阅读说明：本技术 一种高纯无水氯化铍的制备和提纯装置及方法 (Preparation and purification device and method for high-purity anhydrous beryllium chloride ) 是由 肖伟 熊邮票 于 2021-11-01 设计创作，主要内容包括：本发明涉及一种高纯无水氯化铍的制备和提纯装置及方法,包括：用于对氩气和氯气两股气体的流量进行控制的气路系；用于高温下氯气与氧化铍反应生成氯化铍蒸汽的氯化反应器；以及使生成的氯化铍冷凝并与尾气分离的冷凝器和多级旋风分离器；和用于氯气尾气吸收的多级尾气吸收装置；其中,气路系统通过主进气管路与氯化反应器连通,氯化反应器与冷凝器连接,并通过管路与多级旋风分离器连通；多级旋风分离器和尾气吸收系统通过管路连通。本发明还涉及一种高纯无水氯化铍的制备方法。本发明的制备装置和制备方法可以实现除去原料中硅、铝和铁杂质的功能,可在冷凝器底端接收器中得到高纯无水氯化铍固体。(The invention relates to a device and a method for preparing and purifying high-purity anhydrous beryllium chloride, which comprises the following steps: the gas path system is used for controlling the flow of the argon gas and the chlorine gas; a chlorination reactor for generating beryllium chloride steam by the reaction of chlorine and beryllium oxide at high temperature; a condenser and a multi-stage cyclone separator for condensing the generated beryllium chloride and separating the beryllium chloride from tail gas; and a multistage tail gas absorption device for chlorine tail gas absorption; the gas path system is communicated with a chlorination reactor through a main gas inlet pipeline, and the chlorination reactor is connected with a condenser and is communicated with the multi-stage cyclone separator through a pipeline; the multi-stage cyclone separator is communicated with the tail gas absorption system through a pipeline. The invention also relates to a preparation method of the high-purity anhydrous beryllium chloride. The preparation device and the preparation method can realize the function of removing silicon, aluminum and iron impurities in the raw materials, and can obtain high-purity anhydrous beryllium chloride solid in a receiver at the bottom end of a condenser.)

1. A device and a method for preparing and purifying high-purity anhydrous beryllium chloride comprise a preparation device and a preparation method, and are characterized in that the preparation device comprises a beryllium chloride preparation device and comprises: the device comprises a gas circuit control device (3), a chlorination reactor (6), a collector (11) and a tail gas absorption device (15), wherein the gas circuit control device (3) comprises an argon gas source (1) and a chlorine gas source (2), the gas circuit control device (3) can realize the temperature and flow control of the argon gas source (1) and the chlorine gas source (2), the argon gas source (1) and the chlorine gas source (2) are communicated with a gas inlet main pipe (4), the gas inlet main pipe (4) is communicated with the chlorination reactor (6), the chlorination reactor (6) comprises a tray (8), a pressure gauge and cooling water circulation are arranged at the opening of the chlorination reactor (6), the tray (8) is arranged in a heating furnace (7), the chlorination reactor (6) is communicated with a condenser (9), and an electric scraper (10) is arranged in the condenser (9), the bottom of the condenser (9) is communicated with the collector (11), a two-stage cyclone separator (12) is connected to the outlet of the condenser (9) in series, the bottom of the two-stage cyclone separator (12) is communicated with the hopper (13), the outlet of the two-stage cyclone separator (12) is respectively connected with the vacuum pump (14) and the tail gas absorption device (15), and the outlet of the two-stage cyclone separator (12) is provided with the tail gas return pipe (5) communicated with the air inlet main pipe (4).

2. The apparatus and method for preparing and purifying anhydrous beryllium chloride according to claim 1, wherein the preparation method comprises:

s1, carbon-coated agglomerated beryllium oxide (or a mixture of beryllium oxide and carbon) is flatly laid in a tray (8), the tray (8) is placed on a multilayer grid in a chlorination reactor (6), no more than 6 trays (8) can be placed in the multilayer grid, then the chlorination reactor (6) is covered and sealed, a vacuum pump (14) is started, air in each container and pipeline is exhausted, the vacuum pump (14) is closed, the temperature of the heating furnace (7) is raised to 200 ℃, an argon gas source (1) is started, argon enters the chlorination reactor (6) through an argon gas flow meter in the gas path control device (3) through the gas inlet main pipe (4), and beryllium oxide in the chlorination reactor (6) is carried at high temperature for dehydration; wherein the flow of argon is 10-500 ml/min, and the dehydration time of argon carrying is not less than 12 h;

s2, after dehydration is completed, heating the heating furnace (7) to 800-1100 ℃, then starting a chlorine gas source (2), allowing chlorine gas to enter a chlorination reactor (6) through a gas inlet main pipe (4), to contact with beryllium oxide in the tray (8), and to perform chlorination reaction with the beryllium oxide under the action of carbon, so as to generate beryllium chloride steam at high temperature, wherein the chlorination reaction time is not less than 5 hours;

s3, beryllium chloride steam enters the condenser (9) from the chlorination reactor (6) and cools crystals on the wall of the condenser, the electric scraper (10) is started, the electric scraper (10) scrapes the beryllium chloride crystals on the inner wall of the condenser (9) and falls into a collector (11) at the bottom end of the condenser (9), the beryllium chloride steam which is not effectively cooled or beryllium chloride particles carried by gas are separated from unreacted chlorine gas under the action of the two-stage cyclone separator (12) and collected in a hopper (13) at the bottom of the cyclone separator (12);

s4, unreacted chlorine can be subjected to two-stage absorption treatment by a tail gas absorption device (15), or enters the chlorination reactor (6) again for recycling through the tail gas return pipe (5), a chlorine gas source (2) is closed after the chlorination reaction is finished, an argon gas source (1) is started, residual chlorine in the system is blown into the tail gas absorption device (15), and the chlorine is absorbed by the tail gas absorption device (15) and then is discharged.

3. The apparatus and method for preparing and purifying high-purity anhydrous beryllium chloride as claimed in claims 1-2, wherein for beryllium oxide containing silicon, aluminum and iron, after the step of dehydrating raw materials of S1 is completed, the temperature of the chlorination reactor (6) can be set to be between 200 and 500 ℃, chlorine gas is introduced into the chlorination reactor (6), and the silicon, aluminum and iron react with the chlorine gas to generate corresponding chlorides and sublimate to remove impurities of silicon, aluminum and iron in the beryllium oxide raw materials.

4. The device and the method for preparing and purifying high-purity anhydrous beryllium chloride as claimed in claims 1-2, wherein the chlorine flow is measured by a flowmeter, and the chlorine flow introduced into the chlorination reactor (6) is 10-500 ml/min.

5. The apparatus and method for preparing and purifying anhydrous beryllium chloride according to claims 1-2, wherein the trays (8) in the chlorination reactor (6) are arranged in multiple layers, the layer spacing is not more than 20mm, and the stacking thickness of the preformed beryllium oxide in the trays (8) is not more than 20 mm.

6. The device and the method for preparing and purifying high-purity anhydrous beryllium chloride as claimed in claims 1-2, wherein the blades of the electric scraper (10) are arranged at 180 degrees, and the rotating speed of the electric scraper is 60-5000 r/min.

7. The device and the method for preparing and purifying high-purity anhydrous beryllium chloride as claimed in claims 1-2, wherein the flow of argon for purging residual chlorine gas after chlorination reaction is 50-500 ml/min, and the purging time is not less than 4 h.

8. The device and the method for preparing and purifying high-purity anhydrous beryllium chloride as claimed in claims 1-2, wherein the residual chlorine in the argon carrying pipeline can be absorbed by two or more stages of potassium hydroxide aqueous solution with any concentration.

Technical Field

The invention relates to the technical field of fine chemical engineering of beryllium, in particular to a device and a method for preparing and purifying high-purity anhydrous beryllium chloride.

Background

Beryllium chloride (chemical formula: BeCl)₂) Is the chloride of alkaline earth metal beryllium and is a snow white solid easy to sublime at room temperature. Is a deliquescent crystal or a block. Dissolving in water and part of organic solvent, and making the aqueous solution have strong acidity. It absorbs moisture in air and can be weathered when heated. Beryllium chloride is an important precursor for preparing high-purity metal beryllium by electrolysis, and the metal belongs to rare light metal and has the advantages of low density, high melting point and large elastic modulusThe material has the advantages of high tensile strength, excellent thermal property, good dimensional stability, small neutron absorption cross section, good X-ray transmission property and the like, is an irreplaceable material in the fields of aerospace, aviation, electronics, nuclear industry and the like, and is called as super metal, tip metal and space metal.

The conventional method for preparing beryllium chloride comprises the steps of adding beryllium oxide into a reactor containing a proper amount of distilled water, slowly adding hydrochloric acid with a certain concentration while continuously stirring until the beryllium oxide powder is completely dissolved, evaporating and concentrating a reaction solution, cooling and crystallizing, centrifugally separating, and drying to obtain a finished beryllium chloride product. In addition, CN201610369772.1 discloses a method for preparing beryllium chloride, in which metal beryllium reacts with hydrogen chloride gas in an anhydrous ether system under an inert atmosphere, the hydrogen chloride gas bubbles into an ether solution containing beryllium particles until the beryllium particles in the ether are completely dissolved, the ether is evaporated and removed, and benzene is washed to obtain an anhydrous beryllium chloride solid.

Based on the technical scheme, the invention designs a device and a method for preparing and purifying high-purity anhydrous beryllium chloride, and aims to solve the problems.

Disclosure of Invention

The invention aims to provide a device and a method for preparing and purifying high-purity anhydrous beryllium chloride, so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme:

a device and a method for preparing and purifying high-purity anhydrous beryllium chloride comprise a preparation device and a preparation method, wherein the preparation device comprises a beryllium chloride preparation device and comprises: the gas circuit control device comprises an argon gas source and a chlorine gas source, the gas circuit control device can realize the temperature and flow control of the argon gas source and the chlorine gas source, the argon gas source and the chlorine gas source are communicated with a gas inlet main pipe, the gas inlet main pipe is communicated with the chlorination reactor, the chlorination reactor comprises a tray, a pressure gauge and cooling water circulation are arranged at the opening of the chlorination reactor, the tray is arranged in a heating furnace, the chlorination reactor is communicated with a condenser, an electric scraper is arranged in the condenser, the bottom of the condenser is communicated with the collector, a two-stage cyclone separator is connected in series at the outlet of the condenser, the bottom of the two-stage cyclone separator is communicated with a hopper, and the outlet of the two-stage cyclone separator is respectively connected with a vacuum pump and a tail gas absorption device, and an outlet of the two-stage cyclone separator is provided with a tail gas return pipe communicated with the air inlet main pipe.

As a further aspect of the present invention, the preparation method comprises:

s1, carbon-coated agglomerated beryllium oxide (or a mixture of beryllium oxide and carbon) is flatly laid in a tray, the tray is placed on a multilayer grid in a chlorination reactor, no more than 6 trays can be placed in the multilayer grid, then the chlorination reactor is covered and sealed, a vacuum pump is started, the vacuum pump is turned off after air in each container and pipeline is exhausted, the temperature of the heating furnace is raised to 200 ℃, an argon gas source is started, argon enters the chlorination reactor through an argon gas flowmeter in the gas path control device through the gas inlet main pipe, and the beryllium oxide in the chlorination reactor is subjected to high-temperature carrier belt dehydration; wherein the flow of argon is 10-500 ml/min, and the dehydration time of argon carrying is not less than 12 h.

S2, after dehydration is completed, heating the heating furnace to 800-1100 ℃, then starting a chlorine gas source, enabling chlorine gas to enter a chlorination reactor through a gas inlet main pipe, contacting beryllium oxide in the tray, and performing chlorination reaction with the beryllium oxide under the action of carbon to generate beryllium chloride steam at high temperature, wherein the chlorination reaction time is not less than 5 hours;

s3, beryllium chloride steam enters the condenser from the chlorination reactor, and is cooled and crystallized on the wall of the condenser, the electric scraper is started, the beryllium chloride crystals on the inner wall of the condenser are scraped by the electric scraper and fall into a collector at the bottom end of the condenser, and the beryllium chloride steam which is not effectively cooled or beryllium chloride particles carried by gas are separated from unreacted chlorine gas under the action of the two-stage cyclone separator and are collected in a hopper at the bottom of the cyclone separator;

and S4, carrying out two-stage absorption treatment on unreacted chlorine gas by a tail gas absorption device, or recycling the unreacted chlorine gas by the tail gas return pipe into the chlorination reactor again, closing a chlorine gas source after the chlorination reaction is finished, starting an argon gas source, blowing residual chlorine gas in the system into the tail gas absorption device, and emptying the chlorine gas after the chlorine gas is absorbed by the tail gas absorption device.

As a further scheme of the invention, for beryllium oxide containing silicon, aluminum and iron, after the raw material dehydration step of S1 is completed, the temperature of the chlorination reactor can be set to be between 200 ℃ and 500 ℃, chlorine gas is introduced into the chlorination reactor, and the silicon, aluminum and iron react with the chlorine gas to generate corresponding chlorides and sublimate to remove impurities of the silicon, aluminum and iron in the beryllium oxide raw material.

As a further scheme of the invention, the chlorine flow is measured by a flowmeter, and the chlorine flow introduced into the chlorination reactor is 10-500 ml/min.

As a further scheme of the invention, trays in the chlorination reactor are arranged in a multi-layer mode, the interlayer spacing is not more than 20mm, and the stacking thickness of the prefabricated beryllium oxide in the trays is not more than 20 mm.

As a further scheme of the invention, the blades of the electric scraper are arranged at 180 degrees, and the rotating speed of the electric scraper is 60-5000 revolutions per minute.

As a further scheme of the invention, the flow of argon for purging residual chlorine after chlorination reaction is 50-500 ml/min, and the purging time is not less than 4 h.

As a further scheme of the invention, the chlorine gas remained in the argon carrying pipeline can be absorbed by two or more stages of potassium hydroxide aqueous solution with any concentration.

Compared with the prior art, the invention has the beneficial effects that:

the preparation device and the preparation method can realize the function of removing silicon, aluminum and iron impurities in the raw materials, can obtain high-purity anhydrous beryllium chloride solid in the receiver at the bottom end of the condenser, realize the batch production of the beryllium chloride and greatly reduce the production cost.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.

Fig. 1 is a schematic diagram of an apparatus and a method for preparing and purifying high-purity anhydrous beryllium chloride according to the present invention.

In the drawings, the components represented by the respective reference numerals are listed below:

1. argon source; 2. a chlorine gas source; 3. a gas path control device; 4. a main air inlet pipe; 5. an exhaust gas return pipe; 6. a chlorination reactor; 7. heating furnace; 8. a tray; 9. a condenser; 10. an electric scraper; 11. a collector; 12. a two-stage cyclone separator; 13. a hopper; 14. a vacuum pump; 15. tail gas absorbing device.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In the description of the present invention, it should be noted that the terms "top", "bottom", "one side", "the other side", "front", "back", "middle part", "inside", "top", "bottom", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, as they may be fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

As shown in fig. 1, the present invention provides a device and a method for preparing and purifying high-purity anhydrous beryllium chloride, wherein,

FIG. 1 is a schematic diagram of an apparatus and method for the preparation and purification of highly pure anhydrous beryllium chloride according to the invention;

as can be seen from fig. 1, in practical application, a device and a method for preparing and purifying high-purity anhydrous beryllium chloride comprise a preparation device and a preparation method, wherein the preparation device comprises a beryllium chloride preparation device which comprises: the device comprises a gas path control device 3, a chlorination reactor 6, a collector 11 and a tail gas absorption device 15, wherein the gas path control device 3 comprises an argon gas source 1 and a chlorine gas source 2, the gas path control device 3 can realize the temperature and flow control of the argon gas source 1 and the chlorine gas source 2, the argon gas source 1 and the chlorine gas source 2 are communicated with a gas inlet main pipe 4, the gas inlet main pipe 4 is communicated with the chlorination reactor 6, the chlorination reactor 6 comprises a tray 8, a pressure gauge and cooling water circulation are arranged at the opening of the chlorination reactor 6, the tray 8 is arranged in a heating furnace 7, the chlorination reactor 6 is communicated with a condenser 9, an electric scraper 10 is arranged in the condenser 9, the bottom of the condenser 9 is communicated with the collector 11, a two-stage cyclone separator 12 is connected in series at the outlet of the condenser 9, the bottom of the two-stage cyclone separator 12 is communicated with a hopper 13, the outlet of the two-stage cyclone separator 12 is respectively connected with a vacuum pump 14 and a tail gas absorption device 15, and the outlet of the two-stage cyclone separator 12 is provided with a tail gas return pipe 5 communicated with the gas inlet main pipe 4.

The preparation method comprises the following steps: s1, carbon-coated agglomerated beryllium oxide or a mixture of beryllium oxide and carbon is flatly laid in a tray 8, the tray 8 is placed on a multilayer grid in a chlorination reactor 6, no more than 6 trays 8 can be placed in the multilayer grid, then the chlorination reactor 6 is covered and sealed, a vacuum pump 14 is started, the vacuum pump 14 is closed after air in each container and pipeline is exhausted, the temperature of a heating furnace 7 is raised to 200 ℃, an argon gas source 1 is started, argon enters the chlorination reactor 6 through an argon gas flow meter in a gas path control device 3 through a gas inlet main pipe 4, and the beryllium oxide in the chlorination reactor 6 is carried at a high temperature for dehydration; wherein the flow of argon is 10-500 ml/min, and the dehydration time of argon carrying is not less than 12 h.

S2, after dehydration is completed, heating the heating furnace 7 to 800-1100 ℃, then starting a chlorine gas source 2, enabling chlorine gas to enter the chlorination reactor 6 through the gas inlet main pipe 4, contacting with beryllium oxide in the tray 8, and performing chlorination reaction with the beryllium oxide under the action of carbon to generate beryllium chloride steam at high temperature, wherein the chlorination reaction time is not less than 5 hours;

s3, beryllium chloride steam enters the condenser 9 from the chlorination reactor 6, the beryllium chloride steam cools and crystallizes on the wall of the condenser, the electric scraper 10 is started, the beryllium chloride crystals on the inner wall of the condenser 9 are scraped by the electric scraper 10 and fall into the collector 11 at the bottom end of the condenser 9, the beryllium chloride steam which is not effectively cooled or beryllium chloride particles carried by gas are separated from unreacted chlorine gas under the action of the two-stage cyclone separator 12 and collected in the hopper 13 at the bottom of the cyclone separator 12;

and S4, carrying out two-stage absorption treatment on unreacted chlorine gas by a tail gas absorption device 15, or recycling the unreacted chlorine gas by the tail gas return pipe 5 into the chlorination reactor 6, closing a chlorine gas source 2 after the chlorination reaction is finished, starting an argon gas source 1, blowing residual chlorine gas in the system into the tail gas absorption device 15, and emptying the chlorine gas after being absorbed by the tail gas absorption device 15.

For beryllium oxide containing silicon, aluminum and iron, after the raw material dehydration step of S1 is completed, the temperature of the chlorination reactor 6 can be set to be between 200 ℃ and 500 ℃, chlorine gas is introduced into the chlorination reactor 6, and the silicon, aluminum and iron react with the chlorine gas to generate corresponding chlorides and sublimate to remove impurities of silicon, aluminum and iron in the beryllium oxide raw material.

The chlorine flow is measured by a flowmeter, and the chlorine flow introduced into the chlorination reactor 6 is 10-500 ml/min.

The trays 8 in the chlorination reactor 6 are arranged in a multilayer mode, the interlayer spacing is not more than 20mm, and the stacking thickness of the prefabricated beryllium oxide in the trays 8 is not more than 20 mm.

The blades of the electric scraper 10 are arranged at 180 degrees, and the rotating speed of the electric scraper is 60-5000 revolutions per minute.

And after the chlorination reaction is finished, the flow of the argon for sweeping the residual chlorine is 50-500 ml/min, and the sweeping time is not less than 4 h.

The residual chlorine in the argon carrying pipeline can be absorbed by two or more stages of potassium hydroxide aqueous solution with any concentration.

The preparation device and the preparation method can realize the function of removing silicon, aluminum and iron impurities in the raw materials, can obtain high-purity anhydrous beryllium chloride solid in the receiver at the bottom end of the condenser, realize the batch production of the beryllium chloride and greatly reduce the production cost.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.