CN211586537U - Reactor for producing potassium dihydrogen phosphate by thermal decomposition of potassium chloride and phosphoric acid - Google Patents
Reactor for producing potassium dihydrogen phosphate by thermal decomposition of potassium chloride and phosphoric acid Download PDFInfo
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- CN211586537U CN211586537U CN201921833885.8U CN201921833885U CN211586537U CN 211586537 U CN211586537 U CN 211586537U CN 201921833885 U CN201921833885 U CN 201921833885U CN 211586537 U CN211586537 U CN 211586537U
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 68
- 235000019796 monopotassium phosphate Nutrition 0.000 title claims abstract description 45
- 238000005979 thermal decomposition reaction Methods 0.000 title claims abstract description 37
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 32
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 32
- 229910000402 monopotassium phosphate Inorganic materials 0.000 title claims abstract description 25
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 49
- 239000007788 liquid Substances 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000010439 graphite Substances 0.000 claims abstract description 33
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 33
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims abstract description 27
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 3
- 239000010959 steel Substances 0.000 claims abstract description 3
- 238000007599 discharging Methods 0.000 claims description 9
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 24
- 238000000034 method Methods 0.000 abstract description 19
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 238000000354 decomposition reaction Methods 0.000 abstract description 15
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000012546 transfer Methods 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 229910019142 PO4 Inorganic materials 0.000 description 10
- 239000011265 semifinished product Substances 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 6
- 239000003337 fertilizer Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 239000007836 KH2PO4 Substances 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- YYRMJZQKEFZXMX-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca+2].OP(O)(O)=O.OP(O)(O)=O YYRMJZQKEFZXMX-UHFFFAOYSA-N 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910000856 hastalloy Inorganic materials 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000002426 superphosphate Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 244000241257 Cucumis melo Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 244000299507 Gossypium hirsutum Species 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000006115 defluorination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 230000006806 disease prevention Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 235000021049 nutrient content Nutrition 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 description 1
- 229940099402 potassium metaphosphate Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000013616 tea Nutrition 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 1
Images
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
A reactor for producing potassium dihydrogen phosphate by thermal decomposition of potassium chloride and phosphoric acid is characterized in that: the gas-liquid separator consists of an upper gas-liquid separator and a lower heater, and is characterized in that: the centrifugal demister is arranged on the top of the upper gas-liquid separator, so that tail gas generated by reaction does not carry liquid, absorption treatment is facilitated, and industrial hydrochloric acid is produced as an by-product. Convection tubes are arranged between the upper and lower material tight spaces of the lower heater, so that heat and mass transfer are facilitated, and air can be introduced into reaction materials to move and react to improve the decomposition rate of KCl. The heater is a block-hole heat exchanger, is circularly heated by a heat carrier, and has large heat exchange surface and high heat efficiency. The method of using the polytetrafluoroethylene material to impregnate graphite, steel lining, etc. The reactor is high temperature resistant, strong acid corrosion resistant, high in heating efficiency and good in gas-liquid separation. Is a special device for producing potassium dihydrogen phosphate by a thermal decomposition method. Its performance has direct influence on MKP production energy consumption, cost, quality and pollution.
Description
Technical Field
The utility model relates to a thermal decomposition reactor especially relates to a be used for KCl + H3PO4→KH2PO4+ a thermal decomposition reactor for producing potassium dihydrogen phosphate from HCl.
Background
Potassium dihydrogen phosphate (MKP), KH2PO4Also being colorless or white with glossCrystal, insoluble in alcohol, hygroscopic and deliquescent, soluble in water, weakly acidic in water solution, heated to 400 deg.C, and cooled to obtain potassium metaphosphate KPO3。
Monopotassium phosphate has a wide application range. The industrial application includes: 1. pharmaceutical industry: can be used as nutrient and enhancer for culturing and fermenting microorganism in antibiotic production, and can be used as uricacidifier and nutrient in medicine. 2. Food industry: flavoring agent for sake, and additive for monosodium glutamate. 3. Feed industry: a nutritional supplement. 4. Chemical production: other phosphate production raw materials, buffers, etc. In agriculture, the fertilizer is an efficient P.K fertilizer, has low salt index, high nutrient content (84%), contains no chlorine, is stable in physical and chemical properties, has no risk of burning seeds, seedlings and roots of crops, and can be used for foliage spraying, seed soaking, seed dressing, base fertilizer, top dressing, micro-fertilizer and other purposes. Has strong adaptability to soil. It is widely used in the production of grains, melons and fruits, vegetables, tea, tobacco and cotton. Especially when the fertilizer is sprayed on the leaves of crops in flowering, fruiting and mature periods, the fertilizer has the effects of increasing yield and quality of crops, and has the advantages of small using amount, high utilization rate and low loss. In addition, the effects of drought resistance, cold resistance and pest and disease prevention are also found.
There are many methods for producing potassium dihydrogen phosphate, such as neutralization method, ion exchange method, electrodialysis method, Gilbert method, double decomposition method, etc. The above methods have advantages and disadvantages, use premises, P.K raw material sources and product quality differences. Each has various difficulties and problems. In general, the medium-sized legal application is the most, the technical difficulty is low, the investment is low, the product quality is stable, and the yield is high. But the cost is the highest and the market price is basically determined by neutralization plus the benefits.
However, the most ideal mode for producing the potassium dihydrogen phosphate is KCl + H3PO4A thermal decomposition method. However, the technical difficulty is high, and the reaction is difficult to carry out. The reaction is first of all carried out at a relatively high temperature. For example, 170-190 ℃ is required, and the problems of the equipment, the material, the heating mode and the heat source are all the problems.
For the production of MKP by thermal decomposition, enamel reactors using organic carriers have been usedCirculation, indirect heating of KCL + H in jacket3PO4(excess), the temperature is also about 170 ℃, and HCl vapor generated in the reaction is removed by vacuumizing, and the results are that:
h-shape of enamel (glass lining) not high temperature resistant3PO4Corrosion perforation, limited moving reaction capacity of a vacuum method, too small heat exchange area, low KCl decomposition rate, and finally perforation of a plurality of reaction kettles does not lead the KCL decomposition rate to reach 70 percent, and qualified MKP products are not produced.
Therefore, a Hastelloy alloy is found through a large amount of work, only produced in China and America and having the price of 50-60 ten thousand yuan/ton, only comprises plates, and only for H3PO4The corrosion rate of HCl at 170 ℃ reaches 0.21-0.23 mm/year, which is more than 1 time of the requirement, and the thermal decomposition reactor processed by the Hastelloy alloy can only be in a 'kettle type'.
Results used: and because the heat exchange area is too small, the production efficiency is very low, various consumptions are very high, and the failure is ended.
Therefore, fuel oil and combustion gas are used for heating in a reaction chamber of a vertical rotary bedroom, a material spraying mode and a wall hanging mode, heat transfer is difficult to achieve an ideal condition, a thermal decomposition effect is only about 70%, the thermal efficiency is low, material loss is large, tail gas is difficult to treat, and the situation cannot exist.
In the last century, "united states chemical company" also used thermal decomposition to produce potassium dihydrogen phosphate, and it is known from limited data that: the thermal decomposition is carried out in a vertical reactor with a high degree of dilution without hydrolysis, wherein the reaction mass K: P is 1:1.762, superheated steam is directly introduced into the reaction mass for heating, the introduction speed of the superheated steam is 7150kg/h, the temperature is 170 +/-5 ℃, generated HCl is brought out by the superheated steam, about 3% of HCl is contained in the escaped steam, the decomposition rate of KCl reaches 88.3%, and the reaction mass is diluted by adding water without hydrolysis, wherein the dilution degree is 1: 1.42. Cooling to 60 deg.C, centrifugal decomposing to obtain potassium dihydrogen phosphate semi-finished product, Cl-The% is 0.024%, although the effect is good and the product quality is good, the following problems still exist: 1. the MKP circulating liquid (mother liquid) per ton is too large, 8230kg/tMKP, K2MKP yield of OToo low, only 21%. 2. The heat consumption is too high, reaches more than 700 kilocalories per kMKP, the heat efficiency is too low, is only 21.5 percent, and 700m is needed for each ton of MKP according to the Chinese condition3The economic feasibility of natural gas, or 1000kg of standard coal, becomes a problem. 3, the environmental protection is also a problem, and the tail gas is water vapor, wherein the HCl content is 3 percent, and the tail gas cannot be directly discharged. Such a thermal decomposition reactor is impossible to use in china.
SUMMERY OF THE UTILITY MODEL
In order to solve the above problem, the utility model provides a following scheme:
a reactor for producing monopotassium phosphate by thermal decomposition of potassium chloride and phosphoric acid comprises a gas-liquid separator and a heater, wherein the gas-liquid separator is of a cylindrical structure, a top cover is arranged at the top end, a hole is formed in the center of the top cover, a demister vertically penetrates through the top cover and extends into the gas-liquid separator, a feed hole is formed in the middle of the upper part of the gas-liquid separator, and a tail gas outlet is formed in the top side of the gas-liquid separator; the heater comprises a feeding chamber, a graphite heat exchanger and a discharging chamber, wherein convection holes are formed in the side walls of the feeding chamber and the discharging chamber and are communicated with each other through convection pipes, an air inlet and a material outlet are further formed in the side wall of the discharging chamber, a sewage discharge outlet is formed in the bottom of the discharging chamber, and an organic heat carrier inlet and an organic heat carrier outlet are formed in the graphite heat exchanger.
Furthermore, the convection tubes are provided with 1-3 tubes, and each convection tube is provided with an expansion joint.
Furthermore, the side walls of the middle part and the lower part of the gas-liquid separator are respectively provided with a viewing mirror.
Further, the top wall of the gas-liquid separator is also provided with a manhole.
Furthermore, a temperature measuring hole is formed in the side wall of the feeding chamber.
Further, the graphite heat exchanger is a block-hole graphite heat exchanger, the graphite heat exchanger has the specification of Dg800, Dg1000 and Dg1200, and the heat exchange area is a square meter of 20, 30, 45, 60 or 90.
Furthermore, the graphite block in the block-hole type graphite heat exchanger is vertically provided with
Article ofMaterial holes with 30 percent of opening rate are horizontally arranged
Organic thermal carrier pores.
Furthermore, the graphite block in the block-hole type graphite heat exchanger is impregnated with polytetrafluoroethylene and sintered at the temperature of over 380 ℃; the temperature of the organic heat carrier passing through the graphite block is less than or equal to 230 ℃; the design pressure of the graphite block is 0.4MPa on the organic heat carrier side and 0.25MPa on the material side.
Further, the demister is a centrifugal demister.
Furthermore, the steel parts of the gas-liquid separator and the heater, which can contact materials, are loosely lined with high-density polytetrafluoroethylene plates, and the thickness of the polytetrafluoroethylene plates is 2-4 mm.
The implementation method comprises the following steps:
(I) KCl with excess H3PO4Mixed material of (2) or equimolar KCl, H3PO4The liquid mixed with the circulating mother liquor (respectively) is injected into the thermal decomposition reactor through the feed port, and the liquid level is also approximately at the upper view mirror. After the materials are added, low-pressure air is introduced from an air inlet, the air flow rate is 0.1-0.2m/s of the empty tower flow rate, a heat carrier inlet and a heat carrier outlet of the heat exchanger are opened simultaneously, the materials are heated by a heat carrier, the temperature of the heat carrier is less than or equal to 230 ℃, and the temperature difference between the heat carrier and the heat carrier is adjusted to be about 30 ℃ by a heat pump at any time. The temperature of the material will gradually rise, and the thermal decomposition will also gradually proceed. Because the air is continuously introduced, the materials are convected from top to bottom, and the air only goes upward until the liquid level of the gas-liquid separator overflows, is discharged from the tail gas outlet through the demister and enters the tail gas absorber. The temperature is high, the moisture in the materials is changed into steam, and HCl generated by thermal decomposition is discharged from tail gas together with air. In the thermal decomposition reactor, the heat carrier provides heat, the temperature is increased to provide reaction heat, air forms bubbles, and the bubbles rise to form material convection, so that mass transfer and heat transfer are facilitated. The bubbles increase the escape area of HCl and promote the decomposition reaction of KCL.
In the gas-liquid separator, the air, water vapor and HCl escaped from the liquid level are discharged from the tail gas outlet through the demister, and the tail gas does not generate superphosphate because the HCl, the water vapor and the HCl are not large in air amount and low in flow rate and the demister is arranged. The tail gas is absorbed and treated into by-product industrial grade hydrochloric acid by conventional HCl, and the rest air and a small amount of water vapor are discharged after reaching the standard.
Reaction materials: when the material temperature reaches 170-190 ℃, the air inlet and the heat carrier inlet are closed when the decomposition rate of KCl naturally reaches 80-90%, the reaction is stopped, and the material liquid level is at the lower sight glass.
Discharging the reacted material from the discharge port, adding water, hydrolyzing, cooling to crystallize, centrifuging, and separating to obtain mother liquid and MKP semi-finished product. Quality important index Cl in MKP semi-finished product-% has reached to be less than or equal to 0.20% (when the decomposition rate of KCl in the process reaches 80%, the semi-finished product MKP Cl is obtained-The percentage is less than or equal to 0.15 percent; when the KCl decomposition rate reaches 85%, the MKP Cl% of the semi-finished product is less than or equal to 0.10%; when the KCl decomposition rate reaches 90 percent, the semi-finished product MKP Cl-Less than or equal to 0.05 percent). The thermal decomposition reactor has easily controlled and stable parameters. The cycle production, the material has no principle loss, and the MKP yield and the first-grade product rate are both more than 98 percent.
Heat consumption: the thermal decomposition reactor is indirectly heated by heat carrier (oil) in circulation mode, the heated organic heat carrier can be returned to the heat carrier furnace for heating and then is continuously used for heating materials, and finally only the reactor and the pipeline are subjected to heat dissipation loss. After the heat preservation, the loss is little. The heat efficiency is high, which reaches more than 70 percent, and the heat consumption of MKP is only 130 ten thousand Kcal/tMKP. Only the neutralization method can produce the MKP with 60 percent of heat consumption. Only United states chemical company processes have less than 20% of their heat rate.
(II) the device can also be used for producing feed grade H by wet-process phosphoric acid concentration and defluorination3PO4And concentrating the dilute H2SO4And has wide application.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
1. A feeding chamber; 2. a graphite heat exchanger; 3. a blanking chamber; 4. a manhole; 5. a tail gas outlet; 6. a demister; 7. a defoaming speed regulator; 8. a feed port; 9. an upper view mirror; 10. a lower view mirror; 11. a temperature measuring hole; 12. a heat carrier outlet; 13. a heat carrier inlet; 14. an air inlet; 15. a material outlet; convection holes; 17. a convection tube; 18. an expansion joint; 19. a sewage draining outlet.
Detailed Description
The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic drawings and illustrate the basic structure of the present invention only in a schematic manner, and thus show only the components related to the present invention.
Example 1: as shown in figure 1 of the drawings, in which,
a reactor for producing potassium dihydrogen phosphate by thermal decomposition of potassium chloride and phosphoric acid comprises a gas-liquid separator and a heater, wherein the gas-liquid separator is of a cylindrical structure, and a lower viewing mirror 10 and an upper viewing mirror 9. The top end of the gas-liquid separator is provided with a flat top cover, the center of the flat top cover is provided with a hole, the demister 6 vertically penetrates through the flat top cover to stretch into the flat top cover for installation, the middle part of the gas-liquid separator is provided with a feed hole 8, and the top of the separator is provided with a tail gas outlet 5 and a manhole 4; the heater includes material loading room 1, graphite heat exchanger 2 and unloading room 3, three pairs of to the discharge orifice 16 are seted up to material loading room 1 and 3 lateral walls of unloading room, the convection orifice 16 one-to-one of material loading room 1 and unloading room 3 uses convection tube 17 intercommunication, each convection tube 17 all is provided with expansion joint 18, material loading room 1 lateral wall has still opened temperature measurement hole 11, air inlet 14, material export 15 have still been seted up to 3 lateral walls of unloading room, drain 19 is seted up to 3 bottoms of unloading room, last heat carrier entry 13, the heat carrier export 12 of having opened of graphite heat exchanger 2.
The graphite heat exchanger 2 is a block-hole graphite heat exchanger, the graphite heat exchanger can be selected according to actual conditions to have the specification of Dg800, Dg1000, Dg1200 and the like, and the selected heat exchange area is a square meter of 20, 30, 45, 60 or 90.
The graphite block in the block-hole type graphite heat exchanger is vertically provided with
The material holes have an opening rate of 30 percent and are horizontally provided with
Organic thermal carrier pores. Block-hole type graphite heat exchangerThe graphite block is formed by impregnating polytetrafluoroethylene and sintering at the temperature of more than 380 ℃; the temperature of the organic heat carrier passing through the graphite block is less than or equal to 230 ℃. The design pressure of the graphite block is 0.4MPa on the organic heat carrier side and 0.25MPa on the material side.
KCl with excess H3PO4Mixed material of (2) or equimolar KCl, H3PO4The material mixed with the circulating mother liquor (respectively) is injected into the thermal decomposition reactor through the inlet opening 8, the liquid level being approximately at the upper viewing mirror 9. After the materials are added, low-pressure air is introduced from an air inlet 14, the air flow rate is 0.1-0.2m/s of the empty tower flow rate, a heat carrier inlet 13 and a heat carrier outlet 12 of the heat exchanger are opened simultaneously, the materials are heated by a heat carrier, the temperature of the heat carrier is less than or equal to 230 ℃, and the temperature difference between the heat carrier and the heat carrier is adjusted to be about 30 ℃ by a heat pump at any time. The temperature of the material will gradually rise, and the thermal decomposition will also gradually proceed. Because the air is continuously introduced, the materials are convected up and down, and the air only goes up until the liquid level of the gas-liquid separator overflows, is discharged from the tail gas outlet 5 through the demister 6 and enters the tail gas absorber. The temperature is high, the moisture in the materials is changed into steam, and HCl generated by thermal decomposition is discharged from tail gas together with air. In the thermal decomposition reactor, the heat carrier provides heat, the temperature is increased to provide reaction heat, air forms bubbles, and the bubbles rise to form material convection, so that mass transfer and heat transfer are facilitated. The bubbles increase the escape area of HCl and promote the decomposition reaction of KCL.
In the gas-liquid separator, the air, water vapor and HCl escaping from the liquid level are discharged from the tail gas outlet 5 through the demister 6, and the tail gas does not generate superphosphate because the HCl, the water vapor and the HCl are not large in air quantity, the flow rate is low and the demister 6 is arranged. The tail gas is absorbed and treated into by-product industrial grade hydrochloric acid by conventional HCl, and the rest air and a small amount of water vapor reach the standard and are discharged.
Reaction materials: when the material temperature reaches 170-190 ℃, the air inlet 17 and the heat carrier inlet 13 are closed when the decomposition rate of KCl naturally reaches 80-90%, the reaction is stopped, and the material liquid level is at the lower view mirror 10.
The material after the reaction is discharged from a material outlet 15, and is subjected to water addition, hydrolysis, cooling crystallization, centrifugal separation and separation (circulation)Ring) mother liquor and MKP intermediates. Quality important index Cl in MKP semi-finished product-% has reached to be less than or equal to 0.20% (when the decomposition rate of KCl in the process reaches 80%, the semi-finished product MKP Cl is obtained-The percentage is less than or equal to 0.15 percent; when the KCl decomposition rate reaches 85 percent, the semi-finished product MKP Cl-％Less than or equal to 0.10 percent; when the KCl decomposition rate reaches 90 percent, the semi-finished product MKP Cl-Less than or equal to 0.05 percent). The thermal decomposition reactor has easily controlled and stable parameters. The cycle production, the material has no principle loss, and the MKP yield and the first-grade product rate are both more than 98 percent.
Heat consumption: the thermal decomposition reactor is indirectly heated by heat carrier (oil) in circulation mode, the heated organic heat carrier can be returned to the heat carrier furnace for heating and then is continuously used for heating materials, and finally only the reactor and the pipeline are subjected to heat dissipation loss. After the heat preservation, the loss is little. The heat efficiency is high, which reaches more than 70 percent, and the heat consumption of MKP is only 130 ten thousand Kcal/tMKP. Only the neutralization method can produce the MKP with 60 percent of heat consumption. Only United states chemical company processes have less than 20% of their heat rate. Finally, it should be noted that the above-mentioned embodiments illustrate only specific embodiments of the invention. Obviously, the present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the invention should be considered as within the scope of the invention.
Claims (10)
1. A reactor for producing potassium dihydrogen phosphate by thermal decomposition of potassium chloride and phosphoric acid is characterized in that: the device comprises a gas-liquid separator and a heater, wherein the gas-liquid separator is of a cylindrical structure, a top cover is arranged at the top end of the gas-liquid separator, a hole is formed in the center of the top cover, a demister vertically penetrates through the top cover and extends into the gas-liquid separator, a feed hole is formed in the middle of the upper part of the gas-liquid separator, and a tail gas outlet is formed in the; the heater comprises a feeding chamber, a graphite heat exchanger and a discharging chamber, wherein convection holes are formed in the side walls of the feeding chamber and the discharging chamber and are communicated with each other through convection pipes, an air inlet and a material outlet are further formed in the side wall of the discharging chamber, a sewage discharge outlet is formed in the bottom of the discharging chamber, and an organic heat carrier inlet and an organic heat carrier outlet are formed in the graphite heat exchanger.
2. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce potassium dihydrogen phosphate as claimed in claim 1, wherein: the convection tubes are provided with 1-3 tubes, and each convection tube is provided with an expansion joint.
3. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce potassium dihydrogen phosphate as claimed in claim 1, wherein: and the side walls of the middle part and the lower part of the gas-liquid separator are respectively provided with a viewing mirror.
4. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce potassium dihydrogen phosphate as claimed in claim 1, wherein: the top wall of the gas-liquid separator is also provided with a manhole.
5. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce potassium dihydrogen phosphate as claimed in claim 1, wherein: and the side wall of the feeding chamber is also provided with a temperature measuring hole.
6. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce potassium dihydrogen phosphate as claimed in claim 1, wherein: the graphite heat exchanger is a block-hole graphite heat exchanger, the specification of the graphite heat exchanger can be selected from the group consisting of Dg800, Dg1000 and Dg1200, and the heat exchange area is a square meter of 20, 30, 45, 60 or 90.
7. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce monopotassium phosphate as claimed in claim 6 wherein: the graphite block in the block-hole type graphite heat exchanger is vertically provided with
The material holes have an opening rate of 30 percent and are horizontally provided with
Organic thermal carrier pores.
8. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce monopotassium phosphate as claimed in claim 6 wherein: the temperature of the organic heat carrier passing through the graphite block is less than or equal to 230 ℃; the design pressure of the graphite block is 0.4MPa on the organic heat carrier side and 0.25MPa on the material side.
9. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce potassium dihydrogen phosphate as claimed in claim 1, wherein: the demister is a centrifugal demister.
10. A reactor for the thermal decomposition of potassium chloride plus phosphoric acid to produce potassium dihydrogen phosphate as claimed in claim 1, wherein: the gas-liquid separator and the heater can be in contact with the steel parts of the materials, and the high-density polytetrafluoroethylene plate is loosely lined, and the thickness of the polytetrafluoroethylene plate is 2-4 mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113713730A (en) * | 2021-09-13 | 2021-11-30 | 山东高密高源化工有限公司 | Be used for high-purity sodium chlorite to prepare blending device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113713730A (en) * | 2021-09-13 | 2021-11-30 | 山东高密高源化工有限公司 | Be used for high-purity sodium chlorite to prepare blending device |
| CN113713730B (en) * | 2021-09-13 | 2023-12-22 | 山东高密高源化工有限公司 | Preparation and blending device for preparing high-purity sodium chlorite |
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