Electronic grade hydrogen bromide rectifying and purifying method
阅读说明：本技术 电子级溴化氢精馏纯化方法 (Electronic grade hydrogen bromide rectifying and purifying method ) 是由 许少鹏 何经余 于 2020-12-22 设计创作，主要内容包括：本发明涉及一种电子级溴化氢精馏纯化方法,采用精馏纯化设备进行溴化氢精馏纯化,所述精馏纯化设备包括依次连接的原料供应管路、溴化氢精馏系统、溴化氢产品充装装置、PC及安装在PC上的DCS控制系统,精馏纯化设备上各个电器元件均与PC电性连接并由DCS控制系统进行控制,溴化氢精馏系统包括依次连接的一级精馏塔、二级精馏塔,溴化氢产品充装装置包括依次连接的缓冲罐、充装管路,各个精馏塔顶部、底部分别安装有冷凝器、再沸器,钢瓶中的溴化氢原理经原料供应管路先进入一级精馏塔分离重组后,得到的轻组进入二级精馏塔进行轻组分离,得到精馏后的溴化氢,并输出在溴化氢产品充装装置进行充装,本发明结构简单,设计合理,采用精馏法直接将纯度为99.5%的工业溴化氢纯化获得电子级高纯溴化氢。(The invention relates to an electronic grade hydrogen bromide rectification and purification method, which adopts rectification and purification equipment to rectify and purify hydrogen bromide, wherein the rectification and purification equipment comprises a raw material supply pipeline, a hydrogen bromide rectification system, a hydrogen bromide product filling device, a PC (personal computer) and a DCS (distributed control system) arranged on the PC which are connected in sequence, each electrical component on the rectification and purification equipment is electrically connected with the PC and controlled by the DCS control system, the hydrogen bromide rectification system comprises a primary rectification tower and a secondary rectification tower which are connected in sequence, the hydrogen bromide product filling device comprises a buffer tank and a filling pipeline which are connected in sequence, the top and the bottom of each rectification tower are respectively provided with a condenser and a reboiler, the hydrogen bromide principle in a steel cylinder firstly enters the primary rectification tower through the raw material supply pipeline for separation and recombination, then the obtained light group enters the secondary rectification tower for light group separation, so as to obtain the rectified hydrogen bromide, the invention has simple structure and reasonable design, and adopts a rectification method to directly purify the industrial hydrogen bromide with the purity of 99.5 percent to obtain the electronic grade high-purity hydrogen bromide.)
1. The utility model provides an electronic grade hydrogen bromide rectification purification method, adopt rectification purification equipment to carry out the rectification purification of hydrogen bromide, rectification purification equipment is including the raw materials supply pipeline that connects gradually, hydrogen bromide rectification system, the hydrogen bromide product fills dress device, PC and install the DCS control system on PC, each electrical components all controls with PC electric connection and by DCS control system on the rectification purification equipment, hydrogen bromide rectification system is including the one-level rectifying column that connects gradually, second grade rectifying column, the hydrogen bromide product fills the dress device and is including the buffer tank that connects gradually, fill the dress pipeline, condenser, the reboiler are installed respectively to each rectifying column top, the bottom, a serial communication port, the device comprises the following steps:
step 1:
1.1, connecting a steel cylinder filled with raw materials with the input end of a raw material supply pipeline, opening a branch valve of an outlet of the steel cylinder, and replacing air in the raw material supply pipeline with nitrogen;
1.2 setting the control pressure of a regulating valve at the outlet of the raw material supply pipeline to be 2.0 MPa;
1.3 checking whether the pipeline has leakage;
step 2:
2.1 introducing nitrogen into the hydrogen bromide rectifying device, and respectively opening an air inlet valve and an air release valve of the primary rectifying tower and the secondary rectifying tower to blow off the whole rectifying system;
2.2 sampling analysis points of the first-stage and second-stage rectifying towers respectively to analyze the moisture content, stopping blowing off after the moisture is less than 3ppm, closing vent valves and air inlet valves of the first-stage and second-stage rectifying towers, and keeping the system pressure;
and step 3:
3.1 slowly opening the inlet regulating valve of the first-stage rectifying tower to control the flow to 300Nm3/h；
3.2 slowly opening a cold source outlet regulating valve of a condenser at the top of the primary rectifying tower, interlocking the opening of the cold source outlet regulating valve with a temperature sensor at the top of the primary rectifying tower, and controlling the temperature at the top of the tower to be-62 ℃;
3.3 when the liquid level in the tower kettle of the primary rectifying tower reaches 700mm, slowly opening a reboiler heat source outlet regulating valve at the bottom of the primary rectifying tower to ensure that the opening degree of the reboiler heat source outlet regulating valve is interlocked with a pressure sensor at the bottom of the primary rectifying tower, and controlling the pressure at the bottom of the tower to be 1.9 MPa;
3.4 slowly opening the regulating valve at the inlet of the secondary rectifying tower to control the flow to be 285Nm3/h；
3.5 slowly opening a cold source outlet regulating valve of a condenser at the top of the secondary rectifying tower, interlocking the opening of the cold source outlet regulating valve with a temperature sensor at the top of the secondary rectifying tower, and controlling the temperature at the top of the tower to be-61 ℃;
3.6 when the liquid level in the tower kettle of the secondary rectifying tower reaches 700mm, slowly opening a reboiler heat source outlet regulating valve at the bottom of the secondary rectifying tower to enable the opening degree of the reboiler heat source outlet regulating valve to be interlocked with a pressure sensor at the bottom of the secondary rectifying tower, and controlling the pressure at the bottom of the tower to be 1.3 MPa;
3.7 slightly opening a condenser tail gas outlet regulating valve at the top of the secondary rectifying tower to control the flow to be 20Nm3/h；
3.8 sampling and analyzing at the bottom analysis point of the secondary rectifying tower, linking a product outlet regulating valve at the bottom of the secondary rectifying tower with a liquid level sensor in a tower kettle of the secondary rectifying tower when the contents of hydrogen, nitrogen, oxygen, argon, carbon monoxide, carbon dioxide, hydrocarbon and hydrogen chloride reach the product quality standard, controlling the liquid level of the tower kettle to be 700mm, and outputting the liquid in the tower kettle to a hydrogen bromide product filling device;
and 4, step 4:
4.1 after the product from the hydrogen bromide rectification system enters the buffer tank, opening an emptying valve on the buffer tank to carry out replacement treatment on the buffer tank, and removing other impurity gases in the tank;
4.2 sampling and analyzing at an analysis point at the top of the product buffer tank, and storing the product when the content of each impurity in the tank meets the product quality standard;
4.3 when the liquid level of the buffer tank reaches 80%, blowing off the filling pipeline, and discharging the blown off tail gas to a tail gas treatment device;
4.4, placing the steel cylinder which is pumped out and completely replaced on the electronic scale, connecting the steel cylinder with the output end of the filling pipeline through a stainless steel hose, and completely replacing the air in the stainless steel hose with nitrogen;
4.5, replacing the nitrogen in the hose with product gas, then weighing the electronic scale to zero, and setting the allowable filling weight;
4.6 opening the valve on the steel cylinder to charge the product into the steel cylinder;
4.7 when the filling weight of the steel cylinder reaches the allowable filling weight, the electronic scale controls the regulating valve at the output end of the filling pipeline to be closed, and the filling of the group of steel cylinders is stopped.
2. The rectification purification method of electronic grade hydrogen bromide according to claim 1, characterized in that: in step 4, the filling pipeline is provided with a plurality of output ends, each output end is connected with one steel cylinder, a valve on one steel cylinder is opened firstly during filling, when the filling weight of the steel cylinder reaches the allowable filling weight, the electronic scale controls the regulating valve at the output end of the filling pipeline to be closed, filling of the group of steel cylinders is stopped, and meanwhile, the control regulating valve on the other output end is opened to fill the other steel cylinder.
3. The rectification purification method of electronic grade hydrogen bromide according to claim 1, characterized in that: the raw materials supply pipeline includes a delivery main, two at least collecting pipes, the delivery main output connects hydrogen bromide rectification system input, the collecting pipe includes the delivery outlet of a connection delivery main input, a plurality of corresponds the entry that converges of connecting a steel bottle respectively, install the manometer on the output of collecting pipe in proper order, the governing valve, pressure sensor, install the governing valve on the delivery main in proper order, pressure sensor, be provided with the bypass pipe of dress valve on the delivery branch pipe, the bypass pipe both ends are connected the input side of governing valve on the delivery main respectively, the output side, the entry that converges is linked together with the treatment pipeline, the treatment pipeline is through the tube coupling tail gas processing apparatus who takes the valve, through the tube coupling nitrogen gas output device who takes the valve in addition.
4. The rectification purification method of electronic grade hydrogen bromide according to claim 1, characterized in that: the utility model discloses a filling device, including buffer tank, filling pipeline, DCS control system, measuring pump, tail gas processing apparatus, buffer tank top and filling pipeline all through the tube coupling tail gas processing apparatus who has the valve, fill the tube coupling nitrogen gas output device of pipeline through having the valve, install level sensor in the buffer tank, the buffer tank bottom is connected through the pipeline that is equipped with the measuring pump and is filled the pipeline input, level sensor in the buffer tank is chain with the measuring pump, when the liquid level falls to the minimum control liquid level, DCS control system passes the signal to the measuring pump and makes its stop filling.
Technical Field
The invention belongs to the field of production and purification of special industrial gases, and particularly relates to a rectification and purification method of electronic-grade hydrogen bromide.
Background
Electronic grade hydrogen bromide is a very important industrial basic material and is widely applied to industries such as semiconductor Integrated Circuits (IC), Liquid Crystal Displays (LCD), semiconductor light-emitting devices (LED), solar cells (PV) and the like. The development of clean energy and energy-saving technology, which focuses on low-carbon economy, has become the mainstream of development. Under the background, solar cells, semiconductor light-emitting devices and related industries in China are rapidly developed, and the market of electronic grade hydrogen bromide is very wide.
Disclosure of Invention
Aiming at the defects, the invention provides the method for rectifying and purifying the electronic grade hydrogen bromide, and the electronic grade high-purity hydrogen bromide is obtained by directly purifying the industrial hydrogen bromide with the purity of 99.5% by adopting a rectification method.
The invention solves the technical problem by adopting a scheme that an electronic grade hydrogen bromide rectification and purification method adopts rectification and purification equipment to rectify and purify hydrogen bromide, wherein the rectification and purification equipment comprises a raw material supply pipeline, a hydrogen bromide rectification system, a hydrogen bromide product filling device, a PC (personal computer) and a DCS (distributed control system) arranged on the PC which are sequentially connected, all electrical elements on the rectification and purification equipment are electrically connected with the PC and are controlled by the DCS, the hydrogen bromide rectification system comprises a primary rectification tower and a secondary rectification tower which are sequentially connected, the hydrogen bromide product filling device comprises a buffer tank and a filling pipeline which are sequentially connected, and the top and the bottom of each rectification tower are respectively provided with a condenser and a reboiler, and the method comprises the following steps:
step 1:
1.1, connecting a steel cylinder filled with raw materials with the input end of a raw material supply pipeline, opening a branch valve of an outlet of the steel cylinder, and replacing air in the raw material supply pipeline with nitrogen;
1.2 setting the control pressure of a regulating valve at the outlet of the raw material supply pipeline to be 2.0 MPa;
1.3 checking whether the pipeline has leakage;
step 2:
2.1 introducing nitrogen into the hydrogen bromide rectifying device, and respectively opening an air inlet valve and an air release valve of the primary rectifying tower and the secondary rectifying tower to blow off the whole rectifying system;
2.2 sampling analysis points of the first-stage and second-stage rectifying towers respectively to analyze the moisture content, stopping blowing off after the moisture is less than 3ppm, closing vent valves and air inlet valves of the first-stage and second-stage rectifying towers, and keeping the system pressure;
and step 3:
3.1 slowly opening the inlet regulating valve of the first-stage rectifying tower to control the flow to 300Nm3/h；
3.2 slowly opening a cold source outlet regulating valve of a condenser at the top of the primary rectifying tower, interlocking the opening of the cold source outlet regulating valve with a temperature sensor at the top of the primary rectifying tower, and controlling the temperature at the top of the tower to be-62 ℃;
3.3 when the liquid level in the tower kettle of the primary rectifying tower reaches 700mm, slowly opening a reboiler heat source outlet regulating valve at the bottom of the primary rectifying tower to ensure that the opening degree of the reboiler heat source outlet regulating valve is interlocked with a pressure sensor at the bottom of the primary rectifying tower, and controlling the pressure at the bottom of the tower to be 1.9 MPa;
3.4 slowly opening the regulating valve at the inlet of the secondary rectifying tower to control the flow to be 285Nm3/h；
3.5 slowly opening a cold source outlet regulating valve of a condenser at the top of the secondary rectifying tower, interlocking the opening of the cold source outlet regulating valve with a temperature sensor at the top of the secondary rectifying tower, and controlling the temperature at the top of the tower to be-61 ℃;
3.6 when the liquid level in the tower kettle of the secondary rectifying tower reaches 700mm, slowly opening a reboiler heat source outlet regulating valve at the bottom of the secondary rectifying tower to enable the opening degree of the reboiler heat source outlet regulating valve to be interlocked with a pressure sensor at the bottom of the secondary rectifying tower, and controlling the pressure at the bottom of the tower to be 1.3 MPa;
3.7 slightly opening a condenser tail gas outlet regulating valve at the top of the secondary rectifying tower to control the flow to be 20Nm3/h；
3.8 sampling and analyzing at the bottom analysis point of the secondary rectifying tower, linking a product outlet regulating valve at the bottom of the secondary rectifying tower with a liquid level sensor in a tower kettle of the secondary rectifying tower when the contents of hydrogen, nitrogen, oxygen, argon, carbon monoxide, carbon dioxide, hydrocarbon and hydrogen chloride reach the product quality standard, controlling the liquid level of the tower kettle to be 700mm, and outputting the liquid in the tower kettle to a hydrogen bromide product filling device;
and 4, step 4:
4.1 after the product from the hydrogen bromide rectification system enters the buffer tank, opening an emptying valve on the buffer tank to carry out replacement treatment on the buffer tank, and removing other impurity gases in the tank;
4.2 sampling and analyzing at an analysis point at the top of the product buffer tank, and storing the product when the content of each impurity in the tank meets the product quality standard;
4.3 when the liquid level of the buffer tank reaches 80%, blowing off the filling pipeline, and discharging the blown off tail gas to a tail gas treatment device;
4.4, placing the steel cylinder which is pumped out and completely replaced on the electronic scale, connecting the steel cylinder with the output end of the filling pipeline through a stainless steel hose, and completely replacing the air in the stainless steel hose with nitrogen;
4.5, replacing the nitrogen in the hose with product gas, then weighing the electronic scale to zero, and setting the allowable filling weight;
4.6 opening the valve on the steel cylinder to charge the product into the steel cylinder;
4.7 when the filling weight of the steel cylinder reaches the allowable filling weight, the electronic scale controls the regulating valve at the output end of the filling pipeline to be closed, and the filling of the group of steel cylinders is stopped.
Further, in step 4, the filling pipeline is provided with a plurality of output ends, each output end is connected with one steel cylinder, a valve on one of the steel cylinders is opened firstly during filling, when the filling weight of the steel cylinder reaches the allowable filling weight, the electronic scale controls the regulating valve at the output end of the filling pipeline to be closed, filling of the group of steel cylinders is stopped, and meanwhile, the control regulating valve on the other output end is opened to fill the other steel cylinder.
Further, the raw materials supply pipeline includes a transport house steward, two at least collecting pipes, the input of hydrogen bromide rectification system is connected to the transport house steward output, the collecting pipe includes the delivery outlet of a connection transport house steward input, a plurality of corresponds the entry that converges of connecting a steel bottle respectively, install the manometer on the output of collecting pipe in proper order, the governing valve, pressure sensor, install the governing valve on the transport house steward in proper order, pressure sensor, be provided with the bypass pipe that is equipped with the valve on the transport branch pipe, the bypass pipe both ends are connected the input side of governing valve on the transport house steward respectively, the output side, the entry that converges is linked together with the treatment line, the treatment line is through the tube coupling tail gas processing apparatus who takes a valve, through another tube coupling nitrogen output.
Further, the buffer tank top and fill the pipeline and all connect tail gas processing apparatus through the tube coupling that has the valve, fill the pipeline through the tube coupling nitrogen gas output device that has the valve, install level sensor in the buffer tank, the buffer tank bottom is connected through the delivery line who is equipped with the measuring pump and is filled the pipeline input, level sensor in the buffer tank is chain with the measuring pump, when the liquid level dropped to the minimum control liquid level, DCS control system passed the signal to the measuring pump and makes it stop filling.
Compared with the prior art, the invention has the following beneficial effects: simple structure, reasonable design, and directly purifying industrial hydrogen bromide with the purity of 99.5 percent by adopting a rectification method to obtain the electronic grade high-purity hydrogen bromide.
Drawings
The invention is further described with reference to the following figures.
FIG. 1 is a schematic view of the construction of a material supply system;
FIG. 2 is a schematic diagram of the structure of a hydrogen bromide rectification system;
figure 3 is a schematic diagram of the configuration of the hydrogen bromide product filling system.
In the figure: 1-a steel cylinder for charging raw materials; 2-electronic scale; 3-a raw material supply line; 301-a collector tube; 302-a delivery manifold; 4-a first-stage rectifying tower; 5-a secondary rectifying tower; 6-a reboiler; 7-a condenser; 8-a buffer tank; 9-a metering pump; 10-a steel cylinder for holding the product; 11-a filling line; PT-pressure sensor; PY-regulating valve; PG-pressure gauge; an FT-flow meter; LT-level sensor; WY-charge regulating valve; WC-weight sensor; TY-condenser cold source outlet regulating valve; a TE-temperature sensor; PY-reboiler heat source outlet regulating valve; an inlet regulating valve of the FY-secondary rectifying tower; AE-analysis point; LY-outlet regulating valve.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
As shown in fig. 1-3, a method for rectifying and purifying electronic grade hydrogen bromide, which adopts a rectifying and purifying device to rectify and purify hydrogen bromide, wherein the rectifying and purifying device comprises a raw material supply pipeline 3, a hydrogen bromide rectifying system, a hydrogen bromide product filling device, a PC and a DCS control system installed on the PC, which are connected in sequence, each electrical component on the rectifying and purifying device is electrically connected with the PC and controlled by the DCS control system, the hydrogen bromide rectifying system comprises a primary rectifying tower 4 and a secondary rectifying tower 5, which are connected in sequence, the hydrogen bromide product filling device comprises a buffer tank 8 and a filling pipeline 11, which are connected in sequence, a condenser 7 and a reboiler 6 are respectively installed at the top and the bottom of each rectifying tower, and the method comprises the following steps:
step 1:
1.1, connecting a steel cylinder 1 filled with raw materials with the input end of a raw material supply pipeline, opening a branch valve of an outlet of the steel cylinder, and replacing air in the raw material supply pipeline with nitrogen;
1.2 setting the control pressure of a regulating valve at the outlet of the raw material supply pipeline to be 2.0 MPa;
1.3 checking whether the pipeline has leakage;
step 2:
2.1 introducing nitrogen into the hydrogen bromide rectifying device, and respectively opening an air inlet valve and an air release valve of the primary rectifying tower and the secondary rectifying tower to blow off the whole rectifying system;
2.2 sampling analysis points of the first-stage and second-stage rectifying towers respectively to analyze the moisture content, stopping blowing off after the moisture is less than 3ppm, closing vent valves and air inlet valves of the first-stage and second-stage rectifying towers, and keeping the system pressure;
and step 3:
3.1 slowly opening the inlet regulating valve of the first-stage rectifying tower to control the flow to 300Nm3/h；
3.2 slowly opening a cold source outlet regulating valve of a condenser at the top of the primary rectifying tower, interlocking the opening of the cold source outlet regulating valve with a temperature sensor at the top of the primary rectifying tower, and controlling the temperature at the top of the tower to be-62 ℃;
3.3 when the liquid level in the tower kettle of the primary rectifying tower reaches 700mm, slowly opening a reboiler heat source outlet regulating valve at the bottom of the primary rectifying tower to ensure that the opening degree of the reboiler heat source outlet regulating valve is interlocked with a pressure sensor at the bottom of the primary rectifying tower, and controlling the pressure at the bottom of the tower to be 1.9 MPa;
3.4 slowly opening the regulating valve at the inlet of the secondary rectifying tower to control the flow to be 285Nm3/h；
3.5 slowly opening a cold source outlet regulating valve of a condenser at the top of the secondary rectifying tower, interlocking the opening of the cold source outlet regulating valve with a temperature sensor at the top of the secondary rectifying tower, and controlling the temperature at the top of the tower to be-61 ℃;
3.6 when the liquid level in the tower kettle of the secondary rectifying tower reaches 700mm, slowly opening a reboiler heat source outlet regulating valve at the bottom of the secondary rectifying tower to enable the opening degree of the reboiler heat source outlet regulating valve to be interlocked with a pressure sensor at the bottom of the secondary rectifying tower, and controlling the pressure at the bottom of the tower to be 1.3 MPa;
3.7 slightly opening a condenser tail gas outlet regulating valve at the top of the secondary rectifying tower to control the flow to be 20Nm3/h；
3.8 sampling and analyzing at the bottom analysis point of the secondary rectifying tower, linking a product outlet regulating valve at the bottom of the secondary rectifying tower with a liquid level sensor in a tower kettle of the secondary rectifying tower when the contents of hydrogen, nitrogen, oxygen, argon, carbon monoxide, carbon dioxide, hydrocarbon and hydrogen chloride reach the product quality standard, controlling the liquid level of the tower kettle to be 700mm, and outputting the liquid in the tower kettle to a hydrogen bromide product filling device;
and 4, step 4:
4.1 after the product from the hydrogen bromide rectification system enters the buffer tank, opening an emptying valve on the buffer tank to carry out replacement treatment on the buffer tank, and removing other impurity gases in the tank;
4.2 sampling and analyzing at an analysis point at the top of the product buffer tank, and storing the product when the content of each impurity in the tank meets the product quality standard;
4.3 when the liquid level of the buffer tank reaches 80%, blowing off the filling pipeline, and discharging the blown off tail gas to a tail gas treatment device;
4.4, placing the steel bottle 10 which is pumped out and completely replaced on the electronic scale 2, connecting the steel bottle with the output end of the filling pipeline through a stainless steel hose, and completely replacing the air in the stainless steel hose with nitrogen;
4.5, replacing the nitrogen in the hose with product gas, then weighing the electronic scale to zero, and setting the allowable filling weight;
4.6 opening the valve on the steel cylinder to charge the product into the steel cylinder;
4.7 when the filling weight of the steel cylinder reaches the allowable filling weight, the electronic scale controls the regulating valve at the output end of the filling pipeline to be closed, and the filling of the group of steel cylinders is stopped.
In this embodiment, in step 4, the charging pipeline is provided with a plurality of output ends, each output end is connected to one steel cylinder, a valve on one of the steel cylinders is opened during charging, when the charging weight of the steel cylinder reaches the allowable charging weight, the electronic scale controls the regulating valve at the output end of the charging pipeline to close, the charging of the group of steel cylinders is stopped, and simultaneously, the control regulating valve at the other output end is opened to charge the other steel cylinder.
In this embodiment, the raw materials supply pipeline includes a delivery main 302, two at least collecting pipes 301, the input of hydrogen bromide rectification system is connected to the delivery main output, the collecting pipe includes the delivery outlet of a connection delivery main input, a plurality of corresponds the entry that converges of connecting a steel bottle respectively, install the manometer on the output of collecting pipe in proper order, the governing valve, pressure sensor, install the governing valve on the delivery main in proper order, pressure sensor, be provided with the bypass pipe that is equipped with the valve on the delivery branch pipe, the input side of governing valve on the delivery main is connected respectively at the bypass pipe both ends, the output side, the entry that converges is linked together with the treatment pipeline, the treatment pipeline is through the tube coupling tail gas processing apparatus who takes the valve, through another tube coupling nitrogen output device who takes the valve.
In this embodiment, buffer tank top and filling pipeline all through the tube coupling tail gas processing apparatus who has the valve, fill the tube coupling nitrogen gas output device of pipeline through having the valve, install level sensor in the buffer tank, buffer tank bottom is connected through the delivery line who is equipped with measuring pump 9 and is filled the pipeline input, level sensor in the buffer tank is chain with the measuring pump, when the liquid level dropped to the minimum control liquid level, DCS control system passed the signal for the measuring pump and makes its stop filling.
In this embodiment, the cooling capacity required by the condenser is provided by the cooling source unit, and the cooling medium is returned to the cooling source unit for circulation after heat exchange by the condenser. The heat required by the reboiler is provided by the heat source unit, and the heat medium is returned to the heat source unit for circulation after heat exchange by the reboiler.
In this embodiment, a Zhejiang central control DCS control system is adopted, a redundant control station, an operator station and an engineer station are configured, and human-computer interface design and configuration are performed according to a purification process.
In this example, the raw material supply general industrial hydrogen bromide is packed in 44L gas bottles as the raw material for the electronic grade hydrogen bromide rectifying and purifying device. The industrial hydrogen bromide 44-liter gas cylinder is connected with a raw material supply pipeline through a stainless steel hose, the gas cylinders are divided into two groups, and when the hydrogen bromide in one group of 44-liter gas cylinders is used up, the other group of 44-liter gas cylinders is automatically switched to be used. The hydrogen bromide belongs to a D low-pressure liquefied gas, the saturated vapor pressure at 60 ℃ is 4.86MPa, pressure control is adopted for automatic switching, when the pressure of a group of gas cylinders is reduced to 2.0MPa, the pressure of raw materials can not meet the requirement of a rectification system, and the raw materials are switched by a DCS control system.
In this embodiment, to ensure that the hydrogen bromide source material is not contaminated by air in the tube, the tube outlet must be purged with nitrogen before opening the hydrogen bromide cylinder valve. Because of the hydrogen bromide is toxic gas, when the steel bottle is dismantled for connection, the hydrogen bromide in the pipeline is replaced cleanly with nitrogen gas, and the hydrogen bromide in the pipeline is discharged to a tail gas treatment device.
In this example, the hydrogen bromide raw material has a purity of about 99.5%, and contains impurities such as hydrogen, nitrogen, oxygen + argon, carbon monoxide, carbon dioxide, hydrocarbons, hydrogen chloride, and water, wherein the boiling point of hydrogen, nitrogen, oxygen + argon, carbon monoxide, carbon dioxide, hydrocarbons, and hydrogen chloride is lower than the boiling point of hydrogen bromide by-66.8 ℃, which is a light component, and the boiling point of water is higher than the boiling point of hydrogen bromide, which is a heavy component. According to the rectification principle of the rectification tower, the components are separated according to different boiling points, so that the process is provided with two stages of rectification towers, wherein the first stage of rectification tower is a heavy component removal tower, and the second stage of rectification tower is a light component removal tower, and the heavy component and the light component are respectively separated. Hydrogen bromide raw material enters a primary rectifying tower through a flowmeter, rising steam is provided by a bottom reboiler, reflux liquid is provided by a top condenser, the rising steam and the reflux liquid are subjected to heat and mass transfer exchange at a packing layer of the rectifying tower, heavy components are separated from light components, the heavy components are gathered at the bottom of the rectifying tower, and the heavy components are discharged out of the primary rectifying tower to a waste liquid treatment device. And the light components enter the condenser from the top of the tower, one part of hydrogen bromide is condensed as reflux liquid and returns to the rectifying tower to participate in rectification, and the other part of uncondensed hydrogen bromide and the light components are used as raw materials of the secondary rectifying tower and enter the secondary rectifying tower. The second-stage rectifying tower is mainly used for separating hydrogen bromide from light components (hydrogen, nitrogen, oxygen + argon, carbon monoxide, carbon dioxide, hydrocarbon and hydrogen chloride), the hydrogen bromide and the light components are subjected to heat and mass transfer exchange in a packing layer of the rectifying tower, so that the hydrogen bromide is separated from the light components, most of the hydrogen bromide and a small amount of the light components are discharged from the top of the tower and enter a condenser, most of the hydrogen bromide is condensed to be used as reflux liquid and returns to the rectifying tower to participate in rectification, and a small amount of uncondensed hydrogen bromide and light components are discharged from a tail gas treatment device of the second-stage rectifying tower through a pipeline. The heavy component hydrogen bromide is gathered at the bottom of the rectifying tower and is sent to a hydrogen bromide product filling system through a pipeline.
In this example, the nitrogen gas needs to be depressurized to 0.6MPa before it can be fed into the pipeline of the rectification purification apparatus.
The design adopts a rectification method to directly purify industrial hydrogen bromide with the purity of 99.5 percent to obtain electronic-grade high-purity hydrogen bromide, the purity is 99.999 percent (5N), and the total impurity content is lower than 10 ppm.
The technical parameters of the raw material hydrogen bromide adopted in the design are as follows:
the quality of the hydrogen bromide product produced in the design is as follows:
the product yield index in the design is as follows:
hydrogen bromide HBr
Minimum size
Is normal
Maximum of
Yield (kg/h)
160
265
320
If this patent discloses or refers to parts or structures that are fixedly connected to each other, the fixedly connected may be understood as: a detachable fixed connection (for example using bolts or screws) is also understood as: non-detachable fixed connections (e.g. riveting, welding), but of course, fixed connections to each other may also be replaced by one-piece structures (e.g. manufactured integrally using a casting process) (unless it is obviously impossible to use an integral forming process).
In the description of this patent, it is to be understood that the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the patent, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the patent.
The above-mentioned preferred embodiments, further illustrating the objects, technical solutions and advantages of the present invention, should be understood that the above-mentioned are only preferred embodiments of the present invention and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.