CN112062091A - Anhydrous hydrogen fluoride production equipment and production process thereof - Google Patents

Anhydrous hydrogen fluoride production equipment and production process thereof Download PDF

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Publication number
CN112062091A
CN112062091A CN202010987767.3A CN202010987767A CN112062091A CN 112062091 A CN112062091 A CN 112062091A CN 202010987767 A CN202010987767 A CN 202010987767A CN 112062091 A CN112062091 A CN 112062091A
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preheater
tower
heating device
hydrogen fluoride
rotary reaction
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江伟
胡洪峰
谢钺
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Xuancheng Hengtai Electronic Chemical Material Co ltd
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Xuancheng Hengtai Electronic Chemical Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/19Fluorine; Hydrogen fluoride
    • C01B7/191Hydrogen fluoride
    • C01B7/192Preparation from fluorspar

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses anhydrous hydrogen fluoride production equipment, which comprises a crusher, a closed conveyor, a preheater, a rotary reaction furnace, a washing tower, a condensing tower, a rectifying tower and a degassing tower which are sequentially arranged, wherein the preheater comprises a first preheater and a second preheater, the front part of the first preheater is connected with the closed conveyor, the rear part of the first preheater is connected with the rotary reaction furnace, the rear part of the second preheater is connected with the rotary reaction furnace, the first preheater and the second preheater are respectively connected with a first heating device and a second heating device, the rotary reaction furnace is connected with a third heating device, and the first heating device, the second heating device and the third heating device respectively control the temperatures of the first preheater, the second preheater and the rotary reaction furnace; the equipment and the process for producing the anhydrous hydrogen fluoride can effectively solve the problem that the rotary reaction furnace is corroded in the production of the anhydrous hydrogen fluoride in the background technology.

Description

Anhydrous hydrogen fluoride production equipment and production process thereof
Technical Field
The invention belongs to the field of preparation of anhydrous hydrogen fluoride, and particularly relates to anhydrous hydrogen fluoride production equipment and process.
Background
The industrial anhydrous hydrogen fluoride is a chemical product with wide application, has the appearance of more than 99 percent of hydrofluoric acid of colorless fuming liquid, and is easy to gasify under reduced pressure or high temperature. It is mainly used for preparing villiaumite, fluorine-halogen alkane, fluorine refrigerant, corrosion glass, impregnating wood, electrolytic element fluorine, etc.
The anhydrous hydrogen fluoride is widely used in atomic energy, chemical industry, petroleum and other industries, is a strong oxidant, is a basic raw material for preparing elemental fluorine, various fluorine refrigerants, inorganic fluorides and various organic fluorides, can be prepared into various kinds of water-containing hydrofluoric acid, and is used as a catalyst for preparing graphite and organic compounds. Is a raw material for producing a refrigerant Freon, fluorine-containing resin, organic fluoride and fluorine. Can be used as a catalyst for organic diaphragm synthesis of alkylation, polymerization, condensation, isomerization and the like in chemical production. It is also used for corroding stratum during mining of some ore deposit and extracting rare earth elements and radioactive elements. In the atomic energy industry and the production of nuclear weapons, the raw material for manufacturing uranium hexafluoride, the raw material for producing rocket fuel and additives, and the raw material can also be used for glass etching agents, impregnated wood and the like.
Hydrogen fluoride has strong oxidizing, corrosive and acidic properties. The violent reaction with water at room temperature releases a great deal of oxygen, and the strong corrosiveness is mainly reflected in that the chemical corrosion of contacting metal and glass can partially dissolve the metal and the glass. However, in the production of anhydrous hydrogen fluoride, the core equipment is a rotary reactor composed of a large number of metallic structures. The contact of the rotary reaction furnace and the anhydrous hydrogen fluoride aggravates the corrosion degree of the equipment, and greatly reduces the service life of the rotary reaction furnace equipment. The strong corrosivity of anhydrous hydrogen fluoride can directly change the appearance of rotary reaction furnace equipment surface and the performance of anticorrosive coating, and then equipment material nature changes, has not only increased the input of the maintenance manpower of equipment and financial cost, can lead to hydrogen fluoride to leak simultaneously, and direct polluted environment constitutes the threat to producers' life safety. In addition, the corrosion of the anhydrous hydrogen fluoride to equipment can reduce the purity of the hydrogen fluoride, introduce certain impurities and cannot realize the stable and continuous production of the anhydrous hydrogen fluoride.
Disclosure of Invention
The invention aims to provide anhydrous hydrogen fluoride production equipment and a production process thereof, which can effectively solve the problem that a rotary reaction furnace is corroded in the anhydrous hydrogen fluoride production process in the background technology.
The invention relates to anhydrous hydrogen fluoride production equipment, which comprises a crusher, a closed conveyor, a preheater, a rotary reaction furnace, a washing tower, a condensing tower, a rectifying tower and a degassing tower which are sequentially arranged, wherein the preheater comprises a first preheater and a second preheater, the front part of the first preheater is connected with the closed conveyor, the rear part of the first preheater is connected with the rotary reaction furnace, the rear part of the second preheater is connected with the rotary reaction furnace, the first preheater and the second preheater are respectively connected with a first heating device and a second heating device, the rotary reaction furnace is connected with a third heating device, and the first heating device, the second heating device and the third heating device respectively control the temperatures of the first preheater, the second preheater and the rotary reaction furnace.
Preferably, the first preheater and the second preheater both comprise a preheating box, a feed inlet, a discharge outlet, an air inlet and an air outlet are arranged on the preheating box, an air inlet pipe is connected to the air inlet, the air inlet pipe extends to a position close to the bottom in the preheating box, and a stirring device is further arranged in the preheating box;
a feed inlet on a preheating box of the first preheater is connected with the closed conveyor, a feed hopper is connected on a feed inlet on a preheating box of the second preheater, and a discharge outlet on the preheating box of the second preheater is arranged at the upper part of the rotary reaction furnace;
the air outlets of the two preheating tanks are connected with hot air circulating pipes which are respectively communicated with the first heating device and the second heating device.
Preferably, the first heating device, the second heating device and the third heating device respectively comprise a cyclone separator, a bag type dust collector and an air heater which are arranged in sequence.
Preferably, the condensation tower comprises a primary condensation tower, a primary condensation tower and a secondary condensation tower which are connected in sequence.
A production process of anhydrous hydrogen fluoride comprises the following steps:
(1) preparing fluorite powder, a catalyst and concentrated sulfuric acid according to the standard quantity of raw materials for preparing anhydrous hydrogen fluoride, adding the fluorite powder raw materials and the catalyst raw materials into a crusher, crushing the raw materials by the crusher, directly conveying the crushed raw materials into a first preheater through a closed conveyor, adding the concentrated sulfuric acid into a second preheater, and opening stirring devices in two preheating tanks to stir the raw materials;
(2) opening the first heating device and the second heating device, heating the air dedusted by the cyclone separator and the bag type dust collector through an air heater, and introducing the air heated to a set temperature into the first preheater and the second preheater;
(3) starting a third heating device, introducing high-temperature air with a set temperature into the rotary reaction furnace, then simultaneously adding fluorite powder, a catalyst and concentrated sulfuric acid which are preheated to the set temperature into the rotary reaction furnace, and immediately starting the rotary reaction furnace to rotate so that reaction raw materials are fully mixed and completely react;
(4) after the reaction of the rotary reaction furnace, the reaction crude product gas enters a washing tower to be cooled, then sequentially enters a primary condensing tower, a primary condensing tower and a secondary condensing tower to obtain condensate, the condensate passes through a rectifying tower, residual liquid in the rectifying tower returns to the washing tower, the gas at the top of the tower enters a degassing tower to remove SO2 and SiF4, and the liquid remained in the kettle of the degassing tower is the anhydrous hydrogen fluoride product.
Preferably, the preheating temperature in the first preheater and the second preheater is 350-400 ℃, the reaction temperature in the rotary reaction furnace is 300-350 ℃, the cooling time in the washing tower is 50-60 minutes, and the cooling time in the primary condensing tower, the primary condensing tower and the secondary condensing tower is 20 minutes.
The anhydrous hydrogen fluoride production equipment provided by the technical scheme of the invention has the beneficial effects that:
the reaction raw materials are preheated by the preheater, the reaction process for preparing the anhydrous hydrogen fluoride is divided into two steps, the time of the raw materials in the rotary reaction furnace is shortened, and the corrosion time of the rotary reaction furnace is reduced.
The anhydrous hydrogen fluoride production process has the beneficial effects that:
the process is simple, the whole process of chemical reaction is divided into two steps, the corrosion to the rotary reaction furnace in the preparation process of the anhydrous hydrogen fluoride is effectively reduced, the service life of the rotary reaction furnace is prolonged, and the purity and the quality of the anhydrous hydrogen fluoride are improved.
Drawings
Fig. 1 is a connection block diagram of an anhydrous hydrogen fluoride production apparatus according to the technical scheme of the invention.
Detailed Description
In order to facilitate the understanding of the technical solutions of the present invention for those skilled in the art, the technical solutions of the present invention will be further described with reference to the drawings attached to the specification.
Referring to fig. 1, the anhydrous hydrogen fluoride production equipment according to the technical scheme of the invention comprises a crusher, a closed conveyor, a preheater, a rotary reaction furnace made of high-corrosion-resistant materials, a washing tower, a condensing tower, a rectifying tower and a degassing tower which are arranged in sequence. The preheater includes a first preheater for preheating the raw fluorite powder and the catalyst and a second preheater for strong sulfuric acid, respectively. The front part of the first preheater is connected with a closed conveyor for closed conveying of the crushed fluorite powder and the like, and the rear part of the first preheater is connected with a rotary reaction furnace for raw material reaction. The rear part of the second preheater is connected with the rotary reaction furnace, the first preheater and the second preheater are respectively connected with a first heating device and a second heating device, the rotary reaction furnace is connected with a third heating device, and the first heating device, the second heating device and the third heating device respectively automatically control the temperature of the first preheater, the second preheater and the rotary reaction furnace through controllers.
According to the technical scheme, in the specific process, the preheating temperature is higher than the reaction temperature, the whole reaction generated by the anhydrous hydrogen fluoride is divided into two steps, the raw materials are respectively preheated, no chemical reaction exists in the preheating process, and the preheated raw materials are placed in a rotary reaction furnace for a chemical reaction after the preheating is finished, so that the hydrogen fluoride is prepared. Like this with regard to effectual shortening in the rotary reaction stove chemical reaction time and rotary reaction stove inner wall and chemical substance's contact time, and reaction temperature is lower than preheating temperature, compare in prior art, the whole process of preheating and reacting is all accomplished in rotary reaction stove, the effectual rotary reaction stove of having avoided receives erosion and corruption for a long time, the life of extension rotary reaction stove, also avoid in long-time reaction, the corrosion appears in rotary reaction stove, reduce the purity of hydrogen fluoride, introduce certain "impurity", can't realize anhydrous hydrogen fluoride's stable continuous production.
As shown in fig. 1, each of the first and second preheaters includes a preheating tank made of a corrosion-resistant material for holding raw materials. The preheating box is provided with a feeding hole, a discharging hole, an air inlet and an air outlet, the air inlet is connected with an air inlet pipe, the air inlet pipe extends to the position close to the bottom in the preheating box, hot air and raw materials in the preheating box are mixed conveniently, and heating of the raw materials is achieved. Still be provided with agitating unit in the preheating cabinet, agitating unit realizes stirring the raw materials for the raw materials is heated evenly, accelerates preheating speed and efficiency.
As shown in fig. 1, a feed inlet on the preheating box of the first preheater is connected with the closed conveyor, and raw materials such as fluorite powder and catalyst are directly conveyed into the preheating box of the first preheater by the closed conveyor, so that the contact between the fluorite powder and the outside or the dust emission loss of the fluorite powder is reduced. The feed hopper is connected to a feed inlet on the preheating box of the second preheater and made of an anticorrosive material and used for temporarily storing concentrated sulfuric acid so as to be convenient for the concentrated sulfuric acid to heat the inside of the second preheater. The discharge gate setting on the preheating cabinet of second preheater is in rotary reaction furnace upper portion position, and the setting of this structure for only need open the valve can introduce the concentrated sulfuric acid in the second preheater in the rotary reaction furnace, need not adopt the pump body etc. increases the reliability of structure, avoids the pump body and the sealing member in it to appear corroding and influence normal work.
As shown in figure 1, the air outlets of the two preheating tanks are connected with hot air circulating pipes respectively, the two hot air circulating pipes are communicated with the first heating device and the second heating device respectively, and gas which passes through the preheater and heats the raw materials in the preheater is discharged and circulated to the heating devices, so that the hot air is recycled, on one hand, the electric energy is saved, and on the other hand, the influence on the environment temperature caused by the direct discharge of the hot air to the air is avoided.
As shown in fig. 1, the first heating device, the second heating device and the third heating device each include a cyclone separator, a bag filter and an air heater, which are sequentially disposed. The cyclone separator and the bag type dust collector realize the filtration and purification of hot gas entering the preheating box and the rotary reaction furnace.
As shown in fig. 1, the condensing tower includes a primary condensing tower, a primary condensing tower and a secondary condensing tower connected in sequence. And by utilizing multi-stage cooling, on one hand, the cooling efficiency is improved, and simultaneously, the extraction efficiency of the anhydrous hydrogen fluoride is improved.
Referring to fig. 1, a process for producing anhydrous hydrogen fluoride comprises the following steps:
according to the method, fluorite powder, a catalyst and concentrated sulfuric acid are prepared according to the standard quantity of preparing raw materials of anhydrous hydrogen fluoride, then the fluorite powder raw materials and the catalyst raw materials are added into a crusher, the raw materials are crushed by the crusher and then directly conveyed into a first preheater through a closed conveyor, the concentrated sulfuric acid is added into a second preheater, stirring devices in two preheating tanks are opened, the raw materials are stirred, and the raw materials are heated and preheated.
And secondly, opening the first heating device and the second heating device, heating the air subjected to dust removal through the cyclone separator and the bag type dust remover through an air heater, and introducing the air heated to the set temperature into the first preheater and the second preheater. The hot gas exhausted from the first preheater and the second preheater returns to the first heating device and the second heating device through the circulating pipes, so that the hot gas is recycled, the electric energy is saved, and the environment is protected.
And thirdly, starting a third heating device, introducing high-temperature air with a set temperature into the rotary reaction furnace, then simultaneously adding the fluorite powder, the catalyst and the concentrated sulfuric acid which are preheated to the set temperature into the rotary reaction furnace, and immediately starting the rotary reaction furnace to rotate so as to fully mix and completely react the reaction raw materials. Because the raw materials are preheated, a large amount of reactions can be immediately carried out after the raw materials enter the rotary reaction furnace, the reaction time in the rotary reaction furnace and the contact time of the rotary reaction furnace and chemical substances are shortened, the temperature in the rotary reaction furnace is reduced, the corrosion time and degree of the rotary reaction furnace are reduced, and the service life of the rotary reaction kettle is prolonged.
And fourthly, after the reaction of the rotary reaction furnace, cooling the reaction crude product gas in a washing tower, then sequentially entering a primary condensing tower, a primary condensing tower and a secondary condensing tower to obtain condensate, passing the condensate through a rectifying tower, returning residual liquid in the rectifying tower to the washing tower, allowing the tower top gas to enter a degassing tower, removing SO2 and SiF4, and obtaining the product anhydrous hydrogen fluoride as the liquid remained in the kettle of the degassing tower.
Wherein the preheating temperature in the first preheater and the second preheater is 350-400 ℃, the reaction temperature in the rotary reaction furnace is 300-350 ℃, the cooling time in the washing tower is 50-60 minutes, and the condensing time in the primary condensing tower, the primary condensing tower and the secondary condensing tower is 20 minutes.
Technical solution of the invention is described above with reference to the accompanying drawings, it is obvious that the specific implementation of the invention is not limited by the above-mentioned manner, and it is within the scope of the invention to adopt various insubstantial modifications of the inventive method concept and technical solution, or to apply the inventive concept and technical solution to other occasions without modification.

Claims (6)

1. The utility model provides an anhydrous hydrogen fluoride production facility, its characterized in that, is including breaker, closed conveyor, pre-heater, rotary reaction stove, scrubbing tower, condensing tower, rectifying column and the degasser that sets gradually, the pre-heater includes first pre-heater and second pre-heater, the closed conveyor is connected to first pre-heater front portion, and the rotary reaction stove is connected at the rear portion, the rotary reaction stove is connected at second pre-heater rear portion, be connected with first heating device and second heating device on first pre-heater and the second pre-heater respectively, be connected with third heating device on the rotary reaction stove, the temperature of first pre-heater, second pre-heater and rotary reaction stove is controlled respectively to first heating device, second heating device and third heating device.
2. The anhydrous hydrogen fluoride production equipment according to claim 1, wherein each of the first preheater and the second preheater comprises a preheating tank, the preheating tank is provided with a feed inlet, a discharge outlet, an air inlet and an air outlet, the air inlet is connected with an air inlet pipe, the air inlet pipe extends to a position close to the bottom in the preheating tank, and a stirring device is further arranged in the preheating tank;
a feed inlet on a preheating box of the first preheater is connected with the closed conveyor, a feed hopper is connected on a feed inlet on a preheating box of the second preheater, and a discharge outlet on the preheating box of the second preheater is arranged at the upper part of the rotary reaction furnace;
the air outlets of the two preheating tanks are connected with hot air circulating pipes which are respectively communicated with the first heating device and the second heating device.
3. The anhydrous hydrogen fluoride production apparatus according to claim 1, wherein the first heating device, the second heating device and the third heating device each comprise a cyclone, a bag filter and an air heater, which are arranged in this order.
4. The anhydrous hydrogen fluoride production apparatus according to claim 1, wherein the condensation tower comprises a primary condensation tower, a primary condensation tower and a secondary condensation tower connected in this order.
5. A production process of anhydrous hydrogen fluoride is characterized by comprising the following steps:
(1) preparing fluorite powder, a catalyst and concentrated sulfuric acid according to the standard quantity of raw materials for preparing anhydrous hydrogen fluoride, adding the fluorite powder raw materials and the catalyst raw materials into a crusher, crushing the raw materials by the crusher, directly conveying the crushed raw materials into a first preheater through a closed conveyor, adding the concentrated sulfuric acid into a second preheater, and opening stirring devices in two preheating tanks to stir the raw materials;
(2) opening the first heating device and the second heating device, heating the air dedusted by the cyclone separator and the bag type dust collector through an air heater, and introducing the air heated to a set temperature into the first preheater and the second preheater;
(3) starting a third heating device, introducing high-temperature air with a set temperature into the rotary reaction furnace, then simultaneously adding fluorite powder, a catalyst and concentrated sulfuric acid which are preheated to the set temperature into the rotary reaction furnace, and immediately starting the rotary reaction furnace to rotate so that reaction raw materials are fully mixed and completely react;
(4) after the reaction of the rotary reaction furnace, the reaction crude product gas enters a washing tower to be cooled, then sequentially enters a primary condensing tower, a primary condensing tower and a secondary condensing tower to obtain condensate, the condensate passes through a rectifying tower, residual liquid in the rectifying tower returns to the washing tower, the gas at the top of the tower enters a degassing tower to remove SO2 and SiF4, and the liquid remained in the kettle of the degassing tower is the anhydrous hydrogen fluoride product.
6. The process for producing anhydrous hydrogen fluoride according to claim 5, wherein the preheating temperature in the first preheater and the second preheater is 350 ℃ to 400 ℃, the reaction temperature in the rotary reaction furnace is 300 ℃ to 350 ℃, the cooling time in the washing tower is 50 minutes to 60 minutes, and the condensing time in the primary condensing tower, the primary condensing tower and the secondary condensing tower is 20 minutes.
CN202010987767.3A 2020-09-18 2020-09-18 Anhydrous hydrogen fluoride production equipment and production process thereof Pending CN112062091A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113880049A (en) * 2021-11-01 2022-01-04 衢州市鼎盛化工科技有限公司 Method and system for recovering hydrogen fluoride

Citations (7)

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Publication number Priority date Publication date Assignee Title
US3878294A (en) * 1971-01-26 1975-04-15 Bayer Ag Production of hydrogen fluoride
US4010245A (en) * 1974-07-24 1977-03-01 Bayer Aktiengesellschaft Production of hydrogen fluoride and calcium sulfate
JP2004352517A (en) * 2003-05-27 2004-12-16 Daikin Ind Ltd Method and device for manufacturing hydrogen fluoride
CN103896215A (en) * 2012-12-31 2014-07-02 天津市泰亨气体有限公司 Fluorite-sulfuric acid method for preparing hydrogen fluoride
CN106276801A (en) * 2016-08-25 2017-01-04 衢州南高峰化工有限公司 A kind of production equipment and process of anhydrous hydrogen fluoride
CN206276053U (en) * 2016-08-29 2017-06-27 王潇 A kind of electronic-stage hydrofluoric acid production rectifying column
CN109437111A (en) * 2018-12-14 2019-03-08 福建龙氟化工有限公司 A kind of high-pure anhydrous hydrogen fluoride production technique and matched rotary reaction furnace

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3878294A (en) * 1971-01-26 1975-04-15 Bayer Ag Production of hydrogen fluoride
US4010245A (en) * 1974-07-24 1977-03-01 Bayer Aktiengesellschaft Production of hydrogen fluoride and calcium sulfate
JP2004352517A (en) * 2003-05-27 2004-12-16 Daikin Ind Ltd Method and device for manufacturing hydrogen fluoride
CN103896215A (en) * 2012-12-31 2014-07-02 天津市泰亨气体有限公司 Fluorite-sulfuric acid method for preparing hydrogen fluoride
CN106276801A (en) * 2016-08-25 2017-01-04 衢州南高峰化工有限公司 A kind of production equipment and process of anhydrous hydrogen fluoride
CN206276053U (en) * 2016-08-29 2017-06-27 王潇 A kind of electronic-stage hydrofluoric acid production rectifying column
CN109437111A (en) * 2018-12-14 2019-03-08 福建龙氟化工有限公司 A kind of high-pure anhydrous hydrogen fluoride production technique and matched rotary reaction furnace

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113880049A (en) * 2021-11-01 2022-01-04 衢州市鼎盛化工科技有限公司 Method and system for recovering hydrogen fluoride

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Application publication date: 20201211