooling, blocks up the filter core. In this embodiment, for the purpose of long-term use of the precision filter, the side wall of the precision filter is communicated with a back flush pipeline and a forward flush pipeline, the back flush pipeline is communicated with a back flush water inlet pipe and a back flush nitrogen inlet pipe, and the back flush water inlet pipe and the back flush nitrogen inlet pipe are both provided with valves. The positive flushing pipeline is communicated with a positive flushing water inlet pipe and a positive nitrogen-blowing gas inlet pipe, and valves are arranged on the positive flushing water inlet pipe and the positive nitrogen-blowing gas inlet pipe. After a certain amount of slag is accumulated, the precision filter blows out liquid in the forward direction through nitrogen, and can be repeatedly used after slag is discharged in the reverse direction.
Accomplish filterable solution and carry to the transfer inslot and keep in, be provided with the coiled pipe in the transfer inslot, the one end of coiled pipe supplies steam to get into, and the other end supplies the condensate water to discharge, carries out heat preservation through the liquid of coiled pipe in the transfer inslot, avoids the crystal to appear in the transfer inslot.
As shown in fig. 1 and 4, the solution is then fed into a DTB crystallization system for recrystallization. The DTB crystallization system comprises a DTB crystallizer, a crystallization cooler, a crystallization circulating pump, a crystal extraction pump and a liquid outlet pump, wherein the bottom of the DTB crystallizer is connected with the crystallization circulating pump through a pipeline, the output end of the crystallization circulating pump is communicated with the input end of the crystallization cooler, the output end of a transit trough is communicated with the input end of the crystallization cooler through a pipeline, the output end of the crystallization cooler is communicated with the input end of the DTB crystallizer through a pipeline, the bottom of the DTB crystallizer is communicated with a thickener through a pipeline, and the crystal extraction pump is arranged on the pipeline. And after mixing the fed barium hydroxide solution with barium hydroxide slurry at the bottom of the DTB crystallizer, feeding the mixed barium hydroxide solution into a crystallization cooler through a pipeline by a crystallization circulating pump for circulating heat exchange, cooling and recrystallizing, wherein the solubility of the barium hydroxide is reduced after cooling, crystals are separated out, and the temperature of the whole system is maintained at about 40 ℃. The purpose of recrystallization is to remove soluble ionic impurities, such as Ca2+, K +, Na +, Sr2+, CL-, SO 42-and the like. The content of the impurities is very small, when the solution is cooled and the barium hydroxide reaches saturated concentration to be separated out, the impurities still far reach the separation concentration, so that soluble ions are left in the mother solution, and pure barium hydroxide octahydrate crystals are separated out. After repeated recrystallization cycles, various impurity ions in the mother liquor can be enriched, the quality of crystallized barium hydroxide can be gradually reduced, and when the barium hydroxide reaches a certain degree, the mother liquor is discharged to the next procedure for treatment, and fresh water is added again. Carbonate is usually added into the high-impurity mother liquor to precipitate and recover barium salt, and the residual waste liquor is subjected to salt evaporation treatment.
And after the recrystallization is finished, continuously extracting barium hydroxide slurry from the bottom of the DTB crystallizer by a crystal extraction pump. In this embodiment, the DTB crystallization system further includes corresponding detection and control instruments such as liquid level, temperature, flow rate, etc., which are all in signal connection with the control system, and the obtained signals are reacted to the control system and integrally controlled by the controller.
The outlet of the crystallization feeding pump is provided with a regulating valve which is linked with a flowmeter, so that the purpose of controlling the feeding flow and the retention time is achieved, and the longer the retention time is, the larger the crystal particles are; the pipeline for circulation of the crystallization cooler is provided with an adjusting valve and is interlocked with the online thermometer of the DTB crystallizer, so that the temperature control of the system is achieved, the temperature of the system of the crystallizer also determines the crystallization speed and the crystal nucleus size, the crystallization speed is slower and the crystal form is compact when the temperature is higher, the crystallization speed is faster and the crystal form is broken up when the temperature is lower, and proper temperature needs to be selected to balance the production energy consumption and the product quality. The solid content in the DTB system is controlled and the crystal growth interval is adjusted according to the extraction proportion of the crystal extraction pump and the liquid outlet pump. By means of the above means, analysis and sampling are carried out, so that the crystallization process is stable, and a large-particle and compact barium hydroxide crystal form is formed.
As shown in FIGS. 1 and 5, barium hydroxide slurry was continuously withdrawn from the bottom of the DTB crystallizer and fed into a thickener for thickening. The intercommunication is provided with the clear liquid overflow pipe on the lateral wall of stiff ware, and in this embodiment, the other end and the mother liquor groove intercommunication of clear liquid overflow pipe, clear liquid directly from stiff ware top overflow to mother liquor groove and carry out reuse.
As shown in fig. 1 and 6, the water content in the thick slurry is greatly reduced, and the thick slurry can be conveyed to a centrifugal separator for solid-liquid separation, and the solid phase output end of the centrifugal separator is communicated with a dryer through a pipeline. In order to reuse the mother liquor in this embodiment, the liquid phase output end of the centrifugal separator is communicated with the mother liquor tank through a pipeline.
As shown in FIGS. 1 and 7, the wet barium hydroxide solid having completed the solid-liquid separation was sent to a dryer to be dried, and dehydration was started at 100 ℃ since the melting point of barium hydroxide octahydrate was 78 ℃. The conventional temperature of electric heating and steam drying is about 120 degrees, and in order to prevent agglomeration and dehydration of the barium hydroxide octahydrate solid, a vacuum drying mode of 60 ℃ is adopted in the embodiment, so that the quality of the barium hydroxide octahydrate solid cannot be damaged in the drying process.
As shown in FIGS. 1 and 8, the dried barium hydroxide solid was sent to a jet mill and crushed to 10 μm. In this embodiment, the air current breaker includes feeding storehouse, nitrogen breaker, cyclone collector and pulse bag collector, the input in feeding storehouse passes through the output intercommunication of pipeline with the desiccator, and the output in feeding storehouse and the input intercommunication of nitrogen breaker, and the output of nitrogen breaker passes through the input intercommunication of pipeline with cyclone collector, and cyclone collector's discharge gate passes through pipeline and automatic packaging machine's input intercommunication, and cyclone collector's air-out end passes through the input intercommunication of pipeline and pulse bag collector, and pulse bag collector's output passes through pipeline and automatic packaging machine intercommunication. The airflow crusher adopts nitrogen as circulating gas to prevent the generation of barium carbonate. The crushed barium hydroxide octahydrate is powdered and is collected by the cooperation of a cyclone collector and a pulse bag type dust collector. The crushed barium octahydrate is powdery and uneven in particle size, the diameter of the barium octahydrate particles collected by the cyclone collector is larger than that of the barium octahydrate particles collected by the pulse bag type dust collector, and the barium octahydrate particles collected by the cyclone collector and the pulse bag type dust collector are mixed and then conveyed to an automatic packaging machine for packaging, so that the uniformity of the barium octahydrate particles in the same batch is basically the same, and the influence of the barium octahydrate particles in different packaging bags on the formulation precision of certain downstream of a client due to the difference of particle sizes is reduced. And the cyclone collector and the pulse bag type dust collector are adopted for cooperative collection, so that the collection efficiency is improved, the components are very uniform, and the caking is not easy to occur. The barium hydroxide octahydrate solid that accomplishes the collection directly transports to pack in the automatic packaging machine, accomplishes whole lithium hydroxide octahydrate's purification and packaging process, and whole process is continuous high-efficient, and operating personnel need not to carry out direct contact with barium hydroxide.
In this implementation, the top in one-level dissolving tank, second grade dissolving tank and mother liquor groove all is connected with the exhaust gas discharge pipe, and the exhaust gas discharge pipe discharges the atmosphere after handling in the same emission to supporting scrubbing tower with waste gas.
The whole manufacturing process is operated continuously, full-automatic production can be carried out through the design control system, the labor intensity of operators is reduced while the production efficiency is improved, meanwhile, raw materials are manufactured in a closed environment in the whole manufacturing process, contact between barium hydroxide and the operators is effectively reduced, and the safety factor of the working environment of the operators is improved.
The using process comprises the following steps:
s1, manually transferring industrial barium octahydrate Ba (OH)2.8H20 to a raw material bin, metering by a metering belt, conveying to a primary dissolving tank, simultaneously conveying a mother solution in a mother solution tank to the primary dissolving tank through a pipeline, stirring and dissolving the industrial barium octahydrate and the mother solution according to a certain mass ratio, wherein the mass ratio of the industrial barium octahydrate and the mother solution is 9:10, mixing and dissolving to obtain (27% concentration slurry), overflowing to a secondary dissolving tank for temporary storage after the mixed slurry stays in the primary dissolving tank for a period of time, controlling the temperature of the primary dissolving tank and the temperature of the secondary dissolving tank to be 80 ℃ in the dissolving process, just completing the dissolution of solids in the dissolving tank, and conveying the primary dissolving tank and the secondary dissolving tank at 90 +/-2 ℃ when conveying is needed, so that the solution is in an unsaturated state, and crystal precipitation caused by temperature reduction in the pipeline conveying process is prevented, plugging pipes and equipment;
s2, continuously dropwise adding a liquid strontium removal agent in the stirring and dissolving process of the primary dissolving tank, wherein in the embodiment, the selected strontium removal agent is an ammonium fluoride solution, after the strontium removal agent enters the primary dissolving tank, fluorine ions are preferentially combined with strontium and calcium ions due to the combination of cations and fluorine ions and solubility difference, strontium fluoride and calcium fluoride precipitates are formed, and strontium ions and calcium ions in the original solution are removed;
s3, pressurizing the barium hydroxide solution completely dissolved by the pump body, sending the barium hydroxide solution into a precision filter to filter insoluble impurities, and placing the filtered solution into a transfer tank for heat preservation and temporary storage to avoid crystal precipitation in the transfer tank;
s4, sending the liquid in the transit tank into a DTB crystallizer system for recrystallization to remove soluble ions, wherein the temperature of the DTB crystallizer system is set to be 40 +/-2 ℃;
s5, conveying the crystallized barium hydroxide octahydrate into a centrifugal separator for dry-wet separation, conveying the separated solid phase into a dryer for drying, wherein the drying adopts vacuum drying, and the temperature is controlled at 60 ℃;
and S6, feeding the dried barium hydroxide octahydrate into an airflow crusher for crushing, and finally conveying the crushed barium hydroxide octahydrate into an automatic packaging machine for packaging.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; while the utility model has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the utility model as defined by the appended claims.
The utility model adopts industrial grade barium hydroxide as a raw material (first-class index of HG/T2566-2014 industrial barium hydroxide, 97% purity), removes insoluble impurities and soluble ions in the raw material through a plurality of processes such as dissolution, chemical impurity removal, filtration, recrystallization, drying, crushing and the like, improves the purity to more than 99.5%, and obtains the high-purity barium hydroxide octahydrate.
The product quality is high (more than or equal to 99.5 percent) when the equipment is adopted for production, and is far superior to the standard that the first-class product of HGT 2629 plus 2011 chemical reagent barium hydroxide octahydrate (barium hydroxide) in the current market is more than or equal to 98 percent.
Claims (9)
1. A high-purity barium hydroxide octahydrate purification production system which characterized in that:
comprises a raw material bin, a mother liquor tank, a dissolving tank, a precision filter, a transfer tank, a DTB crystallization system, a thickener, a centrifugal separator, a dryer, an airflow crusher and an automatic packaging machine which are sequentially communicated;
the raw material bin is communicated with the dissolving tank through a metering belt, and the mother liquid tank, the dissolving tank, the precision filter, the transfer tank, the DTB crystallization system, the thickener, the centrifugal separator, the dryer, the airflow crusher and the automatic packaging machine are sequentially communicated through pipelines;
the top end of the dissolving tank is provided with a feed inlet for receiving materials output by a metering belt, the top end of the dissolving tank is connected with a strontium removal agent storage tank through a pipeline, the top end of the dissolving tank is also communicated with a mother liquor tank through a pipeline for conveying mother liquor into the dissolving tank to dissolve raw materials in the dissolving tank, and the pipeline is provided with a pump body and a valve for controlling normal transportation of the materials;
the dissolving tank comprises a first-stage dissolving tank and a second-stage dissolving tank, a feed inlet is formed in the top end of the first-stage dissolving tank, a strontium removal agent storage tank is communicated with the first-stage dissolving tank, the output end of the first-stage dissolving tank and the output end of the second-stage dissolving tank are connected with the input end of a precision filter through a pipeline, an overflow outlet is formed in the side wall of the first-stage dissolving tank, an overflow inlet is formed in the side wall of the second-stage dissolving tank, the overflow outlet is communicated with the overflow inlet, and the height of the overflow inlet is not higher than that of the overflow outlet.
2. The purification production system of high-purity octahydrate barium hydroxide as claimed in claim 1, wherein the side walls of the primary dissolving tank and the secondary dissolving tank are provided with interlayers, and the side walls of the primary dissolving tank and the secondary dissolving tank are provided with a steam inlet for introducing steam into the interlayers and a condensed water outlet for allowing condensed water in the interlayers to flow out.
3. The system for purifying and producing the high-purity octahydrate barium hydroxide as claimed in claim 1, wherein the side wall of the precision filter is provided with an interlayer, and the side wall of the precision filter is provided with a steam inlet for introducing steam into the interlayer and a condensed water outlet for allowing condensed water in the interlayer to flow out.
4. The system for purifying and producing high-purity octahydrate barium hydroxide as claimed in claim 1, wherein a coiled pipe is arranged in the transit tank, steam enters from one end of the coiled pipe, and condensed water is discharged from the other end of the coiled pipe.
5. The purification production system of high-purity octahydrate barium hydroxide of claim 1, wherein a back flush pipeline and a positive flush pipeline are arranged on the side wall of the precision filter in a communication manner;
a back washing water inlet pipe and a back blowing nitrogen inlet pipe are communicated with the back washing pipeline, and valves are arranged on the back washing water inlet pipe and the back blowing nitrogen inlet pipe;
the positive flushing pipeline is communicated with a positive flushing water inlet pipe and a positive nitrogen-blowing gas inlet pipe, and valves are arranged on the positive flushing water inlet pipe and the positive nitrogen-blowing gas inlet pipe.
6. The purification production system of high-purity barium hydroxide octahydrate according to claim 1, wherein the DTB crystallization system comprises a DTB crystallizer, a crystallization cooler, a crystallization circulating pump, a crystal extraction pump and a liquid outlet pump;
the bottom of the DTB crystallizer is connected with a crystallization circulating pump through a pipeline, the output end of the crystallization circulating pump is communicated with the input end of a crystallization cooler, the output end of a transit tank is communicated with the input end of the crystallization cooler through a pipeline, the output end of the crystallization cooler is communicated with the input end of the DTB crystallizer through a pipeline, the bottom of the DTB crystallizer is communicated with a thickener through a pipeline, and a crystal extraction pump is arranged on the pipeline.
7. The purification production system of high-purity barium hydroxide octahydrate according to claim 1, wherein a clear liquid overflow pipe is arranged on the side wall of the thickener in a communication mode, the other end of the clear liquid overflow pipe is communicated with a mother liquid tank, the liquid phase output end of the centrifugal separator is communicated with the mother liquid tank through a pipeline, and the solid phase output end of the centrifugal separator is communicated with the dryer through a pipeline.
8. The purification production system of high-purity barium hydroxide octahydrate according to claim 1, wherein the airflow crusher comprises a feeding bin, a nitrogen crusher, a cyclone collector and a pulse bag type dust collector, the input end of the feeding bin is communicated with the output end of the dryer through a pipeline, the output end of the feeding bin is communicated with the input end of the nitrogen crusher, the output end of the nitrogen crusher is communicated with the input end of the cyclone collector through a pipeline, the discharge port of the cyclone collector is communicated with the input end of the automatic packaging machine through a pipeline, the air outlet end of the cyclone collector is communicated with the input end of the pulse bag type dust collector through a pipeline, and the output end of the pulse bag type dust collector is communicated with the automatic packaging machine through a pipeline.
9. The purification production system of high-purity octahydrate barium hydroxide as claimed in claim 1, wherein the feed end of the raw material bin is provided with a gas-collecting hood.
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