CN115448351A - Preparation method of alpha semi-hydrated gypsum - Google Patents
Preparation method of alpha semi-hydrated gypsum Download PDFInfo
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- CN115448351A CN115448351A CN202211038409.3A CN202211038409A CN115448351A CN 115448351 A CN115448351 A CN 115448351A CN 202211038409 A CN202211038409 A CN 202211038409A CN 115448351 A CN115448351 A CN 115448351A
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- 239000010440 gypsum Substances 0.000 title claims abstract description 30
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 142
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 72
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000013078 crystal Substances 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 57
- 230000009466 transformation Effects 0.000 claims abstract description 37
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 36
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 238000011084 recovery Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000002367 phosphate rock Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 9
- 238000007865 diluting Methods 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000003860 storage Methods 0.000 claims description 125
- 238000004321 preservation Methods 0.000 claims description 46
- 238000010790 dilution Methods 0.000 claims description 45
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- 238000005406 washing Methods 0.000 claims description 33
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 31
- 238000000605 extraction Methods 0.000 claims description 30
- 239000010410 layer Substances 0.000 claims description 29
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- 239000012071 phase Substances 0.000 claims description 22
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 20
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- 239000000945 filler Substances 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
- CVOQYKPWIVSMDC-UHFFFAOYSA-L dipotassium;butanedioate Chemical group [K+].[K+].[O-]C(=O)CCC([O-])=O CVOQYKPWIVSMDC-UHFFFAOYSA-L 0.000 claims description 14
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- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 229910000838 Al alloy Inorganic materials 0.000 claims description 10
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 10
- 239000010445 mica Substances 0.000 claims description 10
- 229910052618 mica group Inorganic materials 0.000 claims description 10
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- 150000001875 compounds Chemical class 0.000 claims description 8
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- 238000005260 corrosion Methods 0.000 claims description 8
- 239000007790 solid phase Substances 0.000 claims description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 4
- 239000001384 succinic acid Substances 0.000 claims description 4
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 239000002918 waste heat Substances 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 238000005234 chemical deposition Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 238000005240 physical vapour deposition Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 30
- 238000007789 sealing Methods 0.000 description 19
- 238000012546 transfer Methods 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- 239000011574 phosphorus Substances 0.000 description 9
- 229910052698 phosphorus Inorganic materials 0.000 description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 8
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 150000004683 dihydrates Chemical class 0.000 description 6
- 230000000149 penetrating effect Effects 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
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- 230000001276 controlling effect Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 5
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- 239000010703 silicon Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
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- 229920005830 Polyurethane Foam Polymers 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
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- 239000010959 steel Substances 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- 239000004831 Hot glue Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
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- 239000004566 building material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009837 dry grinding Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/466—Conversion of one form of calcium sulfate to another
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The application relates to the technical field of alpha hemihydrate gypsum preparation, in particular to a preparation method of alpha hemihydrate gypsum. Crushing phosphate rock into phosphate rock powder, adding water into concentrated sulfuric acid to dilute to 8-20%, collecting the heat produced by diluting the concentrated sulfuric acid through a heat recovery system, adding the crushed phosphate rock powder into the diluted sulfuric acid solution, stirring for reaction, extracting and separating while collecting the heat by the heat recovery system, sampling and detecting, adjusting the concentration of sulfuric acid and phosphoric acid and the solid-liquid ratio, adding a crystal transformation agent, stirring uniformly, carrying out crystal transformation reaction for 3-4h to obtain a mixed solution containing alpha semi-hydrated gypsum, and carrying out solid-liquid separation to obtain a finished product of alpha semi-hydrated gypsum. The method can be used for producing the high-quality alpha semi-hydrated gypsum, fully utilizes the reaction heat, reduces the whole production loss, improves the energy utilization rate, and accords with the environment-friendly, safe and high-quality production concept of a green factory.
Description
Technical Field
The application relates to the technical field of alpha hemihydrate gypsum preparation, in particular to a preparation method of alpha hemihydrate gypsum.
Background
Latest statistical data of China Association for phosphorus and fertilizer industries, china P in 2020 2 O 5 The yield reaches about 1600 million tons, the byproduct phosphogypsum is more than 8000 million tons, the utilization rate is about 40 percent, the newly increased phosphogypsum is stockpiled for 4800 million tons, the newly increased land occupation is 15000 mu each year, and the total stock reaches more than 6 hundred million tons. The stockpiling of a large amount of phosphogypsum not only occupies a large amount of land, but also can bring about dust pollution, landslide, underground water and soil pollution and other environmentsProblem, the treatment of phosphogypsum has become an environmental problem associated with the development of phosphorus chemical industry.
In order to solve the environmental protection problem brought by the phosphogypsum, the alpha-hemihydrate gypsum autoclaved production process disclosed by the publication number CN102659331A in the related technology comprises the following process steps: putting dihydrate gypsum into production equipment, and sealing; (2) heating dihydrate gypsum; (3) Keeping for 4-5 hours under the saturated steam pressure of 0.3-0.4 MPa to generate moist alpha-semi-hydrated gypsum; (4) Opening a steam exhaust valve, discharging the pressurized steam, and closing the steam exhaust valve; (5) Continuously heating, opening a valve of a steam extraction pipe, starting a vacuum pump, and keeping the vacuum degree in the equipment between 0.06MPa and 0.09MPa while extracting water vapor; until the alpha-hemihydrate gypsum is completely dried; (6) Stopping heating, closing the vacuum pump, and opening the discharging device to obtain a dry alpha-hemihydrate gypsum finished product.
Aiming at the alpha-hemihydrate gypsum steam-pressing production process in the related technology, the applicant finds that the technical scheme has the following defects: the pressurized water vapor method is adopted, so that the drying time is shortened, the production efficiency is improved, but the method needs a pressure container to be carried out at high temperature and high pressure, and has the problems of long steam pressure reaction time and high energy consumption.
Disclosure of Invention
In order to solve the technical problem, the application provides a preparation method of alpha hemihydrate gypsum.
The preparation method of the alpha hemihydrate gypsum is realized by the following scheme:
a preparation method of alpha semi-hydrated gypsum comprises the steps of firstly, crushing phosphorite into phosphorite powder for standby;
step two, adding water into concentrated sulfuric acid to dilute the concentrated sulfuric acid to 8-20%, collecting heat generated by diluting the concentrated sulfuric acid through a heat recovery system, adding the crushed phosphorite powder obtained in the step one into the diluted sulfuric acid solution, stirring and reacting for 1-3 hours to obtain slurry;
step three, extraction and separation: adding an extracting agent into the slurry obtained in the second step, wherein the extraction temperature is 50-60 ℃, the extraction time is 20-30 min, and carrying out mixed countercurrent extraction to remove an organic phase to obtain phosphogypsum powder and water phase mixed slurry, wherein the phosphogypsum powder and water phase mixed slurry contains sulfuric acid and phosphoric acid, the sulfuric acid accounts for 8-12% of the mass of the water body, and the phosphoric acid accounts for 12-15% of the mass of the water body; extracting and collecting crude phosphoric acid produced by the reaction of sulfuric acid solution and phosphorite powder in an organic phase, and washing and recovering the entrained phosphoric acid by the organic phase water for later use after heat in the organic phase is collected by a heat recovery system;
step four, sampling and detecting, then adding water, recovered phosphoric acid and dilute sulfuric acid, and controlling the concentration of the sulfuric acid to be 10 +/-0.5%, the concentration of the phosphoric acid to be 14 +/-0.5% and the solid-to-liquid ratio of the phosphogypsum powder to the water to be 40-50%;
step five, adding a crystal transformation agent, stirring uniformly, combining heat collected by a heat recovery system with supplementary heat, heating to 90-110 ℃ to perform crystal transformation reaction for 3-4h to obtain a mixed solution containing alpha semi-hydrated gypsum;
the crystal transformation agent is aluminum sulfate matched with one of citric acid, citrate, succinic acid and succinate;
the mass of the crystal transformation agent is equal to 0.12-0.25% of the mass of the water phase in the phosphogypsum powder and water phase mixed slurry;
step six, carrying out solid-liquid separation on the mixed liquid containing the alpha semi-hydrated gypsum to obtain a solid phase and a liquid phase, and carrying out phosphoric acid and sulfuric acid separation on the liquid phase to obtain phosphoric acid which is recycled as the recovered phosphoric acid in the step four; washing the solid phase with hot water, recycling the washing water, and washing to obtain alpha hemihydrate gypsum;
and the hot water heat source of the solid phase in the washing step six comprises heat recovered by a heat recovery system.
By adopting the technical scheme, the method can be used for producing the high-quality alpha semi-hydrated gypsum, fully utilizing the reaction heat, reducing the overall production loss, improving the energy utilization rate and meeting the environment-friendly, safe and high-quality production concept of a green factory.
Preferably, the crystal transformation agent is a compound of aluminum sulfate and succinic acid or succinate; the aluminum sulfate accounts for 25-40% of the total mass of the crystal modifier.
By adopting the technical scheme, the alpha hemihydrate gypsum is favorably converted into a short columnar crystal form, and the quality of the alpha hemihydrate gypsum is further improved.
Preferably, the crystal transformation agent is a compound of aluminum sulfate and succinate; the succinate is dipotassium succinate; the mass ratio of the aluminum sulfate to the dipotassium succinate is 1: (2-2.5); the length-diameter ratio of the alpha hemihydrate gypsum is 1.
By adopting the technical scheme, the alpha hemihydrate gypsum can be favorably converted into a short columnar crystal form, the length-diameter ratio of the alpha hemihydrate gypsum can be adjusted, and the quality of the alpha hemihydrate gypsum is further improved.
Preferably, the mass ratio of the aluminum sulfate to the dipotassium succinate is 32:68.
the mass ratio of aluminum sulfate to dipotassium succinate is 32:68 as a crystal modifier to produce the alpha semi-hydrated gypsum, not only reduces the difficulty of regulating and controlling the length-diameter ratio of the alpha semi-hydrated gypsum, but also has relatively low comprehensive production energy consumption on the premise of ensuring the quality of the alpha semi-hydrated gypsum.
Preferably, the extractant is prepared by P204 or naphthenic acid with cyclohexane; the mass of the cyclohexane accounts for 40-60% of the mass of the extracting agent.
Through adopting above-mentioned technical scheme, can promote crude phosphoric acid collection efficiency.
Preferably, the extractant is prepared from P204 and cyclohexane; the mass ratio of the P204 to the cyclohexane is 2:3.
by adopting the technical scheme, the crude phosphoric acid collection efficiency can be further improved.
Preferably, the heat recovery system comprises a normal-temperature heat exchange medium storage tank, a concentrated sulfuric acid dilution tank, an organic phase washing tank, an energy storage tank group, a crystal form conversion storage tank and a heat preservation communication pipe network, wherein a normal-temperature heat exchange medium in the normal-temperature heat exchange medium storage tank flows to a jacket layer of the concentrated sulfuric acid dilution tank through the heat preservation communication pipe network, a normal-temperature heat exchange medium which absorbs heat generated by dilution of the concentrated sulfuric acid flows to the energy storage tank group through the heat preservation communication pipe network, and the heat generated by dilution of the absorbed concentrated sulfuric acid is stored in the energy storage tank group; the normal-temperature heat exchange medium in the normal-temperature heat exchange medium storage tank flows to a jacket layer of the organic-phase washing tank through the heat-preservation communicating pipe network, the normal-temperature heat exchange medium absorbing heat of the organic-phase liquid material flows to the energy storage tank group through the heat-preservation communicating pipe network, and recycling of organic-phase waste heat is completed; and the heat exchange medium output from the energy storage tank group is input into the jacket layer of the crystal transformation storage tank through the heat-preservation communicating pipe network, and the liquid material in the crystal transformation storage tank is heated to 90-110 ℃.
By adopting the technical scheme, the heat recovery system can fully utilize reaction heat, reduce the whole production loss, improve the energy utilization rate and accord with the environmental-friendly, safe and high-quality production concept of a green factory.
Preferably, the concentrated sulfuric acid dilution tank comprises an inner container tank body and an outer shell tank body, and a heat exchange jacket is formed between the inner container tank body and the outer shell tank body; the bottom of the heat exchange jacket is communicated with a normal-temperature heat exchange medium storage tank, and the top of the heat exchange jacket is communicated with the energy storage tank group; the heat insulation filler is integrally formed inside the shell tank body; the inner container tank body is mainly formed by die casting a metal framework, an acid-resistant resin matrix, glass fiber powder and a heat-conducting filler; the heat conducting filler comprises an acid corrosion resistant ceramic carrier and a heat conducting substance, wherein the heat conducting substance is fixedly connected to the surface of the acid corrosion resistant ceramic carrier through chemical deposition or physical vapor deposition.
The core difficulty of the heat recovery system of the present application is: and recovering heat energy generated by diluting concentrated sulfuric acid. In the laboratory test process, concentrated sulfuric acid can be diluted to obtain a sulfuric acid aqueous solution with ideal concentration by adopting a glass material, but the concentrated sulfuric acid dilution cannot be completed by adopting a large container made of the glass material on the basis of practical considerations such as cost, actual production difficulty and the like in industrial production. At present, in the industrial production, concentrated sulfuric acid dilutes the pressure vessel of glass steel material that adopts, however the pressure vessel of glass steel material has acidproof wear resistance, but its self heat conductivility is relatively poor, and this has just caused the problem that concentrated sulfuric acid dilutes the heat energy that produces and can't effectively retrieve. The technical scheme who this application adopted can solve above-mentioned problem, the inner bag jar body mainly adopts metal framework, the acidproof resin base member, fine powder of glass in this application, heat conduction filler die casting forms, both guaranteed the weatherability corrosivity of the inner bag jar body, mechanical strength, the overall quality has been reduced again, be convenient for assemble, the transportation provides basic assurance with improving holistic heat conductivility for the heat recovery that concentrated sulfuric acid dilutes the production, in addition, the die casting production technology of the inner bag jar body is simple controllable relatively, the production degree of difficulty and the manufacturing cost of the inner bag jar body have been reduced.
Preferably, the acid-resistant resin matrix is at least one of ES-1001N and ES-1002T; the acid corrosion resistant ceramic carrier is microcrystalline mica ceramic powder; the heat conducting substance is at least one of silver, copper, aluminum, tin, bismuth and carbon nano tubes; the glass fiber powder is C glass fiber powder with the granularity controlled between 500 and 2000 meshes; the metal framework is made of aluminum alloy material; the heat-conducting filler accounts for 5-8% of the total mass of the acid-resistant resin matrix.
By adopting the technical scheme, the ES-1001N and ES-1002T silicone resins can effectively ensure the chemical corrosion resistance and the heat resistance of the tank, and the service life of the liner tank body of the tank is ensured. The microcrystalline mica ceramic powder has good chemical corrosion resistance and can form a heat-conducting network by combining with a heat-conducting substance, so that the heat-conducting property of the liner tank body is improved. The metal framework made of the aluminum alloy material has good compatibility with ES-1001N and ES-1002T silicon resin, and can form a compact heat conduction network by combining with a heat conduction filler which is uniformly dispersed, so that the heat conduction performance of the aluminum alloy material is effectively improved, the heat exchange effect is improved, and the heat recovery efficiency can be effectively improved.
Preferably, the energy storage tank group comprises a first heat exchange medium storage tank for collecting heat exchange media passing through a jacket layer of the concentrated sulfuric acid dilution tank, a second heat exchange medium storage tank for collecting heat exchange media absorbing heat of the organic phase liquid material, a third heat exchange medium storage tank, a hot supplement tank and a constant temperature heat exchange medium storage tank, wherein the first heat exchange medium storage tank is communicated with a heat exchange medium outlet pipe of the jacket layer of the concentrated sulfuric acid dilution tank through a heat preservation communication pipe network; the first heat exchange medium storage tank is communicated with the hot replenishing tank through a heat preservation communicating pipe network; the second heat exchange medium storage tank is communicated with the heat exchange medium outlet pipe of the jacket layer of the organic phase washing tank through a heat insulation communication pipe network; the second heat exchange medium storage tank is communicated with the hot replenishing tank through a heat preservation communicating pipe network; the third heat exchange medium storage tank is communicated with a heat exchange medium outlet pipe of the jacket layer of the crystal conversion storage tank through a heat preservation communication pipe network; the third heat exchange medium storage tank is communicated with the hot supplement tank through a heat preservation communicating pipe network; the heat supplement tank is communicated with the constant-temperature heat exchange medium storage tank through a heat preservation communicating pipe network; the constant-temperature heat exchange medium storage tank is communicated with the heat exchange medium inlet pipe of the jacket layer of the crystal conversion storage tank through a heat-preservation communicating pipe network.
Through adopting above-mentioned technical scheme, the energy storage tank crowd of the different designs of demand of heating according to each workshop section, not only can satisfy alpha hemihydrate gypsum's production demand, and to heat subregion adjustment ability intensity, heat utilization rate is high, effectively reduce invalid heat transmission, optimize the heat utilization management and control, effectively promote heat recovery efficiency, accord with the environmental protection safety high quality production theory of green mill, simultaneously can reduce the expense of electricity heating production for the enterprise, alleviate the social problem of electric tension, change the rugged energy utilization form of trade, accelerate traditional enterprise transformation.
In summary, the present application has the following advantages:
1. the method can produce high-quality alpha semi-hydrated gypsum, fully utilize reaction heat, reduce the overall production loss, improve the energy utilization rate and relieve the social problem of electric power shortage.
2. The heat recovery system that this application adopted has solved the heat utilization difficult problem of core, effectively promotes heat recovery efficiency, accords with the environmental protection safety high quality production theory of green mill.
3. The inner container jar body of production has good weatherability corrosivity, mechanical strength in this application, and whole quality is slim and graceful relatively, and the equipment of being convenient for, transportation improve holistic heat conductivility and provide basic assurance for the heat recovery that concentrated sulfuric acid dilutes the production. In addition, the die casting production process of the inner container tank body is relatively simple and controllable, and the production difficulty and the production cost of the inner container tank body are reduced.
Drawings
Fig. 1 is a schematic diagram of the overall structure of the heat recovery system of the present application.
Fig. 2 is a schematic diagram of the structure of a concentrated sulfuric acid dilution tank in the heat recovery system of the present application.
FIG. 3 is a schematic view of a linkage connection structure of a rotating shaft and a concentrated sulfuric acid draft tube in the concentrated sulfuric acid dilution tank.
Fig. 4 is a schematic diagram of the construction of the insulating filler in the heat recovery system of the present application.
In the figure, 1, a normal temperature heat exchange medium storage tank; 2. a concentrated sulfuric acid dilution tank; 20. a heat exchange jacket; 200. closing plates; 201. a rubber seal ring; 21. a liner tank body; 211. a spiral heat dissipating wire; 22. a shell tank body; 220. a thermally insulating filler; 221. a first joint; 222. a second joint; 23. an acid liquor adding pipe; 231. an extract liquid extraction pipe; 24. a phosphorite powder adding pipe; 241. a phosphogypsum powder and water phase mixed slurry extraction pipe; 25. a rotating shaft; 251. a drive motor; 252. a pitched blade stirring paddle; 253. a spiral conveyor belt; 254. a first vortex type stirring paddle; 26. a concentrated sulfuric acid adding component; 261. a concentrated sulfuric acid draft tube; 2611. a flow guide port; 262. a concentrated sulfuric acid input pipe; 263. a second vortex type stirring paddle; 264. a driven gear; 265. a linkage rod; 266. a driving gear; 267. a first pulley; 268. a second pulley; 269. a belt; 3. an organic phase water washing tank; 4. an energy storage tank group; 41. a first heat exchange medium storage tank; 42. a second heat exchange medium storage tank; 43. a third heat exchange medium storage tank; 44. a heat-replenishing tank; 45. a constant temperature heat exchange medium storage tank; 5. a crystal form conversion storage tank; 6. a heat-preservation communication pipe network; 7. aerogel felt cloth; 71. an aluminum foil sheet; 72. polyurethane foam.
Detailed Description
The present application will be described in further detail below with reference to the drawings, comparative examples and examples.
Preparation examples
The heat conducting filler is prepared by taking microcrystalline mica ceramic powder as a carrier and carbon nano tubes as heat conducting substances.
The preparation method of the heat-conducting filler comprises the following steps:
step one, preparing microcrystalline mica ceramic powder:
s1.1, preparing materials: 1818g of zirconium oxide ZrO were weighed 2 Raw material, 58.6g of magnesium oxide MgO, and 68.4g of aluminum oxide Al 2 O 3 25.7g of calcium oxide CaO, 128.3g of yttrium oxide, 3.5g of silicon nitride whisker, 4g of potassium titanate whisker and 3.5g of zinc oxide whisker, and placing the materials in a high-speed stirring kettle to be mixed and stirred for 20min at 500rpm for later use;
s1.2, placing the mixture in the S1.1 in a planetary ball mill for grinding: after dry grinding for 15min at the grinding speed of 180rpm, adding 2000mL of anhydrous alcohol for wet ball milling for 2.0h, transferring the mixed powder after ball milling into an oven, and drying for 1.0h at 100 ℃ for later use;
s1.3, transferring the mixed powder in S1.2 into a muffle furnace, calcining for 3.0h at 780 ℃, discharging, putting into a planetary ball mill, performing wet ball milling for 2.0h under the same ball milling conditions as those in S1.2, transferring the ball-milled mixed powder into an oven, drying for 1.0h at 100 ℃, screening by using a screen of 400-500 meshes to obtain mixed powder of 400-500 meshes, performing isostatic pressing granulation at 60MPa, isostatic pressing for molding at 240MPa, transferring into the muffle furnace, sintering for 3.0h at 1720 ℃ and MgO atmosphere, and then sintering into Al at 1350 ℃ and Al 2 O 3 And (4) performing heat treatment on the embedded materials for 12 hours, naturally cooling, and performing ball milling and crushing to obtain the microcrystalline mica ceramic powder.
Step two, adding 0.8mol of 2-ethyl-4-methylimidazole 2E4MI and 0.4mol of silver acetate AgAc into 16L of dichloromethane at room temperature, magnetically stirring at the rotating speed of 240r/min for 100min until AgAc particles completely disappear to obtain clear and transparent Ag (2E 4 MI) 2 Ac complex solution in Ag (2E 4 MI) 2 Adding 20g of CNTs and 20g of PVP into the Ac complex solution, performing ultrasonic dispersion (the power of an ultrasonic generator is 1200W, the frequency is 20 kHz) for 3h, adding 2000 g of microcrystalline mica ceramic powder in S1.3, and continuing to perform ultrasonic dispersion for 0.5h to obtain dispersion liquid;
and step three, carrying out reduced pressure distillation treatment on the dispersion liquid, removing dichloromethane in the dispersion liquid, then carrying out high-temperature sintering treatment on the solid, controlling the high-temperature sintering temperature at 210 ℃, and carrying out high-temperature sintering for 4 hours to obtain the solid, placing the solid in a three-roller machine for 3 times of grinding and crushing, dispersing the solid in 16L ethanol at a roller spacing of 15 micrometers of the three-roller machine, pouring the solid into a basket grinder for grinding, grinding for 0.5 hour at the rotating speed of 2000r/min, and then filtering and drying to obtain the micaceous microcrystalline ceramic powder-CNTs hybrid material.
Device
Referring to fig. 1, the heat recovery system includes a normal temperature heat exchange medium storage tank 1, a concentrated sulfuric acid dilution tank 2, an organic phase washing tank 3, an energy storage tank group 4, a crystal form conversion storage tank 5, and a heat preservation communication pipe network 6. The normal-temperature heat exchange medium storage tank 1 stores a normal-temperature heat exchange medium, and the heat exchange medium is selected from tap water or an ethanol water solution with a volume ratio of 1. The normal temperature heat transfer medium in the normal temperature heat transfer medium storage tank 1 flows to the jacket layer of the concentrated sulfuric acid dilution tank 2 through the heat preservation communicating pipe network 6, and the heat generated by diluting the concentrated sulfuric acid in the concentrated sulfuric acid dilution tank 2 by adopting the normal temperature heat transfer medium coefficient is adopted.
Referring to fig. 1, the energy storage tank group 4 includes a first heat exchange medium storage tank 41 for collecting a heat exchange medium passing through a jacket layer of the concentrated sulfuric acid dilution tank 2, a second heat exchange medium storage tank 42 for collecting a heat exchange medium absorbing heat of an organic phase liquid material, a third heat exchange medium storage tank 43, a hot-replenishing tank 44, and a constant-temperature heat exchange medium storage tank 45. Wherein, the first heat exchange medium storage tank 41 is communicated with the heat exchange medium outlet pipe of the jacket layer of the concentrated sulfuric acid dilution tank 2 through a heat preservation communicating pipe network 6. The first heat exchange medium storage tank 41 is communicated with the heat supplement tank 44 through the heat preservation communication pipe network 6, heat of the heat supplement tank 44 is supplemented and then input into the constant temperature heat exchange medium storage tank 45, and a heating medium in the constant temperature heat exchange medium storage tank 45 is used for heating the crystal form conversion storage tank 5 and maintaining the temperature of materials to be constant. The second heat exchange medium storage tank 42 is communicated with the heat exchange medium outlet pipe of the jacket layer of the organic phase washing tank 3 through a heat preservation communication pipe network 6, and the second heat exchange medium storage tank 42 is communicated with the heat supplement tank 44 through the heat preservation communication pipe network 6 and is input into the constant temperature heat exchange medium storage tank 45 after heat supplement of the heat supplement tank 44.
Referring to fig. 1, the third heat exchange medium storage tank 43 is communicated with the heat exchange medium outlet pipe of the jacket layer of the crystal conversion storage tank 5 through the heat preservation communication pipe network 6. The third heat exchange medium storage tank 43 is communicated with the heat supplement tank 44 through the heat preservation communicating pipe network 6, the heat supplement tank 44 is communicated with the constant temperature heat exchange medium storage tank 45 through the heat preservation communicating pipe network 6, and the heating medium in the constant temperature heat exchange medium storage tank 45 is used for heating the crystal form conversion storage tank 5 and maintaining the temperature of the materials to be constant.
Referring to fig. 1, the normal temperature heat exchange medium that absorbs the heat generated by diluting the concentrated sulfuric acid flows to the first heat exchange medium storage tank 41 of the energy storage tank group 4 through the heat preservation communication pipe network 6, that is, the heat generated by diluting the absorbed concentrated sulfuric acid is stored in the energy storage tank group 4. In addition, the normal temperature heat exchange medium in the normal temperature heat exchange medium storage tank 1 flows to the jacket layer of the organic phase washing tank 3 through the heat preservation communicating pipe network 6, and the normal temperature heat exchange medium absorbing heat of the organic phase liquid material flows to the second heat exchange medium storage tank 42 of the energy storage tank group 4 through the heat preservation communicating pipe network 6, so that the recycling of the organic phase waste heat is completed. The heat exchange medium output by the constant-temperature heat exchange medium storage tank 45 in the energy storage tank group 4 is input into the jacket layer of the crystal transformation storage tank 5 through the heat-preservation communicating pipe network 6, and the liquid material in the crystal transformation storage tank 5 is heated and controlled at the temperature of 90-110 ℃, so that the dihydrate gypsum is transformed into the high-quality alpha hemihydrate.
Referring to fig. 2, the concentrated sulfuric acid dilution tank 2 includes an inner container tank 21 and a housing tank 22, the inner container tank 21 is embedded in the housing tank 22, and a gap between the inner container tank 21 and the housing tank 22 is sealed by silicone sealant, so that a heat exchange jacket 20 is formed in the concentrated sulfuric acid dilution tank 2. The liner tank 21 is fixedly connected with a sealing plate 200 through bolts. The outer wall of the closing plate 200 is sleeved with a rubber sealing ring 201. The lower surface of the rubber sealing ring 201 is fixedly connected to the upper surfaces of the liner tank body 21 and the shell tank body 22 through silicone sealant, so that a better sealing effect is achieved. In order to ensure the heat exchange effect, the outer wall of the inner container tank body 21 is integrally formed with a spiral heat radiation wire 211.
Referring to fig. 2, a first joint 221 is fixedly connected to the circumferential bottom of the housing tank 22. One end of the first joint 221 is fixedly communicated with the bottom of the heat exchange jacket 20, and the other end of the first joint is fixedly communicated with the normal-temperature heat exchange medium storage tank 1, so that the normal-temperature heat exchange medium storage tank 1 is communicated with the heat exchange jacket 20 through the heat-insulation communicating pipe network 6. A second joint 222 is fixedly connected to the upper portion of the peripheral side of the outer shell can 22. One end of the second joint 222 is fixedly communicated with the top of the heat exchange jacket 20, and the other end is fixedly communicated with the heat preservation pipe, namely fixedly communicated with the first heat exchange medium storage tank 41 of the energy storage tank group 4 through the heat preservation communication pipe network 6.
Referring to fig. 2, the sealing plate 200 is fixedly connected to an acid solution adding pipe 23 and a phosphate rock powder adding pipe 24. The acid liquor adding pipe 23 is used for adding dilute sulfuric acid and recycled phosphoric acid and water, and the phosphorite powder adding pipe 24 is used for adding phosphorite powder, so that the aims of controlling the concentration of the phosphoric acid to be 10 +/-0.5%, the concentration of the sulfuric acid to be 14 +/-0.5% and the solid-to-liquid ratio of the phosphogypsum powder to the water to be 40-50% are fulfilled. The sealing plate 200 is fixedly communicated with an extraction liquid extraction pipe 231, a phosphogypsum powder and water phase mixed slurry extraction pipe 241. The extraction liquid extraction pipe 231, the phosphogypsum powder and water phase mixed slurry extraction pipe 241 are one of heat preservation communication pipe networks 6, and have good heat preservation performance. The organic phase water washing tank 3 is communicated with the concentrated sulfuric acid dilution tank 2 through an extraction liquid extraction pipe 231, the mixed countercurrent extraction is carried out to remove the organic phase, the organic phase flows into the organic phase water washing tank 3 through the extraction liquid extraction pipe 231, and the organic phase water washing tank 3 is used for washing and recovering the entrained phosphoric acid. The phosphogypsum powder and water phase mixed slurry extraction pipe 241 is used for carrying out solid-liquid separation on liquid materials which finish crystal transformation reaction to obtain alpha hemihydrate gypsum.
Referring to fig. 2, a rotary shaft 25 is rotatably connected to the center of the upper surface of the sealing plate 200. The shrouding 200 is worn to establish in pivot 25 one end and is located the outside of concentrated sulfuric acid dilution tank 2, and the shrouding 200 is worn to establish in the other end of pivot 25 and is located the inside of concentrated sulfuric acid dilution tank 2. The rotating shaft 25 penetrating through the sealing plate 200 and located outside the concentrated sulfuric acid dilution tank 2 is coaxially and fixedly connected with a driving motor 251 through a coupler, and the driving motor 251 is fixedly connected to the upper surface of the sealing plate 200. The rotating shaft 25 penetrating the sealing plate 200 and located inside the concentrated sulfuric acid dilution tank 2 is circumferentially and fixedly connected with an inclined blade stirring paddle 252, a spiral conveying belt 253 and a first vortex type stirring paddle 254. The spiral conveyer belt 253 is positioned between the inclined blade stirring paddle 252 and the first vortex stirring paddle 254. The height of the inclined blade stirring paddle 252 is equal to 0.7-0.78 times of the height of the inner container tank body 21. The shaft end of the rotating shaft 25 penetrating through the sealing plate 200 and positioned in the concentrated sulfuric acid dilution tank 2 is rotatably connected to the center of the inner bottom surface of the inner container tank body 21. The first vortex type stirring paddle 254 is fixedly connected to the peripheral side of the shaft end of the rotating shaft 25, and a gap of 6-10cm is reserved between the first vortex type stirring paddle 254 and the inner bottom surface of the inner container tank body 21.
Referring to fig. 2, the sealing plate 200 is fixedly connected with at least two concentrated sulfuric acid adding assemblies 26. The two concentrated sulfuric acid adding assemblies 26 are symmetrically arranged about the rotating shaft 25. The concentrated sulfuric acid adding assembly 26 includes a concentrated sulfuric acid guiding pipe 261, and the concentrated sulfuric acid guiding pipe 261 is rotatably connected to the lower surface of the sealing plate 200. The upper surface of the sealing plate 200 is fixedly connected with a concentrated sulfuric acid input pipe 262. The concentrated sulfuric acid input pipe 262 and the concentrated sulfuric acid draft pipe 261 are connected together in a rotating and sealing manner. The concentrated sulfuric acid input pipe 262 is provided with an electromagnetic valve and a flowmeter. The concentrated sulfuric acid draft tube 261 is provided with a draft opening 2611 communicated with the concentrated sulfuric acid input tube 262 in a circumferential direction in a penetrating manner. The diversion ports 2611 are distributed around the concentrated sulfuric acid diversion pipe 261 in a dot matrix manner. The length of the concentrated sulfuric acid draft tube 261 opened with the draft opening 2611 is 0.6-0.8 times of the total length of the concentrated sulfuric acid draft tube 261. The bottom end of the concentrated sulfuric acid draft tube 261 is closed, and the bottom end of the concentrated sulfuric acid draft tube 261 is circumferentially and fixedly connected with a second vortex type stirring paddle 263. The vertical distance from the bottom end of the concentrated sulfuric acid draft tube 261 to the inner bottom surface of the inner container tank body 21 is equal to 0.3-0.36 time of the total height of the inner container tank body 21.
Referring to fig. 2 and 3, a driven gear 264 is fixedly connected to the concentrated sulfuric acid guiding pipe 261 in the circumferential direction, and a gap of 0.5-1cm is left between the driven gear 264 and the lower surface of the sealing plate 200. The closing plate 200 is rotatably connected with a linkage rod 265. The shrouding 200 is worn to establish by gangbar 265 one end and is located the outside of concentrated sulfuric acid dilution jar 2, and the other end wears to establish shrouding 200 and is located the inside of concentrated sulfuric acid dilution jar 2. The linkage rod 265 penetrating through the sealing plate 200 and located inside the concentrated sulfuric acid dilution tank 2 is circumferentially and fixedly connected with a driving gear 266, and the driving gear 266 is meshed with a driven gear 264. The linkage rod 265 penetrating through the sealing plate 200 and located outside the concentrated sulfuric acid dilution tank 2 is circumferentially and fixedly connected with a first belt pulley 267. Wear to establish shrouding 200 and be located outside the concentrated sulfuric acid dilution tank 2 pivot 25 circumference fixedly connected with second belt pulley 268. A belt 269 is fitted between the first pulley 267 and the second pulley 268. The drive motor 251 drives the pivot 25 circumference, and the pivot 25 rotates under the transmission of belt 269 around self axial rotation, and gangbar 265 rotates around self axial, and driving gear 266 drives driven gear 264 and rotates for concentrated sulfuric acid honeycomb duct 261 rotates around self axial, realizes the purpose of rapid dilution concentrated sulfuric acid, and the heat that produces is diluted to steerable concentrated sulfuric acid, is convenient for carry out the heat recovery regulation and control.
Referring to fig. 4, in order to reduce heat loss, an insulating filler 220 is integrally formed inside the outer shell can 22. The heat insulation filler 220 is made of composite heat insulation cotton. The composite heat-preservation cotton comprises aerogel felt cloth 7 as a core layer, and aluminum foil pieces 71 and polyurethane cotton 72 which are compounded on the upper surface and the lower surface of the aerogel felt cloth 7. The polyurethane foam 72 is bonded on the surface of the aluminum foil 71 opposite to the aerogel felt 7 by hot melt adhesive.
In addition, solenoid valve and temperature detector have all been installed at the insulating tube both ends between normal atmospheric temperature heat transfer medium storage tank 1 and concentrated sulfuric acid dilution tank 2, and temperature detector connects in the wiring end of digital display screen, and digital display screen shows normal atmospheric temperature heat transfer medium outflow temperature T1 and the normal atmospheric temperature heat transfer medium temperature T2 before entering the heat transfer jacket 20 of concentrated sulfuric acid dilution tank 2. Electromagnetic valves and temperature detectors are arranged at two ends of the heat preservation pipe between the concentrated sulfuric acid dilution tank 2 and the first heat exchange medium storage tank 41, the temperature detectors are connected to wiring ends of a digital display screen, and the digital display screen displays the output heat exchange medium temperature T3 after heat exchange through the heat exchange jacket 20 and the heat exchange medium temperature T4 before entering the first heat exchange medium storage tank 41.
Solenoid valve and temperature detector have all been installed at the insulating tube both ends between normal atmospheric temperature heat transfer medium storage tank 1 and the organic phase washing jar 3, and the temperature detector connects in digital display screen's wiring end, and digital display screen shows normal atmospheric temperature heat transfer medium outflow temperature T1 and gets into normal atmospheric temperature heat transfer medium temperature T5 before organic phase washing jar 3 presss from both sides the jacket layer. Solenoid valve and temperature detector have all been installed at the insulating tube both ends between organic phase washing jar 3 and the second heat transfer medium storage tank 42, and the temperature detector connects in digital display screen's wiring end, and digital display screen shows through organic phase washing jar 3 press from both sides output heat transfer medium temperature T6 after jacket layer heat transfer and heat transfer medium temperature T7 before getting into second heat transfer medium storage tank 42.
Solenoid valves and temperature detectors are arranged at two ends of the heat preservation pipe between the constant-temperature heat exchange medium storage tank 45 and the crystal type conversion storage tank 5, the temperature detectors are connected to wiring ends of a digital display screen, and the digital display screen displays the temperature T8 of a heating medium flowing out of the constant-temperature heat exchange medium storage tank 45 and the temperature T9 of the heating medium flowing into the front of a jacket layer of the crystal type conversion storage tank 5. Electromagnetic valves and temperature detectors are arranged at two ends of the heat preservation pipe between the crystal transformation storage tank 5 and the third heat exchange medium storage tank 43, the temperature detectors are connected to wiring ends of a digital display screen, and the digital display screen displays the temperature T10 of the medium flowing out of the jacket layer of the crystal transformation storage tank 5 after heat exchange and the temperature T11 of the medium before flowing into the third heat exchange medium storage tank 43.
An electromagnetic valve and a temperature detector are installed on a heat preservation pipe fixedly communicated with the bottom of the first heat exchange medium storage tank 41, the temperature detector is connected to a wiring terminal of a digital display screen, and the digital display screen displays the temperature T12 of the heat exchange medium in the flow in the first heat exchange medium storage tank 41.
An electromagnetic valve and a temperature detector are installed on a heat preservation pipe fixedly communicated with the bottom of the second heat exchange medium storage tank 42, the temperature detector is connected to a wiring terminal of a digital display screen, and the digital display screen displays the temperature T13 of the heat exchange medium in the flow in the second heat exchange medium storage tank 42.
An electromagnetic valve and a temperature detector are installed on the heat preservation pipe fixedly communicated with the bottom of the third heat exchange medium storage tank 43, the temperature detector is connected to a wiring terminal of a digital display screen, and the digital display screen displays the temperature T14 of the heat exchange medium in the flow in the third heat exchange medium storage tank 43.
The insulating pipe that communicates in 41 bottoms of first heat transfer medium storage tanks, the insulating pipe that communicates in 42 bottoms of second heat transfer medium storage tanks and the insulating pipe that communicates in 43 bottoms of third heat transfer medium storage tanks all fix the circumference that communicates in the insulating pipe that another specification is slightly bigger, and the insulating pipe one end that this specification is slightly bigger is sealed, and the other end communicates in hot-patch jar 44 lateral wall upper portion. An electromagnetic valve and a temperature detector are arranged on the slightly larger heat preservation pipe close to the upper part of the outer side wall of the heat supplementing tank 44, the temperature detector is connected to a terminal of a digital display screen, and the digital display screen displays the temperature T15 of the heat exchange medium before being input into the heat supplementing tank 44. The heating power of the heat supplement tank 44 can be adjusted according to T15, heat supplement is completed quickly, the temperature is raised to an ideal temperature efficiently, and the production efficiency is improved. The heating medium completing the hot patching in the hot patching tank 44 is input into the constant-temperature heat exchange medium storage tank 45 to be used for regulating and controlling the temperature of the material in the crystal conversion storage tank 5, so that the high-efficiency utilization of heat is realized, the overall production loss is reduced, the energy utilization rate is improved, and the environment-friendly, safe and high-quality production concept of a green factory is met.
The tank body 21 of the liner in the concentrated sulfuric acid diluting tank 2 is made of an aluminum alloy framework, 500-2000-mesh C glass fiber powder, ES-1001N silicon resin and the microcrystalline mica ceramic powder-CNTs hybrid material in the preparation example 1. The mass of the microcrystalline mica ceramic powder-CNTs hybrid material in the preparation example 1 is 0.06 times that of ES-1001N silicone resin. The mass of the 500-2000 mesh C glass fiber powder is 0.03 times of that of ES-1001N silicone resin.
The preparation method of the liner tank body comprises the following steps:
step one, preparing die casting resin: weighing 18.2kg of ES-1001N silicon resin, 0.6kg of 500-2000 mesh C glass fiber powder and 1.2kg of the microcrystalline mica ceramic powder-CNTs hybrid material in the preparation example 1, placing the materials in a high-speed stirring kettle, keeping the temperature between 4 and 10 ℃, stirring the materials at 400rpm for 20min, defoaming the materials in vacuum, and heating to remove 75 percent of organic solvent carried in the ES-1001N silicon resin to obtain die casting resin;
and step two, placing the aluminum alloy framework in a forming die, injecting the die casting resin prepared in the step one into the forming die, wherein the liquid level of the die casting resin is higher than the upper surface of the aluminum alloy framework, namely, the aluminum alloy framework is immersed in the die casting resin, heating to remove the organic solvent carried by the residual 25% of the ES-1001N silicon resin, the aluminum alloy framework is immersed in the die casting resin, the liquid level of the die casting resin is 1-2cm higher than the upper surface of the aluminum alloy framework, heating to 140 ℃, pressurizing to 2.0MPa, curing for 4h, demolding and polishing to obtain the liner tank body.
Examples
Example 1
The application discloses a preparation method of alpha hemihydrate gypsum, which comprises the following steps:
crushing phosphate ore into phosphate ore powder for later use;
step two, concentrated sulfuric acid is uniformly added into the inner container tank body 21 through a concentrated sulfuric acid draft tube 261, a driving motor 251 works in the concentrated sulfuric acid adding process to drive a rotating shaft 25 to rotate and the concentrated sulfuric acid draft tube 261 to rotate, so that heat generated by dilution of the concentrated sulfuric acid is quickly exchanged by water, the heated water in the inner container tank body 21 exchanges heat with a normal-temperature heat exchange medium in a heat exchange jacket 20 of the concentrated sulfuric acid dilution tank 2, the heat exchange medium absorbs the heat generated by dilution of the concentrated sulfuric acid and sequentially flows through a heat insulation communicating pipe network 6 to form a first heat exchange medium storage tank 41, a heat supplement filling tank 44 and a constant-temperature heat exchange medium storage tank 45 (heat of the heat exchange medium in the constant-temperature heat exchange medium storage tank 45 is used for heating and temperature maintenance of a crystal form conversion storage tank 5), namely, a heat recovery system realizes heat recovery of dilution of the concentrated sulfuric acid, the concentrated sulfuric acid is stopped to be added after the difficulty of the sulfuric acid in the concentrated sulfuric acid dilution tank 2 reaches 10%, phosphate rock powder crushed in the step one is added into the inner container body 21 through a phosphate powder adding tube 24 for stirring reaction, the stirring reaction is carried out, and the stirring reaction is carried out after the temperature is reduced to 60 ℃, and the normal-temperature slurry is obtained after 3.0 h;
step three, extraction and separation: an extracting agent is added into the inner container tank body 21 through a phosphorite powder adding pipe 24, the extracting agent is prepared by P204 or naphthenic acid matched with cyclohexane, and the mass ratio of the P204 to the cyclohexane is 2:3, performing mixed countercurrent extraction at the extraction temperature of 55 ℃ for 30min, taking the organic phase away through an extraction liquid extraction pipe 231, wherein the residual liquid material of the inner container tank body 21 is mixed slurry of phosphogypsum powder and water, the mixed slurry of the phosphogypsum powder and the water contains sulfuric acid and phosphoric acid, the sulfuric acid accounts for 8-12% of the mass of the water, and the phosphoric acid accounts for 12-15% of the mass of the water;
the organic phase taken away by the extraction liquid extraction pipe 231 flows into the organic phase washing tank 3, the organic phase in the organic phase washing tank 3 exchanges heat by adopting a normal-temperature medium, a heat exchange medium absorbing heat of the organic phase sequentially passes through the second heat exchange medium storage tank 42, the heat replenishing tank 44 and the constant-temperature heat exchange medium storage tank 45 (heat energy of the heat exchange medium in the constant-temperature heat exchange medium storage tank 45 is used for heating and maintaining the temperature of the crystal form conversion storage tank 5), namely, the heat recovery system realizes heat recovery of the organic phase, when the temperature of the organic phase is reduced to be below 28 ℃, phosphoric acid carried by the organic phase is recovered by adopting normal-temperature water washing, and the preparation and collection of crude phosphoric acid are completed;
sampling and detecting the phosphogypsum powder and water phase mixed slurry, and performing the operation of the next working section when the concentration of phosphoric acid in the phosphogypsum powder and water phase mixed slurry is 10 +/-0.5%, the concentration of phosphoric acid is 14 +/-0.5% and the solid-to-liquid ratio of the phosphogypsum powder to water is 45-46%; otherwise, adding 25% of dilute sulfuric acid into the inner container tank body 21 through an acid liquid adding pipe 23, recovering concentrated 30% of phosphoric acid, adjusting the concentration of sulfuric acid in the phosphogypsum powder and water phase mixed slurry to be 10% +/-0.5%, the concentration of phosphoric acid to be 14 +/-0.5%, and the solid-liquid ratio of the phosphogypsum powder to water to be 45-46%, and then transferring the mixture into a crystal form conversion storage tank 5 through a phosphogypsum powder and water phase mixed slurry extracting pipe 241 to prepare for crystal conversion reaction;
step five, adding a crystal transformation agent into the crystal transformation storage tank 5, wherein the crystal transformation agent is a compound of aluminum sulfate and dipotassium succinate, and the mass ratio of the aluminum sulfate to the dipotassium succinate is 32:68, the crystal modifier is 0.2 percent of the mass of the water phase in the phosphogypsum powder and water phase mixed slurry, and after a compound of aluminum sulfate and dipotassium succinate is added, the mixture is stirred for 6 to 8min at the speed of 300pm and is uniformly stirred;
adding a crystal transformation agent, simultaneously inputting constant-temperature water with the temperature controlled at 98 ℃ in a constant-temperature heat exchange medium storage tank 45 into a jacket layer of the crystal transformation storage tank 5, starting electric heating of the crystal transformation storage tank 5 to maintain the temperature of liquid materials at 98 ℃, and starting crystal transformation reaction for 3.5 hours to obtain mixed liquid containing alpha semi-hydrated gypsum;
the heat exchange medium in the crystal conversion storage tank 5 flows to the third heat exchange medium storage tank 43, the hot replenishing tank 44 and the constant-temperature heat exchange medium storage tank 45 in sequence, so that the circulation of the heat exchange medium is completed, and the production effect is improved;
step six, carrying out solid-liquid separation on the mixed liquid containing the alpha semi-hydrated gypsum by adopting a tape filter type to obtain a solid phase and a liquid phase, and after carrying out phosphoric acid and sulfuric acid separation on the liquid phase, recycling the obtained phosphoric acid as the recovered phosphoric acid in the step four; the solid phase is washed by the stored hot water in the third heat exchange medium storage tank 43, the water temperature is 90-93 ℃, the washing water is filtered to remove suspended and particle impurities and then is input into the second heat exchange medium storage tank 42 to realize water body recycling, and the alpha semi-hydrated gypsum is obtained by washing. The content of the obtained alpha hemihydrate gypsum water-soluble phosphorus is below 0.1 percent.
In the process of transforming the dihydrate gypsum into the hemihydrate gypsum, the method greatly reduces the intercrystalline phosphorus in the dihydrate gypsum crystal lattice and the unreacted phosphorus in the phosphorite, so that the total P in the phosphogypsum 2 O 5 The content is reduced to below 0.3 percent, and compared with the traditional phosphoric acid by a dihydrate method, the content of P is reduced to be below 0.3 percent 2 O 5 The recovery rate of the method is improved to more than 99 percent from 96.0 percent.
The obtained alpha hemihydrate gypsum water-soluble phosphorus has a complete regular hexagonal prism shape, the length-diameter ratio is 1-4, and the performance reaches more than alpha 30 standard.
The low-phosphorus high-strength alpha-type hemihydrate gypsum prepared by the application can be used for producing gypsum blocks, can be used as raw materials of gypsum products such as gypsum-based self-leveling mortar, high-quality plastic filler, cast-in-place wall bodies, gypsum plasterboards with paper surfaces, gypsum boards without paper surfaces, plastering mortar and the like, effectively meets the requirements of the domestic building market on high-quality low-cost gypsum building materials, expands the new application field of phosphogypsum, and has good development prospect.
Example 2
Example 2 differs from example 1 in that: the crystal modifier is a compound of aluminum sulfate and dipotassium succinate, and the mass ratio of the aluminum sulfate to the dipotassium succinate is 24: and 76, the crystal transformation agent is 0.18 percent of the mass of the water phase in the phosphogypsum powder and water phase mixed slurry. The obtained alpha hemihydrate gypsum water-soluble phosphorus has a complete regular hexagonal prism shape, the length-diameter ratio is 1-5, and the performance reaches more than alpha 30 standard.
Example 3
Example 3 differs from example 1 in that: the crystal modifier is a compound of aluminum sulfate and dipotassium succinate, and the mass ratio of the aluminum sulfate to the dipotassium succinate is 40:60, the crystal transformation agent is 0.24 percent of the mass of the water phase in the phosphogypsum powder and water phase mixed slurry. While adding the crystal transformation agent, inputting constant-temperature water with the temperature controlled at 95 ℃ in the constant-temperature heat exchange medium storage tank 45 into a jacket layer of the crystal transformation storage tank 5, and starting electrical heating of the crystal transformation storage tank 5 to maintain the temperature of the liquid material at 95 ℃ to start crystal transformation reaction for 4.0h. The obtained alpha hemihydrate gypsum water-soluble phosphorus has a complete regular hexagonal prism shape, the length-diameter ratio is 1-7, and the performance reaches more than alpha 30 standard.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A preparation method of alpha hemihydrate gypsum is characterized by comprising the following steps: the method comprises the following steps:
crushing phosphate ore into phosphate ore powder for later use;
step two, adding water into concentrated sulfuric acid to dilute the concentrated sulfuric acid to 8-20%, collecting heat generated by diluting the concentrated sulfuric acid through a heat recovery system, adding the crushed phosphorite powder obtained in the step one into the diluted sulfuric acid solution, stirring and reacting for 1-3 hours to obtain slurry;
step three, extraction and separation: adding an extracting agent into the slurry obtained in the second step, wherein the extraction temperature is 50-60 ℃, the extraction time is 20-30 min, and carrying out mixed countercurrent extraction to remove an organic phase to obtain phosphogypsum powder and water phase mixed slurry, wherein the phosphogypsum powder and water phase mixed slurry contains sulfuric acid and phosphoric acid, the sulfuric acid accounts for 8-12% of the mass of the water body, and the phosphoric acid accounts for 12-15% of the mass of the water body; extracting and collecting crude phosphoric acid produced by the reaction of sulfuric acid solution and phosphorite powder in an organic phase, and washing and recovering the entrained phosphoric acid by the organic phase water for later use after heat in the organic phase is collected by a heat recovery system;
step four, sampling and detecting, then adding water, recovered phosphoric acid and dilute sulfuric acid, and controlling the concentration of the sulfuric acid to be 10 +/-0.5%, the concentration of the phosphoric acid to be 14 +/-0.5% and the solid-to-liquid ratio of the phosphogypsum powder to the water to be 40-50%;
step five, adding a crystal transformation agent, stirring uniformly, combining heat collected by a heat recovery system with supplementary heat, heating to 90-110 ℃ to perform crystal transformation reaction for 3-4h to obtain a mixed solution containing alpha semi-hydrated gypsum;
the crystal transformation agent is aluminum sulfate matched with one of citric acid, citrate, succinic acid and succinate;
the mass of the crystal transformation agent is equal to 0.12-0.25% of the mass of the water phase in the phosphogypsum powder and water phase mixed slurry;
step six, carrying out solid-liquid separation on the mixed liquid containing the alpha semi-hydrated gypsum to obtain a solid phase and a liquid phase, and carrying out phosphoric acid and sulfuric acid separation on the liquid phase to obtain phosphoric acid which is recycled as the recovered phosphoric acid in the step four; washing the solid phase with hot water, recycling the washing water, and washing to obtain alpha hemihydrate gypsum;
and the hot water heat source of the solid phase in the washing step six comprises heat recovered by a heat recovery system.
2. The method for preparing alpha hemihydrate gypsum according to claim 1, wherein: the crystal transformation agent is a compound of aluminum sulfate and succinic acid or succinate; the aluminum sulfate accounts for 25-40% of the total mass of the crystal modifier.
3. The method for preparing alpha hemihydrate gypsum according to claim 2, wherein: the crystal transformation agent is a compound of aluminum sulfate and succinate; the succinate is dipotassium succinate; the mass ratio of the aluminum sulfate to the dipotassium succinate is 1: (2-2.5); the length-diameter ratio of the alpha hemihydrate gypsum is 1.
4. The method for preparing alpha hemihydrate gypsum according to claim 3, wherein: the mass ratio of the aluminum sulfate to the dipotassium succinate is 32:68.
5. the method for preparing alpha hemihydrate gypsum according to claim 1, wherein: the extractant is prepared by P204 or naphthenic acid and cyclohexane; the mass of the cyclohexane accounts for 40-60% of the mass of the extracting agent.
6. The method for preparing alpha hemihydrate gypsum according to claim 5, wherein: the extracting agent is prepared from P204 and cyclohexane; the mass ratio of the P204 to the cyclohexane is 2:3.
7. the method for preparing alpha hemihydrate gypsum according to claim 1, wherein: the heat recovery system comprises a normal-temperature heat exchange medium storage tank (1), a concentrated sulfuric acid dilution tank (2), an organic phase washing tank (3), an energy storage tank group (4), a crystal form conversion storage tank (5) and a heat preservation communication pipe network (6), wherein a normal-temperature heat exchange medium in the normal-temperature heat exchange medium storage tank (1) flows to a jacket layer of the concentrated sulfuric acid dilution tank (2) through the heat preservation communication pipe network (6), a normal-temperature heat exchange medium absorbing heat generated by dilution of concentrated sulfuric acid flows to the energy storage tank group (4) through the heat preservation communication pipe network (6), and the heat generated by dilution of the absorbed concentrated sulfuric acid is stored in the energy storage tank group (4); the normal-temperature heat exchange medium in the normal-temperature heat exchange medium storage tank (1) flows to a jacket layer of the organic-phase washing tank (3) through the heat-preservation communicating pipe network (6), the normal-temperature heat exchange medium absorbing heat of the organic-phase liquid material flows to the energy storage tank group (4) through the heat-preservation communicating pipe network (6), and recycling of organic-phase waste heat is completed; and the heat exchange medium output from the energy storage tank group (4) is input into a jacket layer of the crystal transformation storage tank (5) through the heat insulation communication pipe network (6), and the liquid material in the crystal transformation storage tank (5) is heated to 90-110 ℃.
8. The method for preparing alpha hemihydrate gypsum according to claim 7, wherein: the concentrated sulfuric acid dilution tank (2) comprises an inner container tank body (21) and an outer shell tank body (22), and a heat exchange jacket (20) is formed between the inner container tank body (21) and the outer shell tank body (22); the bottom of the heat exchange jacket (20) is communicated with a normal-temperature heat exchange medium storage tank (1), and the top of the heat exchange jacket (20) is communicated with an energy storage tank group (4); the heat insulation filler (220) is integrally formed in the shell tank body (22); the inner container tank body (21) is mainly formed by die casting a metal framework, an acid-resistant resin matrix, glass fiber powder and a heat-conducting filler; the heat conducting filler comprises an acid corrosion resistant ceramic carrier and a heat conducting substance, wherein the heat conducting substance is fixedly connected to the surface of the acid corrosion resistant ceramic carrier through chemical deposition or physical vapor deposition.
9. The method for preparing alpha hemihydrate gypsum according to claim 7, wherein: the acid-resistant resin matrix is at least one of ES-1001N and ES-1002T; the acid corrosion resistant ceramic carrier is microcrystalline mica ceramic powder; the heat conducting substance is at least one of silver, copper, aluminum, tin, bismuth and carbon nano tubes; the glass fiber powder is C glass fiber powder with the granularity controlled between 500 and 2000 meshes; the metal framework is made of aluminum alloy material; the heat-conducting filler accounts for 5-8% of the total mass of the acid-resistant resin matrix.
10. The method for preparing alpha hemihydrate gypsum according to claim 7, wherein: the energy storage tank group (4) comprises a first heat exchange medium storage tank (41) for collecting heat exchange media passing through a jacket layer of the concentrated sulfuric acid dilution tank (2), a second heat exchange medium storage tank (42) for collecting heat exchange media absorbing heat of organic phase liquid materials, a third heat exchange medium storage tank (43), a heat supplementing tank (44) and a constant-temperature heat exchange medium storage tank (45), wherein the first heat exchange medium storage tank (41) is communicated with a heat exchange medium outlet pipe of the jacket layer of the concentrated sulfuric acid dilution tank (2) through a heat-insulating communication pipe network (6); the first heat exchange medium storage tank (41) is communicated with the hot-filling tank (44) through a heat-preservation communication pipe network (6); the second heat exchange medium storage tank (42) is communicated with a heat exchange medium outlet pipe of the jacket layer of the organic phase washing tank (3) through a heat insulation communication pipe network (6); the second heat exchange medium storage tank (42) is communicated with the hot compensation tank (44) through a heat insulation communication pipe network (6); the third heat exchange medium storage tank (43) is communicated with a heat exchange medium outlet pipe of the jacket layer of the crystal conversion storage tank (5) through a heat insulation communication pipe network (6); the third heat exchange medium storage tank (43) is communicated with the hot compensation tank (44) through a heat insulation communication pipe network (6); the heat supplement tank (44) is communicated with a constant-temperature heat exchange medium storage tank (45) through a heat preservation communication pipe network (6); the constant-temperature heat exchange medium storage tank (45) is communicated with a heat exchange medium inlet pipe of the jacket layer of the crystal conversion storage tank (5) through a heat insulation communication pipe network (6).
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