CN220940640U - Device for preparing ammonium bifluoride by AHF continuous reaction - Google Patents
Device for preparing ammonium bifluoride by AHF continuous reaction Download PDFInfo
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- CN220940640U CN220940640U CN202322036181.0U CN202322036181U CN220940640U CN 220940640 U CN220940640 U CN 220940640U CN 202322036181 U CN202322036181 U CN 202322036181U CN 220940640 U CN220940640 U CN 220940640U
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- reaction
- communicated
- reaction kettle
- tank
- ammonium bifluoride
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 91
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 238000001816 cooling Methods 0.000 claims description 37
- 238000005406 washing Methods 0.000 claims description 15
- 239000012452 mother liquor Substances 0.000 claims description 14
- 239000012295 chemical reaction liquid Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000006096 absorbing agent Substances 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 7
- 239000007790 solid phase Substances 0.000 claims 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 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 21
- 238000000034 method Methods 0.000 description 19
- 239000000047 product Substances 0.000 description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 14
- 238000007599 discharging Methods 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 4
- 239000011344 liquid material Substances 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910001506 inorganic fluoride Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- -1 reation kettle 1 Chemical compound 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The application relates to the technical field of ammonium bifluoride preparation, and particularly discloses a device for preparing ammonium bifluoride by AHF continuous reaction, which comprises a reaction kettle, wherein the reaction kettle is communicated with a heat exchanger for controlling the constant temperature of the reaction kettle through a pipeline, raw materials for preparing ammonium bifluoride are pumped into the reaction kettle for reaction, materials of the reaction kettle are self-circulated through a pump, the reaction heat in the reaction kettle is taken away through the heat exchanger, and the temperature in the reaction kettle is controlled to be constant. The temperature of the reaction materials is prevented from being too low, crystals are separated out, and a tube array for conveying the materials is prevented from being blocked; too high a temperature, decomposition of ammonium bifluoride and ammonium fluoride is also avoided, resulting in lower yields of ammonium bifluoride.
Description
Technical Field
The utility model relates to the technical field of ammonium bifluoride preparation, in particular to a device for preparing ammonium bifluoride by AHF continuous reaction.
Background
Ammonium bifluoride has molecular formula of NH 4HF2, is an inorganic fluoride salt with large dosage, and is mainly used as glass etchant, chemical reagent, boiler cleaning agent, fermentation industrial disinfectant, steel plate surface treating agent and the like. According to different production processes, the preparation method of ammonium bifluoride can be divided into a liquid phase method and a gas phase method, and the gas phase method has strict requirements on processes and equipment, and has large investment and high production cost; the liquid phase synthesis process has simple equipment, material saving, mild process conditions and easy control of production operation. So, at present, the liquid phase method is mostly adopted for producing ammonium bifluoride in China.
The prior liquid phase method for producing ammonium bifluoride has various devices, for example, chinese patent publication No. CN209367816U discloses a device capable of continuously producing ammonium bifluoride, which comprises an AHF finished product tank, an ammonia storage tank, a reaction tank, a circulation tank, a wind cooling tower, a material tower, a centrifugal machine and a mother liquor collecting tank, wherein the AHF finished product tank and the ammonia storage tank are communicated with the reaction tank, the reaction tank is communicated with the circulation tank, the circulation tank is communicated with the wind cooling tower, the wind cooling tower is communicated with the material tower, the material tower is communicated with the centrifugal machine, and the mother liquor collecting tank is respectively communicated with the reaction tank and the centrifugal machine. The method comprises the steps of metering AHF in an AHF finished product tank and liquid ammonia in an ammonia storage tank, introducing the metered pressure difference into a reaction tank with added mother liquor, carrying out reaction according to corresponding reaction proportion to obtain ammonium bifluoride and ammonium fluoride semi-finished products, pumping materials into a circulation tank after the reaction reaches a discharging temperature, pumping the materials in the circulation tank into an air cooling tower for circulating cooling through the pump, pumping the cooled materials into a material tower through the pump, finally delivering the materials in the material tower to a centrifugal machine, separating solid and liquid materials through the centrifugal machine, packaging solid and liquid materials in bags to obtain products, collecting the liquid materials by a mother liquor collecting tank, and introducing the liquid materials into the reaction tank for reaction. Solves the problems of low production efficiency, high labor cost and high labor intensity of the traditional ammonium bifluoride. However, the device and the method for controlling the temperature of the reaction in the reaction tank are not provided, so that the heat of the reaction generated in the reaction tank is completely taken away by air, the temperature of the reaction materials is uncontrollable, if the temperature is too low, crystals can be separated out of the reaction materials, the pipelines are easy to be blocked in the process of pipeline transportation, and if the temperature is too high, the materials of ammonium bifluoride and ammonium fluoride products generated in the reaction can be decomposed, so that the yield is too low.
Disclosure of utility model
The utility model aims to provide a device for preparing ammonium bifluoride by AHF continuous reaction, which aims to solve the problem that the reaction temperature in a reaction tank is uncontrollable.
In order to solve the problems, the technical scheme is as follows:
the device for preparing ammonium bifluoride by AHF continuous reaction comprises a reaction kettle, wherein the reaction kettle is communicated with a heat exchanger through a pipeline, reaction materials circularly flow in the heat exchanger and the reaction kettle, and the reaction materials and constant-temperature hot water exchange heat in the heat exchanger. The basic principle of the technical scheme is as follows: and (3) throwing the raw materials for preparing the ammonium bifluoride into a reaction kettle for reaction, starting a heat exchanger to take away the reaction heat in the reaction kettle, and controlling the temperature in the reaction kettle to be constant.
The beneficial effects of the technical scheme are that: compared with the existing device for preparing ammonium bifluoride by continuous AHF reaction, the technical scheme has the advantages that the temperature of the reaction kettle is controlled to be constant after the reaction kettle, so that the phenomenon that the temperature of reaction materials is too low, crystals are separated out and a tube array for conveying the materials is blocked is avoided; too high a temperature, decomposition of ammonium bifluoride and ammonium fluoride is also avoided, resulting in lower yields of ammonium bifluoride.
Further, the heat exchanger is communicated with a hot water tank through a pipeline, a variable pump is arranged between the hot water tank and the heat exchanger, and water in the hot water tank is discharged out of the hot water tank for cooling and then is discharged into the hot water tank to form circulating water. The hot water tank and the heat exchanger are matched to recycle water in the hot water tank, water resources are saved, and the variable pump is used for controlling the quantity of hot water introduced into the heat exchanger by the hot water tank so as to control the heat exchange temperature in the heat exchanger.
Further, the reaction kettle is communicated with a Venturi mixing injector. The reaction materials are mixed by the Venturi mixing ejector and then are introduced into the reaction kettle, the reaction kettle plays a role of a buffer tank, the Venturi mixing ejector uniformly mixes the reactants and then is introduced into the reaction kettle, stirring vibration in the reaction kettle is reduced, the reaction is more stable, and the reaction is more thoroughly mixed.
Further, the reaction kettle is communicated with a Venturi absorber. Before the hydrogen fluoride or ammonia which is not completely reacted in the reaction kettle enters the tail gas treatment, the hydrogen fluoride or ammonia is absorbed once through a Venturi absorber and then enters a gas phase pipeline, so that the situation that the hydrogen fluoride or ammonia which is not completely reacted in the reaction kettle is directly discharged into the tail gas treatment is avoided, the tail gas treatment capacity is increased, and meanwhile, the reactant is wasted.
Further, the venturi absorber is communicated with a secondary tail scrubber through a pipeline. The tail gas of the reaction kettle is firstly absorbed by a Venturi absorber on the reactor and then is absorbed by water in a second-stage tail washing tower, and the tail washing absorbing liquid with high concentration is recycled by controlling the concentration of each stage of tail gas tower and step absorption.
Further, the reaction kettle is sequentially communicated with a reaction liquid buffer tank, an air cooling circulation tank, a centrifugal buffer tank and a centrifugal machine through pipelines, the solid phase outlet end of the centrifugal machine is communicated with a product stirrer through the pipelines, the liquid phase outlet end of the centrifugal machine is communicated with a mother liquor tank through the pipelines, the top of the air cooling circulation tank is communicated with an air cooling tower through the pipelines, and the top of the air cooling tower is communicated with a secondary tail washing tower through the pipelines. And discharging the reaction liquid in the reaction liquid buffer tank into an air cooling circulation tank for circulating air cooling crystallization, enabling a high-temperature material and cold air to be in countercurrent contact for cooling in the air cooling circulation process to form ammonium fluoride (hydrogen) crystal slurry, gradually discharging the ammonium fluoride crystal slurry into a centrifugal buffer tank, then entering a centrifugal machine, centrifugally dehydrating, then entering a product package, and enabling centrifugal mother liquor to enter the air cooling circulation tank. The high-concentration tail washing absorption liquid is recovered and used as mother liquid after the air cooling tower is cleaned, and the tail gas and part of water taken away by the product are supplemented to reach water balance.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing ammonium bifluoride.
Reference numerals in the drawings of the specification include: the reaction kettle 1, a reaction liquid buffer tank 2, an air cooling circulation tank 3, a centrifugal buffer tank 4, a centrifugal machine 5, a product stirrer 6, an anti-caking agent tank 7, a mother liquor tank 8, an air cooling tower 9, a secondary tail washing tower 10, an air spraying tower 101, a packing tower 102, an induced draft fan 103, a tubular heat exchanger 11, a hot water tank 12, a venturi mixing ejector 13 and a venturi absorber 14.
Detailed Description
The following is a further detailed description of the embodiments:
an example is substantially as shown in figure 1:
The utility model provides a device of AHF continuous reaction preparation ammonium bifluoride, including reation kettle 1, reation kettle 1 has arranged intercommunication reaction liquid buffer tank 2 from the right through the pipeline in proper order, forced air cooling circulation tank 3, centrifugal buffer tank 4 and centrifuge 5, centrifuge 5 solid phase exit end has product agitator 6 through the pipeline intercommunication, there is anti-caking agent groove 7 through the pipeline intercommunication on the product agitator 6, centrifuge 5 liquid phase exit end has air cooling tower 9 through the pipeline intercommunication mother liquor groove 8 and forced air cooling circulation tank 3 simultaneously, forced air cooling circulation tank 3 top has air cooling tower 9 through the pipeline intercommunication, forced air cooling tower 9 top has second grade tail washing tower 10 through the pipeline intercommunication, reation kettle 1 left side has tubular heat exchanger 11 through the pipeline intercommunication, tubular heat exchanger 11 left side has hot water tank 12 through the pipeline intercommunication, be equipped with variable pump control inflow between hot water tank 12 and the tubular heat exchanger 11, be equipped with thermometer and temperature sensor on reation kettle 1, reation kettle 1 top left side intercommunication has SN-I type venturi mixing ejector 13, reation kettle 1 top right side intercommunication has venturi absorber 14 through pipeline intercommunication second grade tail washing tower 10.
The specific implementation process is as follows:
S1, anhydrous hydrogen fluoride and liquid ammonia are sent to a venturi mixing injector 13 for mixing through a conveying pump by a pipeline, a proper amount of process water is added into a reaction kettle 1, the pump is started to run through a tubular heat exchanger 11 for self-circulation, and then materials uniformly mixed in the venturi mixing injector 13 are introduced into the reaction kettle 1;
s2, adding process water into a hot water tank 12, introducing steam to heat the process water to 70 ℃, starting a variable pump, starting a tube array heat exchanger 11 to circulate water in the hot water tank 12, enabling a tube layer of the tube array heat exchanger 11 to remove materials, enabling a shell side to remove circulating hot water, enabling the variable pump to control the quantity of the circulating hot water, releasing heat in the reaction process of the reaction kettle 1, and controlling the reaction temperature in the reaction kettle 1 to be 50-65 ℃ by controlling the quantity of the circulating hot water through the variable pump;
S3, when the reaction pH value in the reaction kettle 1 reaches 3-3.5, discharging the reaction liquid in the reaction kettle 1 into a reaction liquid buffer tank 2, discharging the reaction liquid into an air cooling circulation tank 3 from the reaction liquid buffer tank 2 for circulating air cooling crystallization, enabling high-temperature materials to be in countercurrent contact with cold air for cooling in the air cooling circulation process to form ammonium bifluoride crystal slurry, gradually discharging the ammonium bifluoride crystal slurry into a centrifugal buffer tank 4, entering a centrifugal machine 5, centrifugally dehydrating solids into a product stirrer 6, simultaneously adding an anti-caking agent into the product stirrer 6 by an anti-caking agent tank 7, packaging the ammonium bifluoride product after the stirring of the product stirrer 6, enabling centrifugal mother liquor to enter the air cooling circulation tank 3, discharging all the liquid in the air cooling circulation tank 3 to the centrifugal buffer tank 4 for centrifugation after the air cooling of a certain temperature, simultaneously switching the mother liquor into a mother liquor tank 8, and pumping the mother liquor into the reaction kettle 1 for recycling by a mother liquor circulating pump. And when the pH value of the reaction in the reaction kettle 1 reaches 6-7, repeating the operation S3 to obtain an ammonium fluoride product.
S4, introducing the tail gas of the air cooling tower 9 and the tail gas of the reaction kettle 1 into a tail gas washing tower, performing two-stage treatment, and introducing the tail gas into a certain height through a draught fan 103 for emptying. The primary tail gas washing tower is an air-jet tower 101, the secondary tail gas washing tower 10 is a packed tower 102, fresh process water is supplemented from the secondary tail gas washing tower 10, the fresh process water is replaced into the primary tail gas washing tower, the fresh process water is replaced into the air-cooled circulating tank 3 through the primary tail gas washing tower, the reaction tail gas is introduced into the two-stage tail gas absorption tower for absorption, and after being separated by the gas-liquid separator, the non-condensable gas is led to a certain height for evacuation through the induced draft fan 103.
The foregoing is merely exemplary embodiments of the present utility model, and specific structures and features that are well known in the art are not described in detail herein. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the structure of the present utility model, and these should also be considered as the scope of the present utility model, which does not affect the effect of the implementation of the present utility model and the utility of the patent. The protection scope of the present utility model is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (5)
1. The device for preparing ammonium bifluoride by AHF continuous reaction comprises a reaction kettle and is characterized in that: the reaction kettle is communicated with a heat exchanger through a pipeline, reaction materials circularly flow in the heat exchanger and the reaction kettle, the reaction materials exchange heat with constant-temperature hot water in the heat exchanger, the heat exchanger is communicated with a hot water tank through a pipeline, a variable pump is arranged between the hot water tank and the heat exchanger, and water in the hot water tank is discharged into the hot water tank to form circulating water after being discharged out of the hot water tank for cooling.
2. The apparatus for preparing ammonium bifluoride by continuous reaction of AHF according to claim 1, wherein: and the reaction kettle is communicated with a Venturi mixing injector.
3. The apparatus for preparing ammonium bifluoride by continuous reaction of AHF according to claim 2, wherein: and the reaction kettle is communicated with a Venturi absorber.
4. An apparatus for preparing ammonium bifluoride by continuous reaction of AHF according to claim 3, characterized in that: the venturi absorber is communicated with a secondary tail washing tower through a pipeline.
5. The apparatus for preparing ammonium bifluoride by continuous reaction of AHF according to claim 4, wherein: the reaction kettle is sequentially communicated with a reaction liquid buffer tank, an air cooling circulation tank, a centrifugal buffer tank and a centrifugal machine through pipelines, the solid phase outlet end of the centrifugal machine is communicated with a product stirrer through the pipelines, the liquid phase outlet end of the centrifugal machine is communicated with a mother liquor tank through the pipelines, the top of the air cooling circulation tank is communicated with an air cooling tower through the pipelines, and the top of the air cooling tower is communicated with a secondary tail washing tower through the pipelines.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322036181.0U CN220940640U (en) | 2023-07-31 | 2023-07-31 | Device for preparing ammonium bifluoride by AHF continuous reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322036181.0U CN220940640U (en) | 2023-07-31 | 2023-07-31 | Device for preparing ammonium bifluoride by AHF continuous reaction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220940640U true CN220940640U (en) | 2024-05-14 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322036181.0U Active CN220940640U (en) | 2023-07-31 | 2023-07-31 | Device for preparing ammonium bifluoride by AHF continuous reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220940640U (en) |
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2023
- 2023-07-31 CN CN202322036181.0U patent/CN220940640U/en active Active
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