CN105645358A - Method for preparing hydrogen fluoride from fluosilicic acid - Google Patents
Method for preparing hydrogen fluoride from fluosilicic acid Download PDFInfo
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- CN105645358A CN105645358A CN201610145084.7A CN201610145084A CN105645358A CN 105645358 A CN105645358 A CN 105645358A CN 201610145084 A CN201610145084 A CN 201610145084A CN 105645358 A CN105645358 A CN 105645358A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/193—Preparation from silicon tetrafluoride, fluosilicic acid or fluosilicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a method for preparing hydrogen fluoride from fluosilicic acid, comprising the following steps: (1) enabling the fluosilicic acid as a raw material to react with liquid ammonia, thus obtaining an ammonium fluoride solution and a silicon dioxide solid; (2) enabling the ammonium fluoride solution obtained in the step (1) to react with calcium oxide, thus obtaining calcium fluoride and weak aqua ammonia; (3) rectifying to purify the weak aqua ammonia obtained in the step (1), thus obtaining liquid ammonia, and entering the step (1) for recycling; (4) sequentially drying and calcining the calcium fluoride obtained in the step (2), then leading into a fluidization reaction bed with superheated steam, thus obtaining the hydrogen fluoride and calcium oxide, and returning the step (2) to reuse the calcium oxide for recycling, wherein the calcium oxide reacting with the ammonium fluoride solution for the first time in the step (2) is from purchased calcium oxide, and the calcium oxide in the second and subsequent reactions is the calcium oxide in the step (4). The preparation method realizes recycling of the calcium oxide generated in the hydrogen fluoride preparation process, and the purity of the hydrogen fluoride reaches 99.9999% or more.
Description
Technical field
The invention belongs to fluohydric acid gas preparing technical field, be specifically related to one and prepared hydrofluoric method by hexafluosilicic acid.
Background technology
Fluohydric acid gas (HydrogenFluoride), chemical molecular formula is HF, molecular weight 20.01, soluble in water, ethanol. It is colourless transparent liquid under anhydrous hydrogen fluoride (abbreviation AHF) low temperature or pressure, boiling point 19.4 DEG C, fusing point-83.37 DEG C, density 1.008g/cm3(water=1). Under room temperature with room temperature, highly volatile becomes white smoke. Its chemical property is extremely active, can react with alkali, metal, oxide and silicate etc. Fluohydric acid gas is the basis of modern fluoride work, is the most basic raw material producing element fluorine, various fluorine refrigerant, fluorine-containing new material, inorganic fluoriding salt, various organic fluorides etc.
China mainly adopts fluorite and sulfuric acid reaction preparation to produce AHF, although the hydrogen fluoride production technology of China has been in world lead level, but the problem existing for " fluorite sulfuric acid process " production technology, as: energy utilization rate is low, production cost is higher, and dust pollution is serious, still can not be ignored. Advocate the epoch energy-saving and cost-reducing, development low-carbon economy in the whole world, explore new production technology and technique has become the common recognition of insider. Adding fluorite is the non-renewable grand strategy resource that national requirements controls, and in recent years, government is increasingly tighter to the control of fluorite ore yield, and policy is also received tighter and tighter, and the fluorine resource price of fluorite must be more and more higher. So, how to develop the fluorine efficient low-consume from by-product fluosilicic acid, produce fluohydric acid gas technology to environmental protection and increasingly draw attention.
Chinese patent application publication number is that CN103754824A discloses one and utilizes phosphate fertilizer by-product hexafluosilicic acid to prepare hydrofluoric method, mainly comprises the following steps and prepares fluohydric acid gas ammonia solid with hexafluosilicic acid for raw material, then will prepare Fluohydric acid. with strong sulfuric acid response. Although the method protects fluorite and fluorine resource, but needs in its preparation process with concentrated sulphuric acid for raw material, not only severe reaction conditions, and environmental effect is big, and the fluohydric acid gas purity that reaction finally gives is relatively low. Further, what this reaction adopted is that ammonia prepares ammonium fluoride, and such ammonium fluoride solution concentration is too low, it is necessary to concentration, has been increased by thermal energy consumption. In order to make silicon dioxide become white carbon, just at low concentrations, the form making silicon dioxide form white carbon can only be only possible to. Liao Jing China in 2014 and Wang Liqiong have delivered in " ammonium fluoride prepares the research of calcium fluoride optimal conditions " in " environmental science guide " the 33rd phase and have mentioned calcium fluoride mainly for the production of Fluohydric acid., calcium fluoride product is prepared with lime cream and ammonium fluoride solution, the calcium fluoride purity that its reaction produces is only 89.17%, this is because the impurity content of pulverized limestone is high, its calcium fluoride product purity is relatively low.
Summary of the invention
For solving the existing problem that preparation process condition is harsh and product purity is low prepared with hexafluosilicic acid for raw material and exist in fluohydric acid gas, the present invention proposes one and is prepared hydrofluoric method by hexafluosilicic acid, this preparation method achieves to be prepared the calcium oxide produced in fluohydric acid gas process and recycles, and makes the purity of final fluohydric acid gas product reach more than 99.9999%.
The technical scheme is that and be achieved in that:
One is prepared hydrofluoric method by hexafluosilicic acid, comprises the following steps:
1) after reacting with liquefied ammonia for raw material with hexafluosilicic acid, it is easily separated by filter, obtains ammonium fluoride solution and silica solid;
2) by step 1) ammonium fluoride solution that obtains reacts with calcium oxide, then solid-liquid separation, obtains calcium fluoride and weak ammonia;
3) by step 2) weak ammonia that obtains obtains liquefied ammonia by rectification and purification and enters step 1) in be circulated utilization;
4) by step 2) calcium fluoride that obtains sequentially passes through drying and calcining, then passes into the fluidized reaction bed added with superheated steam, obtains fluohydric acid gas and calcium oxide, by calcium oxide reuse to step 2) in be circulated utilization;
Wherein, step 2) in reach the calcium oxide be more than or equal to 90% with the calcium oxide of ammonium fluoride solution first set reaction from outsourcing purity, and second time and with post-reacted calcium oxide from step 4) in calcium oxide.
Further, described step 2) in the reaction temperature of ammonium fluoride solution and calcium oxide be 0��99 DEG C.
Further, described step 1) in hexafluosilicic acid be 55 DEG C��150 DEG C with liquefied ammonia reaction temperature, reaction pH is 8��9.
Further, described step 4) in the temperature dried be 180-200 DEG C, calcining heat is 550-650 DEG C.
Further, described step 4) the temperature of superheated steam be 850-1050 DEG C, the temperature of fluidized reaction bed is 800-950 DEG C.
Further, also include step 4) obtain fluohydric acid gas and carry out being condensed into fluohydric acid gas liquid; Or it is absorbed as liquid HF acid with water.
Further, also include step 4) obtain fluohydric acid gas and first use concentrated sulphuric acid to clean, condensation or absorb with water more afterwards.
Further, fluohydric acid gas condensation material therefor is saline, and condensation temperature is-10��-2 DEG C. Temperature is higher than-2 DEG C, and fluohydric acid gas condensation is incomplete, fluorinated hydrogen in tail gas, causes effective ingredient waste and environmental pollution; Temperature is lower than-10 DEG C, although condensation effect is better, but energy consumption increases.
The present invention provides another kind of and is prepared hydrofluoric method by hexafluosilicic acid, comprises the following steps:
1) after reacting with liquefied ammonia for raw material with hexafluosilicic acid, it is easily separated by filter, obtains ammonium fluoride solution and silica solid;
2) by step 1) ammonium fluoride solution that obtains reacts with calcium hydroxide, then solid-liquid separation, obtains calcium fluoride and weak ammonia;
3) by step 2) weak ammonia that obtains obtains liquefied ammonia by rectification and purification and enters step 1) in be circulated utilization;
4) by step 2) calcium fluoride that obtains sequentially passes through drying and calcining, then passes into the fluidized reaction bed added with superheated steam, obtains fluohydric acid gas and calcium oxide, by calcium oxide reuse to step 2) in be circulated utilization;
Wherein, step 2) in reach the calcium hydroxide be more than or equal to 85% with the calcium hydroxide of ammonium fluoride solution first set reaction from outsourcing purity, and second time and the raw material that later reacts with ammonium fluoride solution are used that from step 4) in calcium oxide.
The present invention reoffers one and is prepared hydrofluoric method by hexafluosilicic acid, comprises the following steps:
1) after reacting with liquefied ammonia for raw material with hexafluosilicic acid, it is easily separated by filter, obtains ammonium fluoride solution and silica solid;
2) by step 1) ammonium fluoride solution that obtains reacts with calcium carbonate, then solid-liquid separation, obtains calcium fluoride and sal volatile;
3) by step 2) calcium fluoride that obtains sequentially passes through drying and calcining, then passes into the fluidized reaction bed added with superheated steam, obtains fluohydric acid gas and calcium oxide, by calcium oxide reuse to step 2) in be circulated utilization;
Wherein, step 2) in reach the calcium carbonate be more than or equal to 99% with the calcium carbonate of ammonium fluoride solution first set reaction from outsourcing purity, and second time and the raw material that later reacts with ammonium fluoride solution are used that from step 4) in calcium oxide.
Beneficial effects of the present invention:
1, the present inventor is surprised to find in R&D process (Chinese patent 201310288043X) and prepares in hydrofluoric process with calcium fluoride for raw material, the calcium oxide purity of its generation can reach 99% and more than; And this by-product-calcium oxide and ammonium fluoride solution are reacted, it is possible not only to obtain purity and reaches 99 and above calcium fluoride, thus preparing purity to reach more than 99.9999% fluohydric acid gas product, and achieves recycling of calcium.
2, the present invention is when carrying out, with liquefied ammonia, the ammonium fluoride solution that ammonification prepares for raw material with hexafluosilicic acid, first set reaction is with purchased from the purity calcium hydroxide be more than or equal to 85% and the purity calcium oxide be more than or equal to 90%, the weak ammonia prepared, liquefied ammonia is obtained by rectification and purification, this liquefied ammonia reacts as raw material and hexafluosilicic acid again, it is achieved that recycling of material.
Detailed description of the invention
Embodiment 1
Raw material: (mass percent) 30% hexafluosilicic acid is 1000kg, liquefied ammonia 122kg, and calcium oxide 350kg, this calcium oxide prepares the calcium oxide obtained in fluohydric acid gas from calcium fluoride.
Hexafluosilicic acid and liquefied ammonia are added reaction in aminating reaction still, and reaction condition controls at 60 DEG C, PH8.5, and question response by filter, isolates silicon dioxide and ammonium fluoride solution completely afterwards. The ammonium fluoride solution separated and calcium oxide being reacted in synthesis reaction vessel, reaction condition controls at 90 DEG C, and question response by solid-liquid separating equipment, isolates weak ammonia and calcium fluoride completely afterwards. The calcium fluoride separated is passed through drying machine drying, dry temperature and control at 180 DEG C, then pass through calcining furnace calcining, calcining furnace temperature controls at 600 DEG C, finally pass into the fluidized reaction bed added with 1000 DEG C of superheated steams, reaction generates fluohydric acid gas and calcium oxide, and fluohydric acid gas passes into-5 DEG C of brine-cooled, obtains fluohydric acid gas 228kg.
Embodiment 2
Raw material: 30% hexafluosilicic acid is 1000kg, liquefied ammonia 122kg, the calcium oxide 350kg added first. This calcium oxide prepares the calcium oxide obtained in fluohydric acid gas from calcium fluoride.
Hexafluosilicic acid and liquefied ammonia are added reaction in aminating reaction still, and reaction condition controls at 120 DEG C, PH8.0, and question response by filter, isolates silicon dioxide and ammonium fluoride solution completely afterwards. The ammonium fluoride solution separated and calcium oxide being reacted in synthesis reaction vessel, reaction condition controls at 80 DEG C, and question response by solid-liquid separating equipment, isolates weak ammonia and calcium fluoride completely afterwards. The calcium fluoride separated is passed through drying machine drying, dry temperature and control at 220 DEG C, then pass through calcining furnace calcining, calcining furnace temperature controls at 650 DEG C, finally pass into the fluidized reaction bed added with 1050 DEG C of superheated steams, reaction generates fluohydric acid gas and calcium oxide, and fluohydric acid gas passes into-5 DEG C of brine-cooled, obtains fluohydric acid gas 246kg.
Embodiment 3
Raw material: 30% hexafluosilicic acid is 1000kg, liquefied ammonia 122kg, the calcium oxide 350kg added first. This calcium oxide prepares the calcium oxide obtained in fluohydric acid gas from calcium fluoride.
Hexafluosilicic acid and liquefied ammonia are added reaction in aminating reaction still, and reaction condition controls at 150 DEG C, PH9.0, and question response by filter, isolates silicon dioxide and ammonium fluoride solution completely afterwards. The ammonium fluoride solution separated and calcium oxide being reacted in synthesis reaction vessel, reaction condition controls at 99 DEG C, and question response by solid-liquid separating equipment, isolates weak ammonia and calcium fluoride completely afterwards. The calcium fluoride separated is passed through drying machine drying, dry temperature and control at 180 DEG C, then pass through calcining furnace calcining, calcining furnace temperature controls at 550 DEG C, finally pass into the fluidized reaction bed added with 850 DEG C of superheated steams, reaction generates fluohydric acid gas and calcium oxide, and fluohydric acid gas passes into-5 DEG C of brine-cooled, obtains fluohydric acid gas 237kg.
Embodiment 4
Raw material: 30% hexafluosilicic acid is 1000kg, liquefied ammonia 122kg, calcium oxide 350kg. This calcium oxide prepares the calcium oxide obtained in fluohydric acid gas from calcium fluoride.
Hexafluosilicic acid and liquefied ammonia are added reaction in aminating reaction still, and reaction condition controls at 55 DEG C, PH8.0, and question response by filter, isolates silicon dioxide and ammonium fluoride solution completely afterwards. The ammonium fluoride solution separated and calcium oxide being reacted in synthesis reaction vessel, reaction condition controls at 10 DEG C, and question response by solid-liquid separating equipment, isolates weak ammonia and calcium fluoride completely afterwards. The calcium fluoride separated is passed through drying machine drying, dry temperature and control at 180 DEG C, then pass through calcining furnace calcining, calcining furnace temperature controls at 550 DEG C, finally pass into the fluidized reaction bed added with 850 DEG C of superheated steams, reaction generates fluohydric acid gas and calcium oxide, and fluohydric acid gas passes into-5 DEG C of brine-cooled, obtains fluohydric acid gas 235kg.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (10)
1. prepared hydrofluoric method by hexafluosilicic acid for one kind, it is characterised in that comprise the following steps:
1) after reacting with liquefied ammonia for raw material with hexafluosilicic acid, it is easily separated by filter, obtains ammonium fluoride solution and silica solid;
2) by step 1) ammonium fluoride solution that obtains reacts with calcium oxide, then solid-liquid separation, obtains calcium fluoride and weak ammonia;
3) by step 2) weak ammonia that obtains obtains liquefied ammonia by rectification and purification and enters step 1) in be circulated utilization;
4) by step 2) calcium fluoride that obtains sequentially passes through drying and calcining, then passes into the fluidized reaction bed added with superheated steam, obtains fluohydric acid gas and calcium oxide, by calcium oxide reuse to step 2) in be circulated utilization;
Wherein, step 2) in reach the calcium oxide be more than or equal to 90% with the calcium oxide of ammonium fluoride solution first set reaction from outsourcing purity, and second time and with post-reacted calcium oxide from step 4) in calcium oxide.
2. according to claim 1 prepared hydrofluoric method by hexafluosilicic acid, it is characterised in that described step 2) in the reaction temperature of ammonium fluoride solution and calcium oxide be 0��99 DEG C.
3. according to claim 1 and 2 prepared hydrofluoric method by hexafluosilicic acid, it is characterised in that described step 1) in hexafluosilicic acid be 55 DEG C��150 DEG C with liquefied ammonia reaction temperature, reaction pH is 8��9.
4. according to claim 1 and 2 prepared hydrofluoric method by hexafluosilicic acid, it is characterised in that described step 4) in the temperature dried be 180��200 DEG C, calcining heat is 550��650 DEG C.
5. according to claim 1 and 2 prepared hydrofluoric method by hexafluosilicic acid, it is characterised in that described step 4) the temperature of superheated steam be 850��1050 DEG C, the temperature of fluidized reaction bed is 800��950 DEG C.
6. according to claim 1 prepared hydrofluoric method by hexafluosilicic acid, it is characterised in that also include step 4) obtain fluohydric acid gas and carry out being condensed into fluohydric acid gas liquid; Or it is absorbed as liquid HF acid with water.
7. according to claim 1 prepared hydrofluoric method by hexafluosilicic acid, it is characterised in that also include step 4) obtain fluohydric acid gas and first use concentrated sulphuric acid to clean, condensation or absorb with water more afterwards.
8. according to claim 6 or 7, prepared hydrofluoric method by hexafluosilicic acid, it is characterised in that fluohydric acid gas condensation material therefor is saline, and condensation temperature is-10��-2 DEG C.
9. prepared hydrofluoric method by hexafluosilicic acid for one kind, it is characterised in that comprise the following steps:
1) after reacting with liquefied ammonia for raw material with hexafluosilicic acid, it is easily separated by filter, obtains ammonium fluoride solution and silica solid;
2) by step 1) ammonium fluoride solution that obtains reacts with calcium hydroxide, then solid-liquid separation, obtains calcium fluoride and weak ammonia;
3) by step 2) weak ammonia that obtains obtains liquefied ammonia by rectification and purification and enters step 1) in be circulated utilization;
4) by step 2) calcium fluoride that obtains sequentially passes through drying and calcining, then passes into the fluidized reaction bed added with superheated steam, obtains fluohydric acid gas and calcium oxide, by calcium oxide reuse to step 2) in be circulated utilization;
Wherein, step 2) in reach the calcium hydroxide be more than or equal to 85% with the calcium hydroxide of ammonium fluoride solution first set reaction from outsourcing purity, and second time and the raw material that later reacts with ammonium fluoride solution are used that from step 4) in calcium oxide.
10. prepared hydrofluoric method by hexafluosilicic acid for one kind, it is characterised in that comprise the following steps:
1) after reacting with liquefied ammonia for raw material with hexafluosilicic acid, it is easily separated by filter, obtains ammonium fluoride solution and silica solid;
2) by step 1) ammonium fluoride solution that obtains reacts with calcium carbonate, then solid-liquid separation, obtains calcium fluoride and sal volatile;
3) by step 2) calcium fluoride that obtains sequentially passes through drying and calcining, then passes into the fluidized reaction bed added with superheated steam, obtains fluohydric acid gas and calcium oxide, by calcium oxide reuse to step 2) in be circulated utilization;
Wherein, step 2) in reach the calcium carbonate be more than or equal to 99% with the calcium carbonate of ammonium fluoride solution first set reaction from outsourcing purity, and second time and the raw material that later reacts with ammonium fluoride solution are used that from step 4) in calcium oxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106315650A (en) * | 2016-08-30 | 2017-01-11 | 淄博志华环保科技有限公司 | Method for preparing calcium fluoride from lime calcination residues |
| CN107055477A (en) * | 2017-04-26 | 2017-08-18 | 衢州市鼎盛化工科技有限公司 | The method and its device of hydrogen fluoride are prepared by fluosilicic acid |
| CN107311109A (en) * | 2017-05-12 | 2017-11-03 | 浙江大学 | A kind of circulating fluidized bed system and method that hydrogen fluoride is produced with Fluorspar Powder |
| CN108083231A (en) * | 2018-01-05 | 2018-05-29 | 九江天赐高新材料有限公司 | A kind of method of fluorine-containing sulfuric acid separation hydrofluoric acid |
| CN112119035A (en) * | 2018-05-08 | 2020-12-22 | “新化学产品”有限责任公司 | Method for treating hexafluorosilicic acid to produce hydrogen fluoride |
| CN112225230A (en) * | 2020-10-15 | 2021-01-15 | 昆明理工大学 | Method for preparing sodium hydrogen fluoride by adopting phosphorus chemical industry by-product fluosilicic acid |
| CN115744827A (en) * | 2022-11-30 | 2023-03-07 | 福建省龙氟新材料有限公司 | Method and device for preparing hydrogen fluoride from fluosilicic acid |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106315650A (en) * | 2016-08-30 | 2017-01-11 | 淄博志华环保科技有限公司 | Method for preparing calcium fluoride from lime calcination residues |
| CN106315650B (en) * | 2016-08-30 | 2018-06-01 | 淄博志华环保科技有限公司 | A kind of method that calcirm-fluoride is prepared using lime calcining residue |
| CN107055477A (en) * | 2017-04-26 | 2017-08-18 | 衢州市鼎盛化工科技有限公司 | The method and its device of hydrogen fluoride are prepared by fluosilicic acid |
| CN107311109A (en) * | 2017-05-12 | 2017-11-03 | 浙江大学 | A kind of circulating fluidized bed system and method that hydrogen fluoride is produced with Fluorspar Powder |
| CN107311109B (en) * | 2017-05-12 | 2019-04-30 | 浙江大学 | A kind of circulating fluidized bed system and method with Fluorspar Powder production hydrogen fluoride |
| CN108083231A (en) * | 2018-01-05 | 2018-05-29 | 九江天赐高新材料有限公司 | A kind of method of fluorine-containing sulfuric acid separation hydrofluoric acid |
| CN112119035A (en) * | 2018-05-08 | 2020-12-22 | “新化学产品”有限责任公司 | Method for treating hexafluorosilicic acid to produce hydrogen fluoride |
| CN112119035B (en) * | 2018-05-08 | 2024-01-16 | “新化学产品”有限责任公司 | Method for treating hexafluorosilicic acid to produce hydrogen fluoride |
| CN112225230A (en) * | 2020-10-15 | 2021-01-15 | 昆明理工大学 | Method for preparing sodium hydrogen fluoride by adopting phosphorus chemical industry by-product fluosilicic acid |
| CN112225230B (en) * | 2020-10-15 | 2021-11-05 | 昆明理工大学 | Method for preparing sodium hydrogen fluoride by adopting phosphorus chemical industry by-product fluosilicic acid |
| CN115744827A (en) * | 2022-11-30 | 2023-03-07 | 福建省龙氟新材料有限公司 | Method and device for preparing hydrogen fluoride from fluosilicic acid |
| WO2024113591A1 (en) * | 2022-11-30 | 2024-06-06 | 福建省龙氟新材料有限公司 | Method and apparatus for preparing hydrogen fluoride from fluorosilicic acid |
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Application publication date: 20160608 |