CN217340094U - Production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride - Google Patents
Production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride Download PDFInfo
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- CN217340094U CN217340094U CN202220362107.0U CN202220362107U CN217340094U CN 217340094 U CN217340094 U CN 217340094U CN 202220362107 U CN202220362107 U CN 202220362107U CN 217340094 U CN217340094 U CN 217340094U
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Abstract
The utility model discloses a preparation anhydrous hydrogen fluoride coproduction hydrofluoric acid and hydrogen fluoride's apparatus for producing, including dividing wall type reaction rectifying column, condensation absorption tower, oxidation reaction cauldron, reboiler and condenser, condensation absorption tower gas phase feed inlet passes through pipeline and valve and hydrogen fluoride rectifying section top gas phase exit linkage, the noncondensable gas export at condenser and condensation section top passes through pipeline and rectifying column top gas phase entry linkage, hydrogen fluoride extraction section bottom heavy component export passes through pipeline and scrubbing tower top heavy component entry linkage, oxidation reaction cauldron bottom sets up the oxidant distributor, its gas, the liquid phase export all is connected with dividing wall type reaction rectifying column middle part feed inlet. The utility model discloses with the production process coupling of anhydrous hydrogen fluoride preparation and electron level hydrofluoric acid and electron level hydrogen fluoride, easy operation can reduce energy consumption and investment effectively, also effectively reduces or has retrieved the accessory substance in the electron level product preparation process simultaneously, and realizes the industrialization more easily.
Description
Technical Field
The utility model is suitable for an anhydrous hydrogen fluoride production facility technical field, concretely relates to preparation anhydrous hydrogen fluoride coproduces apparatus for producing of electron level hydrofluoric acid and electron level hydrogen fluoride.
Background
The anhydrous hydrogen fluoride is widely applied to the aspects of chemical industry, metallurgy, food and the like, such as: fluorine refrigerant, inorganic fluoride salt, petroleum alkane catalysis, metal acid pickling, aluminum fluoride, cryolite and secondary fluoride, fluorine-containing plastics, paint, medicine, pesticide intermediate, fluorine-containing surfactant, uranium hexafluoride, military special products and the like. At present, the focus of the development of fluorine chemical industry in China is mainly to adjust the structure of a product, vigorously develop medium-grade and high-grade products, improve the self-sufficiency rate of the product, focus on improving the proportion of fluorine-containing fine chemicals and accelerate the development of fluorine-containing materials with high added values. In particular, electronic-grade hydrofluoric acid or hydrogen fluoride is one of the most used electronic chemicals in the semiconductor manufacturing process, and can be widely applied to the microelectronic industries such as large-scale integrated circuits, thin film liquid crystal displays, semiconductors, and the like. However, the purity and cleanliness of electronic grade hydrofluoric acid have a significant impact on the yield, electrical performance, and reliability of integrated circuits.
The reactor for producing the anhydrous hydrogen fluoride is a rotary reaction furnace, the traditional technical process comprises the steps of washing, dedusting, cooling and purifying crude hydrogen fluoride gas, then condensing, rectifying and degassing to obtain an anhydrous hydrogen fluoride product, and performing dry treatment on furnace slag; the hydrogen fluoride gas is recovered by adopting sulfuric acid absorption, and the tail gas is treated by adopting water washing, so that the environmental protection emission standard is reached. In the above production process, ionic impurities derived from fluorite and sulfuric acid, such As Si, P, N, S, As, B, alkali metals, and other metal elements, are inevitably taken into anhydrous hydrogen fluoride. Wherein the metal elements can be removed by rectification and water washing, while the low boiling point non-metal impurity elements such as arsenic are difficult to removeIn such a way that it is removed by simple direct rectification. The oxidation method, the sulfide method, the electrolysis method, the adsorption method of polymeric chelating agent and mixed bed anion-cation system, etc. are commonly used, and the oxidation method is divided into a hydrogen peroxide method, an oxidant potassium permanganate method, an oxidant fluorine method and an oxidant PtF 6 Methods, and the like. At present, the main problems in the field of production of electronic grade hydrofluoric acid or hydrogen fluoride are that the utilization rate of raw materials is low, the energy consumption is high, the equipment investment is large, and the economical efficiency and the safety of the whole process are not high in order to remove impurities from anhydrous hydrogen fluoride raw materials.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride, which cancels a tail gas absorption system in the traditional electronic grade hydrofluoric acid or hydrogen fluoride production device, saves equipment investment and fully recovers hydrogen fluoride components in non-condensable gas; the waste acid treatment system in the traditional electronic grade hydrofluoric acid or hydrogen fluoride production device is eliminated, so that the equipment investment is saved, and simultaneously, the hydrogen fluoride component in the waste acid is effectively recovered.
In order to achieve the purpose, the utility model adopts the following technical structure to realize:
a production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride comprises: a dividing wall type reaction rectifying tower, a condensation absorption tower, an oxidation reaction kettle, a reboiler and a condenser; the middle gas phase inlet and the liquid phase feed inlet of the dividing wall type reaction rectifying tower are respectively connected with a gas phase outlet and a liquid phase outlet of the oxidation reaction kettle through pipelines, the heavy component outlet at the bottom of the tower is respectively connected with the heavy component inlet at the top of the washing tower or the liquid phase inlet at the bottom of the reboiler through pipelines, and the non-condensable gas outlet at the top of the tower is connected with the gas phase inlet at the top of the rectifying tower through a pipeline; the interior of the condensation absorption tower is divided into an upper section, a middle section and a lower section, and a filler is filled in the condensation absorption tower, wherein the upper section is above a desalted water inlet, the middle section is between the desalted water inlet and an upper gas-phase inlet, and the lower section is between the two gas-phase inlets; the top and bottom gas phase inlets of the lower section are connected with a gas phase outlet at the top of the hydrogen fluoride rectifying section through a pipeline and a valve, the inlet of water at the top of the middle section is connected with a desalted water pipeline through a pipeline, the gas phase outlet at the top of the lower section is connected with a tube pass inlet of a condenser through a pipeline, a liquid phase outlet at the bottom of the condenser is connected with a liquid phase inlet at the top of the upper section of a condensation absorption tower, a liquid phase inlet at the top of the hydrogen fluoride rectifying section and an electronic-grade anhydrous hydrogen fluoride pipeline through pipelines, and the non-condensable gas outlet at the top of the condenser is connected with a gas phase inlet at the top of the rectifying tower through a pipeline.
Meanwhile, the dividing wall type reaction rectifying tower is provided with a clapboard inside the tower body, and divides the inside into four parts, namely a light component rectifying section, a light component stripping section, a hydrogen fluoride rectifying section and a hydrogen fluoride stripping section, and is internally provided with a filler, wherein: the light component rectifying section is a space enclosed by the lower part of the condensing section, the upper part of the feed inlet in the middle of the tower, the left part of the vertical partition plate, the upper part of the horizontal partition plate and the tower wall, the light component stripping section is a space enclosed by the lower part of the feed inlet in the middle of the tower, the left part of the vertical partition plate, the lower end of the vertical partition plate and the tower wall, the hydrogen fluoride rectifying section is a space enclosed by the lower part of the horizontal partition plate, the right part of the vertical partition plate, the upper part of the lower end of the vertical partition plate and the tower wall, and the hydrogen fluoride stripping section is a space enclosed by the lower part of the vertical partition plate and the tower wall.
Meanwhile, the dividing wall type reaction rectifying tower is provided with a condensing section at the top in the tower, a heat exchange tube is arranged in the condensing section, a tube pass inlet is communicated with the tower body of the dividing wall type reaction rectifying tower, and a tube pass outlet is communicated with the tower top and the non-condensable gas phase outlet at the tower top.
Meanwhile, the bottom of the oxidation reaction kettle and the dividing wall type reaction rectifying tower are respectively provided with a No. 1 oxidant distributor and a No. 2 oxidant distributor, the inlets of the distributors are respectively connected with an oxidant pipeline through pipelines, the interior of the condensation absorption tower is divided into an upper section, a middle section and a lower section, packing is filled in the upper section, the upper section is above the desalted water inlet, the middle section is between the desalted water inlet and the upper gas phase inlet, and the lower section is between the two gas phase inlets.
The utility model discloses following beneficial effect has:
1. the non-condensable gas (light component) at the tops of the dividing wall type reaction rectifying tower and the condenser is converged and sent to the top of the rectifying tower, a tail gas absorption system in the traditional electronic grade hydrofluoric acid or hydrogen fluoride production device is omitted, the equipment investment is saved, and the hydrogen fluoride component in the non-condensable gas is fully recovered;
2. the heavy components at the bottom of the dividing wall type reactive distillation tower and the heavy components at the bottom of the distillation tower are converged and sent to the top of the washing tower, a waste acid treatment system in a traditional electronic-grade hydrofluoric acid or hydrogen fluoride production device is omitted, equipment investment is saved, and hydrogen fluoride components in the waste acid are effectively recovered;
3. the dividing wall type reaction rectifying tower is equivalent to the integration of a traditional oxidation reactor, an electronic grade rectifying tower and an electronic grade distillation degassing tower into one tower, and the internal integration of a plurality of devices can share one reboiler, so that the equipment investment is reduced, and the energy consumption of a regeneration tower is effectively reduced;
4. the vertical condensation section of the dividing wall type reaction rectifying tower is equivalent to that the traditional tower top condenser, a reflux tank and a reflux pump are internally integrated, the reflux tank and the reflux pump are cancelled by means of gravity total reflux, the equipment investment is reduced, and the power consumption of the reflux pump is effectively reduced;
5. by arranging the oxidation reaction kettle and the dividing wall type reaction rectifying tower, the two-stage oxidation reaction is realized, so that the contact and the utilization of the oxidant and the hydrogen fluoride liquid are more sufficient, the safety of the system is improved, and the quality of the product is ensured;
6. the relative output of the electronic-grade hydrofluoric acid and the electronic-grade hydrogen fluoride can be adjusted by adjusting the air input of the two gas phase inlets of the condensation recovery tower, and the response to market demands is more flexible.
Drawings
FIG. 1 is a schematic structural view of a production apparatus for co-producing hydrofluoric acid and hydrogen fluoride by preparing anhydrous hydrogen fluoride.
In the figure, 1, a dividing wall type reaction rectifying tower; 2. a light component rectifying section; 3. a light component stripping section; 4. a hydrogen fluoride rectifying section; 5. a hydrogen fluoride stripping section; 6. a condensing section; 7. a reboiler; 8. A condensing absorption tower; 9. a condenser; 10. a # 1 control valve; 11. a # 2 control valve; 12. a rotary reaction furnace; 13. an acid mixing tank; 14. a washing tower; 15. a first-stage condenser; 16. a secondary condenser; 17. a crude hydrofluoric acid tank; 18. a rectifying tower; 19. a rectifying tower condenser; 20. a rectifying tower reboiler; 21. a degassing tower; 22. a degasser reboiler; 23. a degasser condenser; 24. a sulfuric acid absorption tower; 25. a fluosilicic acid washing tower; 26. an exhaust gas precipitation tower; 27. an oxidation reaction kettle; 28. A No. 1 distributor; 29. a 2# distributor; 30. an electronic grade hydrofluoric acid conduit; 31. an electronic grade anhydrous hydrogen fluoride pipeline; 32. a process tail gas pipeline; 33. a waste water conduit; 34. a fluosilicic acid pipeline; 35. an anhydrous hydrogen fluoride conduit; 36. a gypsum residue pipeline; 37. a fluorite powder pipeline; 38. a fuming sulfuric acid conduit; 39-42, a desalting water pipeline; 43. an oxidant conduit.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings:
referring to fig. 1, a production apparatus for preparing anhydrous hydrogen fluoride and co-producing hydrofluoric acid and hydrogen fluoride mainly includes: a dividing wall type reaction rectifying tower 1, a condensation absorption tower 8, an oxidation reaction kettle 27, a reboiler 7 and a condenser 9. The inside of the tower body of the dividing wall type reaction rectifying tower 1 is provided with a clapboard which divides the inside into four parts, namely a light component rectifying section 2, a light component stripping section 3, a hydrogen fluoride rectifying section 4 and a hydrogen fluoride stripping section 5, and regular packing is filled in the clapboard. In addition, the top of the dividing wall type reaction rectifying tower 1 is provided with a condensing section 6 which is internally provided with a heat exchange tube, the tube pass inlet of the condensing section is communicated with the tower body of the dividing wall type reaction rectifying tower 1, the tube pass outlet is communicated with the tower top and the gas phase outlet of the tower top, and the bottom of the condensing section is provided with a No. 2 oxidizer distributor 29.
The dried fluorite powder is fed from the fluorite powder pipe 37 to the rotary reaction furnace 12. The 98% sulfuric acid is sent to the sulfuric acid absorption tower 24 through a desalted water pipeline 39 to absorb HF in the tail gas, then enters the washing tower 14 to wash dust and heavy components carried by reaction gas, then enters the acid mixing tank 13, and the fuming sulfuric acid is also sent to the acid mixing tank 13 through a fuming sulfuric acid pipeline 38. Mixing in an acid mixing tank 13 to make SO 3 Fully reacts with the water in the 98 percent sulfuric acid to reach the water content of the feed acid close to zero, then enters the rotary reaction furnace 12, the calcium fluoride reacts with the sulfuric acid, and the generated gypsum slag is sent out of the battery limit through a gypsum slag pipeline 36.
The crude hydrogen fluoride gas produced by the reaction is first fed to a scrubber 14 to remove moisture, sulfuric acid and a small amount of dust. The gas from the scrubber tower 14 passes through aA secondary condenser 15 and a secondary condenser 16 for condensing most of HF, and respectively flowing the condensate into a crude hydrofluoric acid tank 17; noncondensable gas is SO 2 、CO 2 、SiF 4 The inert gas and a small amount of non-condensable gas of HF enter the sulfuric acid absorption tower 24. The crude HF condensate firstly enters a rectifying tower 18 from a crude hydrofluoric acid tank 17 and then enters a degassing tower 21, part of anhydrous hydrogen fluoride obtained from the bottom of the degassing tower 21 is sent to an oxidation reaction kettle 29, and part of the anhydrous hydrogen fluoride is sent out of a battery limit zone through an anhydrous hydrogen fluoride pipeline 35; the heavies feed from the bottom of rectifier 18 is returned to the top inlet of scrubber 14. The low boilers discharged from the top of the degasser condenser 23 and the rectifying column condenser 19 are introduced together with a part of the uncondensed HF gas into a sulfuric acid absorption column 24, where most of the HF is absorbed by sulfuric acid. Then, the process tail gas at the top of the sulfuric acid absorption tower 24 enters a gas phase inlet at the bottom of the second-stage fluorosilicic acid absorption tower 25, meanwhile, a desalted water pipeline 40 replenishes desalted water for the fluorosilicic acid washing tower 25, and SiF4 reacts with the desalted water in the fluorosilicic acid absorption tower 25 to generate the fluorosilicic acid. And then, the process tail gas from which SiF4 and HF are removed enters a gas phase inlet at the bottom of the washing tower 26, simultaneously, desalted water is supplemented to the waste gas precipitation tower 26 through a desalted water pipeline 41 for water washing, and the waste gas after water washing reaches the standard and is discharged at high altitude through a process tail gas pipeline 32. The waste water is discharged to the outside through a waste water pipe 33.
The oxidant is connected with the No. 1 distributor 28 and the No. 2 distributor 29 through the oxidant pipeline 43 respectively, and the oxidant is fed to the oxidation reaction kettle 27 and the bottom of the dividing wall type reaction rectifying tower 1 respectively, so that the oxidant and the hydrogen fluoride liquid are in full contact and react, and trivalent arsenic ions in the oxidant are oxidized into volatile arsenic pentafluoride and heavy component arsenic acid or arsenate. Arsenic pentafluoride can be removed through the process of removing light components, and arsenic acid and arsenate can be removed through high-boiling rectification. The material from the oxidation reaction kettle 27 enters the dividing wall type reaction rectifying tower 1 through a pipeline connection. The separation and the refining of the light component and the hydrogen fluoride are realized in the light component rectifying section 2 inside the dividing wall type reaction rectifying tower 1; in the light component stripping section 3, the concentration of light components in the hydrogen fluoride is realized; in the hydrogen fluoride rectifying section 4, separation and refining of hydrogen fluoride are realized; in the hydrogen fluoride stripping section 5, concentration of heavy components in the liquid phase hydrogen fluoride is achieved.
The gas phase at the top of the light component rectifying section 2 enters a condensing section 6, flows from bottom to top, the gas fraction obtained at the top is light component, namely non-condensable gas, and is sent to a gas phase inlet at the top of a rectifying tower 18 through pipeline connection so as to recover HF escaped along with the light component, most of hydrogen fluoride gas with the boiling point higher than that of the light component in a heat exchange tube is condensed into liquid, gravity settling is carried out, and the liquid returns to the top of the light component rectifying section 2 again; the gas phase at the top of the hydrogen fluoride rectifying section 4 is connected with a valve through a pipeline and is delivered to gas phase inlets at the top and the bottom of the lower section of the condensation absorption tower 8, part of hydrogen fluoride is absorbed by desalted water added from the middle of the tower through a desalted water pipeline 42 and is delivered out of a boundary area through an electronic hydrofluoric acid pipeline 30 from the bottom of the condensation absorption tower 8, the gas phase at the top of the tower enters a condenser 9, the condensed liquid is electronic-grade hydrogen fluoride liquid, part of the condensed liquid returns to the top of the condensation absorption tower 8, part of the condensed liquid is delivered out of the boundary area through an electronic-grade hydrogen fluoride liquid pipeline 31, and the rest part of the condensed liquid returns to a top inlet of the hydrogen fluoride rectifying section 4 and is used as reflux liquid; the non-condensable gas outlet at the top of the condenser 9 is connected with the gas phase inlet at the top of the rectifying tower 18 through a pipeline and is used for recovering HF escaping with light components; the heavy component at the bottom of the hydrogen fluoride stripping section 5 is sent to the inlet at the top of the washing tower 14 through pipeline connection for recovering HF discharged along with the heavy component, so as to improve the utilization rate of anhydrous hydrogen fluoride as a raw material. In addition, the air inflow of the two gas phase inlets of the condensation recovery tower 8 can be regulated and controlled by adjusting the opening degrees of the 1# control valve 10 and the 2# control valve 11, so that the aim of adjusting the relative yield of the electronic-grade hydrofluoric acid and the electronic-grade hydrogen fluoride is fulfilled, and the market demand change can be flexibly responded.
The analysis shows that the production device for preparing the anhydrous hydrogen fluoride and coproducing the hydrofluoric acid and the hydrogen fluoride has the characteristics of ingenious design, simple structure, small equipment investment, simple operation, safety, reliability and the like, and can be applied to engineering; and provides a new optimized solution structure for the technical field of anhydrous hydrogen fluoride production equipment.
The above description is for the purpose of describing the invention in more detail with reference to specific preferred embodiments, and it is not to be construed that the embodiments of the present invention are limited thereto, and it will be apparent to those skilled in the art that the present invention can be implemented in a variety of forms without departing from the spirit and scope of the present invention.
Claims (4)
1. The production device for preparing the anhydrous hydrogen fluoride and coproducing the hydrofluoric acid and the hydrogen fluoride is characterized by comprising a dividing wall type reaction rectifying tower (1), a condensation absorption tower (8), an oxidation reaction kettle (27), a reboiler (7) and a condenser (9), wherein a gas phase inlet and a liquid phase feed inlet in the middle of the dividing wall type reaction rectifying tower (1) are respectively connected with a gas phase outlet and a liquid phase outlet of the oxidation reaction kettle (27) through pipelines, a heavy component outlet at the bottom of the tower is respectively connected with a heavy component inlet at the top of a washing tower (14) or a liquid phase inlet at the bottom of the reboiler (7) through pipelines, and a non-condensable gas outlet at the top of the tower is connected with a gas phase inlet at the top of a rectifying tower (18) through a pipeline; the interior of the condensation absorption tower (8) is divided into an upper section, a middle section and a lower section, and is filled with fillers, wherein the upper section is above a desalted water inlet, the middle section is between the desalted water inlet and an upper gas-phase inlet, and the lower section is between the two gas-phase inlets; hypomere top and bottom gaseous phase entry pass through pipeline and valve and dividing wall type reaction rectifying column (1) middle part gaseous phase exit linkage, and the import of middle section top water passes through the pipeline to be connected with desalting water pipe way (42), and the tube side entry linkage of top gaseous phase export pipeline and condenser (9), the liquid phase export of condenser (9) bottom is connected with anhydrous hydrogen fluoride pipeline (31) of electron level through pipeline and condensation absorption tower (8) upper segment top liquid phase entry, dividing wall type reaction rectifying column (1) middle part liquid phase entry respectively, and its top noncondensable gas export passes through pipeline and rectifying column (18) top gaseous phase entry linkage.
2. The production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride as claimed in claim 1, wherein the dividing wall type reactive distillation column (1) is provided with a condensation section (6) at the top in the column, a heat exchange tube is arranged in the condensation section, a tube side inlet is communicated with the body of the dividing wall type reactive distillation column (1), and a tube side outlet is communicated with the top of the column and a non-condensable gas phase outlet at the top of the column.
3. The production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride according to claim 1, wherein the oxidation reaction kettle (27) and the bottom of the dividing wall type reactive distillation tower (1) are respectively provided with a # 1 oxidant distributor (28) and a # 2 oxidant distributor (29), and inlets of the two distributors are respectively connected with the oxidant pipeline (43) through pipelines.
4. The production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride as claimed in claim 1, wherein the dividing wall type reactive distillation column (1) is provided with a left vertical partition wall and a horizontal partition wall inside a column body, and divides the interior into four parts, namely a light component rectifying section (2), a light component stripping section (3), a hydrogen fluoride rectifying section (4) and a hydrogen fluoride stripping section (5), and is filled with a filler, wherein: the light component rectifying section (2) is a space enclosed by a condensing section (6) below, a feed inlet in the middle of the tower, a left vertical partition plate, a horizontal partition wall and a tower wall, the light component stripping section (3) is a space enclosed by a feed inlet in the middle of the tower, a left vertical partition plate, a lower end of the vertical partition plate and a tower wall, the hydrogen fluoride rectifying section (4) is a space enclosed by a horizontal partition wall, a right vertical partition plate, an upper end of the vertical partition plate and a tower wall, and the hydrogen fluoride stripping section (5) is a space enclosed by a lower end of the vertical partition plate and a tower wall.
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| CN202220362107.0U CN217340094U (en) | 2022-02-22 | 2022-02-22 | Production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride |
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| CN202220362107.0U CN217340094U (en) | 2022-02-22 | 2022-02-22 | Production device for preparing anhydrous hydrogen fluoride and coproducing hydrofluoric acid and hydrogen fluoride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115990439A (en) * | 2022-11-28 | 2023-04-21 | 兰州理工大学 | Anhydrous hydrogen fluoride production equipment and process based on expansion fluidized bed |
| CN118598447A (en) * | 2024-08-01 | 2024-09-06 | 浙江沃乐科技有限公司 | Treatment method and system for fluorine-containing sludge |
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2022
- 2022-02-22 CN CN202220362107.0U patent/CN217340094U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115990439A (en) * | 2022-11-28 | 2023-04-21 | 兰州理工大学 | Anhydrous hydrogen fluoride production equipment and process based on expansion fluidized bed |
| CN118598447A (en) * | 2024-08-01 | 2024-09-06 | 浙江沃乐科技有限公司 | Treatment method and system for fluorine-containing sludge |
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