CN110065951B - Device and method for producing high-purity boron trichloride - Google Patents
Device and method for producing high-purity boron trichloride Download PDFInfo
- Publication number
- CN110065951B CN110065951B CN201910221456.3A CN201910221456A CN110065951B CN 110065951 B CN110065951 B CN 110065951B CN 201910221456 A CN201910221456 A CN 201910221456A CN 110065951 B CN110065951 B CN 110065951B
- Authority
- CN
- China
- Prior art keywords
- liquid
- rectifying tower
- outlet
- raw material
- heat exchanger
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/061—Halides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention belongs to a device for producing high-purity boron trichloride and a production method thereof; the device comprises a raw material liquid buffer tank, a product tank, a liquid ammonia storage tank and a circulating water return tank, wherein the raw material liquid buffer tank is connected with a first raw material liquid inlet at the upper middle part of a first rectifying tower through a raw material liquid pump, a liquid phase outlet at the bottom of the first rectifying tower is connected with a first raw material liquid inlet of a second rectifying tower, and a top gas phase outlet of the second rectifying tower is connected with the product tank sequentially through a first tube side inlet of a second heat exchanger, a first tube side outlet of the second heat exchanger, a first tee joint and a product pump; the method has the characteristics of high automation degree, stable operation and high purity of 99.9995 percent; provides guarantee for the research of special gas in the electronic industry and the development of the semiconductor field, and has good economic and social benefits.
Description
Technical Field
The invention belongs to the technical field of high-purity boron trichloride production, and particularly relates to a device and a method for producing high-purity boron trichloride, wherein the purity of the device is not lower than 99.9995%.
Background
Boron trichloride is mainly used as doping gas, crystal growth gas, plasma etching gas, ion beam etching gas, ion implantation gas, etc. in the semiconductor field. In other fields, the catalyst can be used as an oxygen scavenger, a nitride and a carbide additive in refining of an alloy by borating steel with a catalyst for organic synthesis, a flux for decomposition of silicate and the like.
The purification production process for industrially producing boron trichloride at present comprises the following steps:
(1) Borax is used as a raw material, borax Na2B4O7.H2O and residual oil are mixed in a rotary furnace, heated to 1038 ℃, then reacted with introduced chlorine in a special reactor, the reaction temperature is controlled to 760 ℃, and the content of carbonyl dichloride impurities in boron trichloride obtained by the reaction is higher, so that the method is not recommended to produce high-purity boron trichloride because of extremely strong toxicity of the carbonyl dichloride.
(2) Mixing borax and carbon, heating to 600-700 deg.C, introducing chlorine gas and making them react to obtain boron trichloride, and the boron trichloride produced by said method also contains carbonyl dichloride, and has the need of removing them by means of thermal decomposition and discharge decomposition, etc. and its technological process is complex.
(3) Under the heating condition, boron trifluoride and aluminum trichloride are adopted to react, and carbon dioxide or alcohol is adopted as a cold source for low-temperature rectification in the reaction to prepare high-purity boron trichloride. However, boron trifluoride in the raw materials is expensive and has high cost.
(4) The simple substance boron and chlorine are directly synthesized into boron trichloride at high temperature: the boron trichloride generated by the method is cooled by a receiver and then by dry ice to prepare the industrial grade boron trichloride product.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a device and a production method for producing high-purity boron trichloride, wherein hot water is used as a heat source, the cold source is automatically controlled, the balance of the system is maintained, the rectification mode is high in automation degree, simple and convenient to operate, stable in operation and low in cost, the heat source is clean and environment-friendly, and the purity of a boron trichloride product can be prepared to be not lower than 99.9995%.
The object of the invention is achieved in that: the liquid phase rectifying device comprises a raw material liquid buffer tank, a product tank, a liquid ammonia storage tank and a circulating water return tank, wherein the raw material liquid buffer tank is connected with a first raw material liquid inlet at the upper part in a first rectifying tower through a raw material liquid pump, a liquid phase outlet at the bottom of the first rectifying tower is connected with a first raw material liquid inlet of a second rectifying tower, and a top gas phase outlet of the second rectifying tower is sequentially connected with the product tank through a first tube side inlet of a second heat exchanger, a first tube side outlet of the second heat exchanger, a first tee joint and a product pump.
Preferably, the gas phase outlet at the top of the first rectifying tower is connected with the inlet of the first gas-liquid separator through the first tube side inlet of the first heat exchanger and the first tube side outlet of the first heat exchanger, the liquid phase outlet of the first gas-liquid separator is connected with the second raw material liquid inlet at the upper middle part of the first rectifying tower, and the gas phase outlet of the first gas-liquid separator is connected with the adsorption tower through the fifth regulating valve and the second tee joint.
Preferably, the liquid phase outlet at the bottom of the second rectifying tower is connected with the adsorption tower through a sixth regulating valve and a third end of the second tee joint.
Preferably, the third end of the first tee is connected with the second raw material liquid inlet of the second rectifying tower.
Preferably, the liquid ammonia outlet of the liquid ammonia storage tank is respectively connected with the second tube side inlet of the first heat exchanger and the second tube side inlet of the second heat exchanger through a third tee joint, the second tube side outlet of the first heat exchanger and the second tube side outlet of the second heat exchanger are respectively connected with a fourth tee joint, and the third end of the fourth tee joint is connected with an air conditioner ice machine; a ninth regulating valve is arranged between the third tee joint and the second tube side inlet of the first heat exchanger, a tenth regulating valve is arranged between the third tee joint and the second tube side inlet of the second heat exchanger, and an eleventh regulating valve is arranged between the third end of the fourth tee joint and the air conditioner ice machine.
Preferably, the water outlet of the circulating water return tank is respectively connected with a first reboiler at the bottom of the first rectifying tower and a second reboiler at the bottom of the second rectifying tower through a fifth tee joint, and the outlets of the first reboiler and the second reboiler are respectively connected with the circulating water supply tank through a sixth tee joint; a seventh regulating valve is arranged between the fifth tee joint and the first reboiler, and an eighth regulating valve is arranged between the fifth tee joint and the second reboiler.
Preferably, a first regulating valve is arranged between the raw material liquid buffer tank and the raw material liquid pump, a second regulating valve is arranged between a liquid phase outlet at the bottom of the first rectifying tower and a first raw material liquid inlet of the second rectifying tower, a third regulating valve is arranged between the first tee joint and the product pump, and a fourth regulating valve is arranged between the product pump and the product tank.
A method for producing a device for producing high-purity boron trichloride, the method comprising the steps of:
step 1: the raw material liquid in the raw material liquid buffer tank sequentially passes through a first regulating valve, a raw material liquid pump and the first rectifying tower at the middle upper partA raw material liquid inlet enters the first rectifying tower; the main composition of the raw material liquid is as follows: boron trichloride, silicon tetrachloride, hydrogen chloride, chlorine, carbon monoxide, oxygen, carbon dioxide, nitrogen, methane, argon and moisture; temperature of raw material liquid: 35-40 ℃, pressure: 0.2Mpa, flow: 5-7 Nm 3 Gas phase fraction/h: 0, BCL 3 Mole fraction: 98% -99.5%;
step 2: the raw material liquid entering the first rectifying tower in the step 1 is subjected to primary rectification purification, and liquid phase after primary rectification purification enters the second rectifying tower through a liquid phase outlet at the bottom of the first rectifying tower, a second regulating valve and a first raw material liquid inlet of the second rectifying tower; liquid phase product temperature at the bottom liquid phase outlet of the first rectifying column: 34-38 ℃, flow: 4-8 Nm 3 /h，BCL 3 Mole fraction: 99.5 to 99.9 percent;
step 3: the liquid phase entering the second rectifying tower in the step 2 is subjected to secondary rectifying purification, the gas phase after the secondary rectifying purification enters the first tee joint through a gas phase outlet at the top of the second rectifying tower, a second tube side inlet of the second heat exchanger and a second tube side outlet of the second heat exchanger, the liquid phase entering the first tee joint is divided into two, one liquid phase enters a product tank through a fifth regulating valve, a product pump and a fourth regulating valve of the first tee joint, and the other liquid phase flows back into the second rectifying tower through a third end of the first tee joint and a second raw material liquid inlet of the second rectifying tower; gas phase temperature at the top gas phase outlet of the second rectifying column: 14-18 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid inlet of the second rectification column: 14-18 ℃, gas phase fraction: 0; liquid phase temperature at the inlet of the product pump: 14-18 ℃, BCL 3 The purity of the product is not lower than 99.9995%;
step 4: the gas phase after primary rectification and purification in the step 2 enters a first gas-liquid separator through a gas phase outlet at the top of a first rectifying tower, a second tube side inlet of a first heat exchanger and a second tube side outlet of the first heat exchanger to carry out gas-liquid separation, and a liquid phase after gas-liquid separation enters the first rectifying tower through a liquid phase outlet of the first gas-liquid separator and a second raw material liquid inlet at the upper middle part of the first rectifying tower; the top of the first rectifying tower Gas phase temperature at partial gas phase outlet: 33-37 ℃, BCL 3 Mole fraction: 99 to 99.5 percent; the liquid phase temperature of the second raw material liquid entering the first rectifying tower through the upper middle-upper part of the first rectifying tower is 14-18 ℃, and the liquid phase temperature of the BCL is the same as the liquid phase temperature of the BCL 3 Mole fraction: 99.1 to 99.5 percent, gas phase fraction: 0;
step 5: in the step 4, the gas phase after gas-liquid separation in the first gas-liquid separator sequentially passes through a gas phase outlet of the first gas-liquid separator, a fifth regulating valve and a second tee joint to enter an adsorption tower; gas phase temperature at the gas phase outlet of the first gas-liquid separator: 14-18 ℃, flow: 0.015 to 0.025Nm 3 Gas phase fraction/h: 1, a step of;
step 6: the liquid phase after the secondary rectification purification in the second rectifying tower in the step 3 enters the adsorption tower through a liquid phase outlet at the bottom of the second rectifying tower, a sixth regulating valve and a third end of a second tee joint; the liquid phase temperature of the liquid phase outlet at the bottom of the second rectifying tower is as follows: 16-20 ℃, the flow is: 0.6 to 1Nm 3 And (3) gas phase fraction: 0;
step 7: liquid ammonia from the liquid ammonia storage tank respectively enters a second tube side of the first heat exchanger and a second tube side of the second heat exchanger through a third tee joint, and enters an air conditioner working condition ice machine through the second tube side of the first heat exchanger, a second tube side outlet of the second heat exchanger, a fourth tee joint and an eleventh regulating valve; the temperature at the inlet of the air conditioner working condition ice machine is as follows: 8-12 ℃, and liquid ammonia: 100%, gas phase fraction: 100%.
Step 8: circulating water in the circulating water return tank respectively enters a first reboiler at the bottom of the first rectifying tower and a second reboiler at the bottom of the second rectifying tower through a fifth tee joint, and respectively enters the circulating water feeding tank through a sixth tee joint from an outlet of the first reboiler and an outlet of the second reboiler; the circulating water is hot water, and the mole fraction of the hot water is as follows: 100%; the outlet circulating liquid temperature of the first reboiler is as follows: 33-37 ℃, gas phase fraction: 0; temperature of the recycle liquid at the outlet of the second reboiler: 33-37 ℃, gas phase fraction: 0.
the invention adopts the rectification technology taking hot water as a heat source to provide heat for the whole system, the device and the production method for producing high-purity boron trichloride by double-tower rectification, the purity of liquid-phase boron trichloride of the product is not lower than 99.9995%, the blank of domestic high-purity boron trichloride production is filled, the foundation for development of the electronic industry and the semiconductor industry is laid, and the method has important significance. Compared with the traditional process technology, the invention has the following advantages: 1. the existing liquid ammonia is utilized to automatically provide cold energy for the system, and the stability of the system is utilized; 2. the rectification production mode with hot water as a heat source is adopted, the heat source is low in price, clean and environment-friendly, and the production cost of the product is low; 3. the purity of the product can reach more than 99.9995 percent, which is higher than the quality of similar products at home and abroad, and the production cost is low. The device and the method not only greatly improve the stability of the system, but also solve the problem of low product purity of the single-tower rectifying device; the method has the characteristics of high automation degree, stable operation and high purity of 99.9995 percent; provides guarantee for the research of special gas in the electronic industry and the development of the semiconductor field, and has good economic and social benefits.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
For a clearer understanding of the technical features, objects and effects of the present invention, embodiments of the present invention will now be described with reference to the drawings, in which like reference numerals refer to like parts throughout the various views. For simplicity of the drawing, only the parts relevant to the present invention are schematically shown in each drawing, and they do not represent the actual structure thereof as a product.
As shown in fig. 1, the invention relates to a device for producing high-purity boron trichloride and a production method thereof, the device comprises a raw material liquid buffer tank 17, a product tank 27, a liquid ammonia storage tank 29 and a circulating water return tank 32, wherein the raw material liquid buffer tank 17 is connected with a first raw material liquid inlet 34 at the middle upper part of a first rectifying tower 19 through a raw material liquid pump 18, a liquid phase outlet 41 at the bottom of the first rectifying tower 19 is connected with a first raw material liquid inlet 42 of a second rectifying tower 24, and a top gas phase outlet of the second rectifying tower 24 is connected with the product tank 27 through a first tube side inlet 43 of a second heat exchanger 23, a first tube side outlet 44 of the second heat exchanger 23, a first tee joint 13 and a product pump 26 in sequence. The gas phase outlet at the top of the first rectifying tower 19 is connected with the inlet of the first gas-liquid separator 21 through a first tube side inlet 35 of the first heat exchanger 22 and a first tube side outlet 36 of the first heat exchanger 22, the liquid phase outlet of the first gas-liquid separator 21 is connected with a second raw material liquid inlet 37 at the middle upper part of the first rectifying tower 19, and the gas phase outlet of the first gas-liquid separator 21 is connected with the adsorption tower 31 through a fifth regulating valve 5 and a second tee joint 16. The liquid phase outlet 48 at the bottom of the second rectifying tower 24 is connected with the adsorption tower 31 through the sixth regulating valve 6 and the third end of the second tee 16. The third end of the first tee 13 is connected with a second raw material liquid inlet 45 of the second rectifying tower 24. The liquid ammonia outlet of the liquid ammonia storage tank 29 is respectively connected with the second tube side inlet 39 of the first heat exchanger 22 and the second tube side inlet 47 of the second heat exchanger 23 through the third tee joint 33, the second tube side outlet 46 of the first heat exchanger 22 and the second tube side outlet 40 of the second heat exchanger 23 are respectively connected with the fourth tee joint 15, and the third end of the fourth tee joint 15 is connected with the air-conditioning ice machine 30; a ninth regulating valve 9 is arranged between the third tee 33 and the second tube side inlet 39 of the first heat exchanger 22, a tenth regulating valve 10 is arranged between the third tee 33 and the second tube side inlet 47 of the second heat exchanger 23, and an eleventh regulating valve 11 is arranged between the third end of the fourth tee 15 and the air conditioner ice maker 30. The water outlet of the circulating water return water tank 32 is respectively connected with a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and the outlets of the first reboiler 20 and the second reboiler 25 are respectively connected with a circulating water upper water tank 28 through a sixth tee joint 14; a seventh regulating valve 7 is arranged between the fifth tee 12 and the first reboiler 20, and an eighth regulating valve 8 is arranged between the fifth tee 12 and the second reboiler 25. A first regulating valve 1 is arranged between the raw material liquid buffer tank 17 and the raw material liquid pump 18, a second regulating valve 2 is arranged between a liquid phase outlet 41 at the bottom of the first rectifying tower 19 and a first raw material liquid inlet 42 of the second rectifying tower 24, a third regulating valve 3 is arranged between the first tee 13 and the product pump 26, and a fourth regulating valve 4 is arranged between the product pump 26 and the product tank 27.
The production method of the device for producing high-purity boron trichloride comprises the following steps:
step 1: the raw material liquid in the raw material liquid buffer tank 17 sequentially passes through the first regulating valve 1, the raw material liquid pump 18 and the first raw material liquid inlet 34 at the middle upper part of the first rectifying tower 19 to enter the first rectifying tower 19; the main composition of the raw material liquid is as follows: boron trichloride, silicon tetrachloride, hydrogen chloride, chlorine, carbon monoxide, oxygen, carbon dioxide, nitrogen, methane, argon and moisture; temperature of raw material liquid: 35-40 ℃, pressure: 0.2Mpa, flow: 5-7 Nm 3 Gas phase fraction/h: 0, BCL 3 Mole fraction: 98% -99.5%;
step 2: the raw material liquid entering the first rectifying tower 19 in the step 1 is subjected to primary rectifying purification, and the liquid phase after primary rectifying purification enters the second rectifying tower 24 through a liquid phase outlet 41 at the bottom of the first rectifying tower 19, a second regulating valve 2 and a first raw material liquid inlet 42 of the second rectifying tower 24; liquid phase product temperature at bottom liquid phase outlet 41 of first rectification column 19: 34-38 ℃, flow: 4-8 Nm 3 /h，BCL 3 Mole fraction: 99.5 to 99.9 percent;
step 3: the liquid phase entering the second rectifying tower 24 in the step 2 is subjected to secondary rectifying purification, the gas phase after the secondary rectifying purification enters the first tee 13 through a gas phase outlet at the top of the second rectifying tower 24, a second tube side inlet 43 of the second heat exchanger 23 and a second tube side outlet 44 of the second heat exchanger 23, the liquid phase entering the first tee 13 is divided into two strands, one liquid phase enters the product tank 27 through a fifth regulating valve 5, a product pump 26 and a fourth regulating valve 4 of the first tee 13, and the other liquid phase flows back into the second rectifying tower 24 through a third end of the first tee 13 and a second raw material liquid inlet 45 of the second rectifying tower 24; gas phase temperature at the top gas phase outlet of the second rectification column 24: 14-18 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid inlet 45 of the second rectifying column 24: 14-18 ℃, gas phase fraction: 0; liquid phase temperature at the inlet of product pump 26: 14-18 ℃, BCL 3 The purity of the product is not lower than 99.9995%;
step 4: the gas phase after primary rectification and purification in the step 2 enters the first gas-liquid separator through a gas phase outlet at the top of the first rectifying tower 19, a second tube side inlet 35 of the first heat exchanger 22 and a second tube side outlet 36 of the first heat exchanger 2221, and the liquid phase after gas-liquid separation enters the first rectifying tower 19 through a liquid phase outlet of the first gas-liquid separator 21 and a second raw material liquid inlet 38 at the middle upper part of the first rectifying tower 19; gas phase temperature at the top gas phase outlet of the first rectifying column 19: 33-37 ℃, BCL 3 Mole fraction: 99 to 99.5 percent; the liquid phase temperature of the second raw material liquid entering the first rectifying tower 19 through the second raw material liquid inlet 38 at the middle and upper part of the first rectifying tower 19 is 14-18 ℃, and the BCL 3 Mole fraction: 99.1 to 99.5 percent, gas phase fraction: 0;
step 5: in the step 4, the gas phase after gas-liquid separation in the first gas-liquid separator 21 sequentially passes through a gas phase outlet of the first gas-liquid separator 21, the fifth regulating valve 5 and the second tee joint 16 to enter the adsorption tower 31; gas phase temperature at the gas phase outlet of the first gas-liquid separator 21: 14-18 ℃, flow: 0.015 to 0.025Nm 3 Gas phase fraction/h: 1, a step of;
step 6: in the step 3, the liquid phase purified by the secondary rectification in the second rectification column 24 enters the adsorption column 31 through a liquid phase outlet 48 at the bottom of the second rectification column 24, a sixth regulating valve 6 and a third end of the second tee 16; the liquid phase temperature of the liquid phase outlet 48 at the bottom of the second rectifying column 24 is: 16-20 ℃, the flow is: 0.6 to 1Nm 3 And (3) gas phase fraction: 0;
step 7: liquid ammonia from the liquid ammonia storage tank 29 enters the second tube side of the first heat exchanger 22 and the second tube side of the second heat exchanger 23 through the third tee joint 33 respectively, and enters the air conditioning ice maker 30 through the second tube side of the first heat exchanger 22, the second tube side outlet of the second heat exchanger 23, the fourth tee joint 15 and the eleventh regulating valve 11; the temperature at the inlet of the air conditioner working condition ice machine 30 is as follows: 8-12 ℃, and liquid ammonia: 100%, gas phase fraction: 100%.
Step 8: circulating water in the circulating water return tank 32 respectively enters a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and respectively enters a circulating water upper water tank 28 through a sixth tee joint 14 from an outlet of the first reboiler 20 and an outlet of the second reboiler 25; the circulating water is hot water, and the mole fraction of the hot water is as follows: 100%; the outlet circulation liquid temperature of the first reboiler 20 is: 33-37 ℃, gas phase fraction: 0; the temperature of the circulating liquid at the outlet of the second reboiler 25: 33-37 ℃, gas phase fraction: 0.
the invention relates to a device and a method for producing high-purity boron trichloride, which refer to the high-purity boron trichloride enterprise standard of China industry gas institute and foreign gas company, and the boron trichloride gas standard for the domestic electronic industry: 99.9995% (GB/T17874-2010), ULSI grade standard abroad: 99.999%, ref: the fifth volume of the general national institute of Industrial gases, 4384, page tables II.3.95-13 and II.3.95-14. The books are published by the university of the company, china industry gas industry Association. The process method has the advantages that a rectification production mode using hot water as a heat source is adopted, the heat source is low in price, clean and environment-friendly, and the production cost of the product is low; on the other hand, the existing liquid ammonia is utilized to automatically provide cold for the system, so that the system stability is good; the industrial grade boron trichloride is purified by double-tower rectification, the purity of the product can reach more than 99.9995 percent, the product is higher than the quality of similar products in the domestic and foreign electronic industries, the production cost is low, and in addition, an automatic remote control start-stop product pump can be realized by arranging a regulating valve at an inlet and an outlet of the product pump.
The invention will now be further illustrated with reference to examples for a more detailed explanation of the invention. Specific examples are as follows:
example 1
The device for producing high-purity boron trichloride comprises a raw material liquid buffer tank 17, a product tank 27, a liquid ammonia storage tank 29 and a circulating water return tank 32, wherein the raw material liquid buffer tank 17 is connected with a first raw material liquid inlet 34 at the middle upper part of a first rectifying tower 19 through a raw material liquid pump 18, a liquid phase outlet 41 at the bottom of the first rectifying tower 19 is connected with a first raw material liquid inlet 42 of a second rectifying tower 24, and a top gas phase outlet of the second rectifying tower 24 is sequentially connected with the product tank 27 through a first tube side inlet 43 of a second heat exchanger 23, a first tube side outlet 44 of the second heat exchanger 23, a first tee joint 13 and a product pump 26. The gas phase outlet at the top of the first rectifying tower 19 is connected with the inlet of the first gas-liquid separator 21 through a first tube side inlet 35 of the first heat exchanger 22 and a first tube side outlet 36 of the first heat exchanger 22, the liquid phase outlet of the first gas-liquid separator 21 is connected with a second raw material liquid inlet 37 at the middle upper part of the first rectifying tower 19, and the gas phase outlet of the first gas-liquid separator 21 is connected with the adsorption tower 31 through a fifth regulating valve 5 and a second tee joint 16. The liquid phase outlet 48 at the bottom of the second rectifying tower 24 is connected with the adsorption tower 31 through the sixth regulating valve 6 and the third end of the second tee 16. The third end of the first tee 13 is connected with a second raw material liquid inlet 45 of the second rectifying tower 24. The liquid ammonia outlet of the liquid ammonia storage tank 29 is respectively connected with the second tube side inlet 39 of the first heat exchanger 22 and the second tube side inlet 47 of the second heat exchanger 23 through the third tee joint 33, the second tube side outlet 46 of the first heat exchanger 22 and the second tube side outlet 40 of the second heat exchanger 23 are respectively connected with the fourth tee joint 15, and the third end of the fourth tee joint 15 is connected with the air-conditioning ice machine 30; a ninth regulating valve 9 is arranged between the third tee 33 and the second tube side inlet 39 of the first heat exchanger 22, a tenth regulating valve 10 is arranged between the third tee 33 and the second tube side inlet 47 of the second heat exchanger 23, and an eleventh regulating valve 11 is arranged between the third end of the fourth tee 15 and the air conditioner ice maker 30. The water outlet of the circulating water return water tank 32 is respectively connected with a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and the outlets of the first reboiler 20 and the second reboiler 25 are respectively connected with a circulating water upper water tank 28 through a sixth tee joint 14; a seventh regulating valve 7 is arranged between the fifth tee 12 and the first reboiler 20, and an eighth regulating valve 8 is arranged between the fifth tee 12 and the second reboiler 25. A first regulating valve 1 is arranged between the raw material liquid buffer tank 17 and the raw material liquid pump 18, a second regulating valve 2 is arranged between a liquid phase outlet 41 at the bottom of the first rectifying tower 19 and a first raw material liquid inlet 42 of the second rectifying tower 24, a third regulating valve 3 is arranged between the first tee 13 and the product pump 26, and a fourth regulating valve 4 is arranged between the product pump 26 and the product tank 27.
The production method of the device for producing high-purity boron trichloride comprises the following steps:
step 1: the raw material liquid in the raw material liquid buffer tank 17 sequentially passes through the first regulating valve 1, the raw material liquid pump 18 and the first raw material liquid inlet 34 at the middle upper part of the first rectifying tower 19 to enter the first rectifying tower 19; by a means ofThe main composition of the raw material liquid is as follows: boron trichloride, silicon tetrachloride, hydrogen chloride, chlorine, carbon monoxide, oxygen, carbon dioxide, nitrogen, methane, argon and moisture; temperature of raw material liquid: 35 ℃, pressure: 0.2Mpa, flow: 5Nm 3 Gas phase fraction/h: 0, BCL 3 Mole fraction: 98% -99.5%;
step 2: the raw material liquid entering the first rectifying tower 19 in the step 1 is subjected to primary rectifying purification, and the liquid phase after primary rectifying purification enters the second rectifying tower 24 through a liquid phase outlet 41 at the bottom of the first rectifying tower 19, a second regulating valve 2 and a first raw material liquid inlet 42 of the second rectifying tower 24; liquid phase product temperature at bottom liquid phase outlet 41 of first rectification column 19: 34 ℃, flow rate: 4Nm 3 /h，BCL 3 Mole fraction: 99.5 to 99.9 percent;
step 3: the liquid phase entering the second rectifying tower 24 in the step 2 is subjected to secondary rectifying purification, the gas phase after the secondary rectifying purification enters the first tee 13 through a gas phase outlet at the top of the second rectifying tower 24, a second tube side inlet 43 of the second heat exchanger 23 and a second tube side outlet 44 of the second heat exchanger 23, the liquid phase entering the first tee 13 is divided into two strands, one liquid phase enters the product tank 27 through a fifth regulating valve 5, a product pump 26 and a fourth regulating valve 4 of the first tee 13, and the other liquid phase flows back into the second rectifying tower 24 through a third end of the first tee 13 and a second raw material liquid inlet 45 of the second rectifying tower 24; gas phase temperature at the top gas phase outlet of the second rectification column 24: 14 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid inlet 45 of the second rectifying column 24: 14 ℃, gas phase fraction: 0; liquid phase temperature at the inlet of product pump 26: 14 ℃, BCL 3 The purity of the product is not lower than 99.9995%;
step 4: the gas phase after primary rectification and purification in the step 2 enters the first gas-liquid separator 21 through a gas phase outlet at the top of the first rectifying tower 19, a second tube side inlet 35 of the first heat exchanger 22 and a second tube side outlet 36 of the first heat exchanger 22 to carry out gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower 19 through a liquid phase outlet of the first gas-liquid separator 21 and a second raw material liquid inlet 38 at the middle upper part of the first rectifying tower 19; the top of the first rectifying tower 19Gas phase temperature at gas phase outlet: 33 ℃, BCL 3 Mole fraction: 99 to 99.5 percent; the liquid phase temperature entering the first rectifying tower 19 through the second raw material liquid inlet 38 at the middle upper part of the first rectifying tower 19 is 14 ℃, and the BCL 3 Mole fraction: 99.1 to 99.5 percent, gas phase fraction: 0;
step 5: in the step 4, the gas phase after gas-liquid separation in the first gas-liquid separator 21 sequentially passes through a gas phase outlet of the first gas-liquid separator 21, the fifth regulating valve 5 and the second tee joint 16 to enter the adsorption tower 31; gas phase temperature at the gas phase outlet of the first gas-liquid separator 21: 14 ℃, flow rate: 0.015Nm 3 Gas phase fraction/h: 1, a step of;
step 6: in the step 3, the liquid phase purified by the secondary rectification in the second rectification column 24 enters the adsorption column 31 through a liquid phase outlet 48 at the bottom of the second rectification column 24, a sixth regulating valve 6 and a third end of the second tee 16; the liquid phase temperature of the liquid phase outlet 48 at the bottom of the second rectifying column 24 is: 16 ℃, the flow rate is: 0.6Nm 3 And (3) gas phase fraction: 0;
step 7: liquid ammonia from the liquid ammonia storage tank 29 enters the second tube side of the first heat exchanger 22 and the second tube side of the second heat exchanger 23 through the third tee joint 33 respectively, and enters the air conditioning ice maker 30 through the second tube side of the first heat exchanger 22, the second tube side outlet of the second heat exchanger 23, the fourth tee joint 15 and the eleventh regulating valve 11; the temperature at the inlet of the air conditioner working condition ice machine 30 is as follows: 8 ℃, liquid ammonia composition: 100%, gas phase fraction: 100%.
Step 8: circulating water in the circulating water return tank 32 respectively enters a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and respectively enters a circulating water upper water tank 28 through a sixth tee joint 14 from an outlet of the first reboiler 20 and an outlet of the second reboiler 25; the circulating water is hot water, and the mole fraction of the hot water is as follows: 100%; the outlet circulation liquid temperature of the first reboiler 20 is: 33 ℃, gas phase fraction: 0; the temperature of the circulating liquid at the outlet of the second reboiler 25: 33 ℃, gas phase fraction: 0.
example 2
The device for producing high-purity boron trichloride comprises a raw material liquid buffer tank 17, a product tank 27, a liquid ammonia storage tank 29 and a circulating water return tank 32, wherein the raw material liquid buffer tank 17 is connected with a first raw material liquid inlet 34 at the middle upper part of a first rectifying tower 19 through a raw material liquid pump 18, a liquid phase outlet 41 at the bottom of the first rectifying tower 19 is connected with a first raw material liquid inlet 42 of a second rectifying tower 24, and a top gas phase outlet of the second rectifying tower 24 is sequentially connected with the product tank 27 through a first tube side inlet 43 of a second heat exchanger 23, a first tube side outlet 44 of the second heat exchanger 23, a first tee joint 13 and a product pump 26. The gas phase outlet at the top of the first rectifying tower 19 is connected with the inlet of the first gas-liquid separator 21 through a first tube side inlet 35 of the first heat exchanger 22 and a first tube side outlet 36 of the first heat exchanger 22, the liquid phase outlet of the first gas-liquid separator 21 is connected with a second raw material liquid inlet 37 at the middle upper part of the first rectifying tower 19, and the gas phase outlet of the first gas-liquid separator 21 is connected with the adsorption tower 31 through a fifth regulating valve 5 and a second tee joint 16. The liquid phase outlet 48 at the bottom of the second rectifying tower 24 is connected with the adsorption tower 31 through the sixth regulating valve 6 and the third end of the second tee 16. The third end of the first tee 13 is connected with a second raw material liquid inlet 45 of the second rectifying tower 24. The liquid ammonia outlet of the liquid ammonia storage tank 29 is respectively connected with the second tube side inlet 39 of the first heat exchanger 22 and the second tube side inlet 47 of the second heat exchanger 23 through the third tee joint 33, the second tube side outlet 46 of the first heat exchanger 22 and the second tube side outlet 40 of the second heat exchanger 23 are respectively connected with the fourth tee joint 15, and the third end of the fourth tee joint 15 is connected with the air-conditioning ice machine 30; a ninth regulating valve 9 is arranged between the third tee 33 and the second tube side inlet 39 of the first heat exchanger 22, a tenth regulating valve 10 is arranged between the third tee 33 and the second tube side inlet 47 of the second heat exchanger 23, and an eleventh regulating valve 11 is arranged between the third end of the fourth tee 15 and the air conditioner ice maker 30. The water outlet of the circulating water return water tank 32 is respectively connected with a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and the outlets of the first reboiler 20 and the second reboiler 25 are respectively connected with a circulating water upper water tank 28 through a sixth tee joint 14; a seventh regulating valve 7 is arranged between the fifth tee 12 and the first reboiler 20, and an eighth regulating valve 8 is arranged between the fifth tee 12 and the second reboiler 25. A first regulating valve 1 is arranged between the raw material liquid buffer tank 17 and the raw material liquid pump 18, a second regulating valve 2 is arranged between a liquid phase outlet 41 at the bottom of the first rectifying tower 19 and a first raw material liquid inlet 42 of the second rectifying tower 24, a third regulating valve 3 is arranged between the first tee 13 and the product pump 26, and a fourth regulating valve 4 is arranged between the product pump 26 and the product tank 27.
The production method of the device for producing high-purity boron trichloride comprises the following steps:
step 1: the raw material liquid in the raw material liquid buffer tank 17 sequentially passes through the first regulating valve 1, the raw material liquid pump 18 and the first raw material liquid inlet 34 at the middle upper part of the first rectifying tower 19 to enter the first rectifying tower 19; the main composition of the raw material liquid is as follows: boron trichloride, silicon tetrachloride, hydrogen chloride, chlorine, carbon monoxide, oxygen, carbon dioxide, nitrogen, methane, argon and moisture; temperature of raw material liquid: 40 ℃, pressure: 0.2Mpa, flow: 7Nm 3 Gas phase fraction/h: 0, BCL 3 Mole fraction: 98% -99.5%;
step 2: the raw material liquid entering the first rectifying tower 19 in the step 1 is subjected to primary rectifying purification, and the liquid phase after primary rectifying purification enters the second rectifying tower 24 through a liquid phase outlet 41 at the bottom of the first rectifying tower 19, a second regulating valve 2 and a first raw material liquid inlet 42 of the second rectifying tower 24; liquid phase product temperature at bottom liquid phase outlet 41 of first rectification column 19: 38 ℃, flow rate: 8Nm 3 /h，BCL 3 Mole fraction: 99.5 to 99.9 percent;
step 3: the liquid phase entering the second rectifying tower 24 in the step 2 is subjected to secondary rectifying purification, the gas phase after the secondary rectifying purification enters the first tee 13 through a gas phase outlet at the top of the second rectifying tower 24, a second tube side inlet 43 of the second heat exchanger 23 and a second tube side outlet 44 of the second heat exchanger 23, the liquid phase entering the first tee 13 is divided into two strands, one liquid phase enters the product tank 27 through a fifth regulating valve 5, a product pump 26 and a fourth regulating valve 4 of the first tee 13, and the other liquid phase flows back into the second rectifying tower 24 through a third end of the first tee 13 and a second raw material liquid inlet 45 of the second rectifying tower 24; gas phase temperature at the top gas phase outlet of the second rectification column 24: 18 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid inlet 45 of the second rectifying column 24: 18 ℃, gas phase fraction: 0; liquid phase temperature at the inlet of product pump 26: 18 ℃, BCL 3 The purity of the product is not lower than 99.9995%;
step 4: the gas phase after primary rectification and purification in the step 2 enters the first gas-liquid separator 21 through a gas phase outlet at the top of the first rectifying tower 19, a second tube side inlet 35 of the first heat exchanger 22 and a second tube side outlet 36 of the first heat exchanger 22 to carry out gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower 19 through a liquid phase outlet of the first gas-liquid separator 21 and a second raw material liquid inlet 38 at the middle upper part of the first rectifying tower 19; gas phase temperature at the top gas phase outlet of the first rectifying column 19: 37 ℃, BCL 3 Mole fraction: 99 to 99.5 percent; the liquid phase temperature entering the first rectifying tower 19 through the second raw material liquid inlet 38 at the middle upper part of the first rectifying tower 19 is 18 ℃, and the BCL 3 Mole fraction: 99.1 to 99.5 percent, gas phase fraction: 0;
step 5: in the step 4, the gas phase after gas-liquid separation in the first gas-liquid separator 21 sequentially passes through a gas phase outlet of the first gas-liquid separator 21, the fifth regulating valve 5 and the second tee joint 16 to enter the adsorption tower 31; gas phase temperature at the gas phase outlet of the first gas-liquid separator 21: 18 ℃, flow rate: 0.025Nm 3 Gas phase fraction/h: 1, a step of;
step 6: in the step 3, the liquid phase purified by the secondary rectification in the second rectification column 24 enters the adsorption column 31 through a liquid phase outlet 48 at the bottom of the second rectification column 24, a sixth regulating valve 6 and a third end of the second tee 16; the liquid phase temperature of the liquid phase outlet 48 at the bottom of the second rectifying column 24 is: 16-20 ℃, the flow is: 1Nm 3 And (3) gas phase fraction: 0;
step 7: liquid ammonia from the liquid ammonia storage tank 29 enters the second tube side of the first heat exchanger 22 and the second tube side of the second heat exchanger 23 through the third tee joint 33 respectively, and enters the air conditioning ice maker 30 through the second tube side of the first heat exchanger 22, the second tube side outlet of the second heat exchanger 23, the fourth tee joint 15 and the eleventh regulating valve 11; the temperature at the inlet of the air conditioner working condition ice machine 30 is as follows: 12 ℃, liquid ammonia composition: 100%, gas phase fraction: 100%.
Step 8: circulating water in the circulating water return tank 32 respectively enters a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and respectively enters a circulating water upper water tank 28 through a sixth tee joint 14 from an outlet of the first reboiler 20 and an outlet of the second reboiler 25; the circulating water is hot water, and the mole fraction of the hot water is as follows: 100%; the outlet circulation liquid temperature of the first reboiler 20 is: 33-37 ℃, gas phase fraction: 0; the temperature of the circulating liquid at the outlet of the second reboiler 25: 33-37 ℃, gas phase fraction: 0.
Example 3
The device for producing high-purity boron trichloride comprises a raw material liquid buffer tank 17, a product tank 27, a liquid ammonia storage tank 29 and a circulating water return tank 32, wherein the raw material liquid buffer tank 17 is connected with a first raw material liquid inlet 34 at the middle upper part of a first rectifying tower 19 through a raw material liquid pump 18, a liquid phase outlet 41 at the bottom of the first rectifying tower 19 is connected with a first raw material liquid inlet 42 of a second rectifying tower 24, and a top gas phase outlet of the second rectifying tower 24 is sequentially connected with the product tank 27 through a first tube side inlet 43 of a second heat exchanger 23, a first tube side outlet 44 of the second heat exchanger 23, a first tee joint 13 and a product pump 26. The gas phase outlet at the top of the first rectifying tower 19 is connected with the inlet of the first gas-liquid separator 21 through a first tube side inlet 35 of the first heat exchanger 22 and a first tube side outlet 36 of the first heat exchanger 22, the liquid phase outlet of the first gas-liquid separator 21 is connected with a second raw material liquid inlet 37 at the middle upper part of the first rectifying tower 19, and the gas phase outlet of the first gas-liquid separator 21 is connected with the adsorption tower 31 through a fifth regulating valve 5 and a second tee joint 16. The liquid phase outlet 48 at the bottom of the second rectifying tower 24 is connected with the adsorption tower 31 through the sixth regulating valve 6 and the third end of the second tee 16. The third end of the first tee 13 is connected with a second raw material liquid inlet 45 of the second rectifying tower 24. The liquid ammonia outlet of the liquid ammonia storage tank 29 is respectively connected with the second tube side inlet 39 of the first heat exchanger 22 and the second tube side inlet 47 of the second heat exchanger 23 through the third tee joint 33, the second tube side outlet 46 of the first heat exchanger 22 and the second tube side outlet 40 of the second heat exchanger 23 are respectively connected with the fourth tee joint 15, and the third end of the fourth tee joint 15 is connected with the air-conditioning ice machine 30; a ninth regulating valve 9 is arranged between the third tee 33 and the second tube side inlet 39 of the first heat exchanger 22, a tenth regulating valve 10 is arranged between the third tee 33 and the second tube side inlet 47 of the second heat exchanger 23, and an eleventh regulating valve 11 is arranged between the third end of the fourth tee 15 and the air conditioner ice maker 30. The water outlet of the circulating water return water tank 32 is respectively connected with a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and the outlets of the first reboiler 20 and the second reboiler 25 are respectively connected with a circulating water upper water tank 28 through a sixth tee joint 14; a seventh regulating valve 7 is arranged between the fifth tee 12 and the first reboiler 20, and an eighth regulating valve 8 is arranged between the fifth tee 12 and the second reboiler 25. A first regulating valve 1 is arranged between the raw material liquid buffer tank 17 and the raw material liquid pump 18, a second regulating valve 2 is arranged between a liquid phase outlet 41 at the bottom of the first rectifying tower 19 and a first raw material liquid inlet 42 of the second rectifying tower 24, a third regulating valve 3 is arranged between the first tee 13 and the product pump 26, and a fourth regulating valve 4 is arranged between the product pump 26 and the product tank 27.
The production method of the device for producing high-purity boron trichloride comprises the following steps:
step 1: the raw material liquid in the raw material liquid buffer tank 17 sequentially passes through the first regulating valve 1, the raw material liquid pump 18 and the first raw material liquid inlet 34 at the middle upper part of the first rectifying tower 19 to enter the first rectifying tower 19; the main composition of the raw material liquid is as follows: boron trichloride, silicon tetrachloride, hydrogen chloride, chlorine, carbon monoxide, oxygen, carbon dioxide, nitrogen, methane, argon and moisture; temperature of raw material liquid: 37.5 ℃, pressure: 0.2Mpa, flow: 6Nm 3 Gas phase fraction/h: 0, BCL 3 Mole fraction: 98% -99.5%;
step 2: the raw material liquid entering the first rectifying tower 19 in the step 1 is subjected to primary rectifying purification, and the liquid phase after primary rectifying purification enters the second rectifying tower 24 through a liquid phase outlet 41 at the bottom of the first rectifying tower 19, a second regulating valve 2 and a first raw material liquid inlet 42 of the second rectifying tower 24; liquid phase product temperature at bottom liquid phase outlet 41 of first rectification column 19: 36 ℃, flow rate: 6Nm 3 /h，BCL 3 Mole fraction: 99.5 to 99.9 percent;
step 3: the liquid phase entering the second rectifying tower 24 in the step 2 is subjected to secondary rectifying purification, the gas phase after the secondary rectifying purification enters the first tee 13 through a gas phase outlet at the top of the second rectifying tower 24, a second tube side inlet 43 of the second heat exchanger 23 and a second tube side outlet 44 of the second heat exchanger 23, the liquid phase entering the first tee 13 is divided into two strands, one liquid phase enters the product tank 27 through a fifth regulating valve 5, a product pump 26 and a fourth regulating valve 4 of the first tee 13, and the other liquid phase flows back into the second rectifying tower 24 through a third end of the first tee 13 and a second raw material liquid inlet 45 of the second rectifying tower 24; gas phase temperature at the top gas phase outlet of the second rectification column 24: 16 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid inlet 45 of the second rectifying column 24: 16 ℃, gas phase fraction: 0; liquid phase temperature at the inlet of product pump 26: 16 ℃, BCL 3 The purity of the product is not lower than 99.9995%;
step 4: the gas phase after primary rectification and purification in the step 2 enters the first gas-liquid separator 21 through a gas phase outlet at the top of the first rectifying tower 19, a second tube side inlet 35 of the first heat exchanger 22 and a second tube side outlet 36 of the first heat exchanger 22 to carry out gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower 19 through a liquid phase outlet of the first gas-liquid separator 21 and a second raw material liquid inlet 38 at the middle upper part of the first rectifying tower 19; gas phase temperature at the top gas phase outlet of the first rectifying column 19: 35 ℃, BCL 3 Mole fraction: 99 to 99.5 percent; the liquid phase temperature entering the first rectifying tower 19 through the second raw material liquid inlet 38 at the middle upper part of the first rectifying tower 19 is 16 ℃, and the BCL 3 Mole fraction: 99.1 to 99.5 percent, gas phase fraction: 0;
step 5: in the step 4, the gas phase after gas-liquid separation in the first gas-liquid separator 21 sequentially passes through a gas phase outlet of the first gas-liquid separator 21, the fifth regulating valve 5 and the second tee joint 16 to enter the adsorption tower 31; gas phase temperature at the gas phase outlet of the first gas-liquid separator 21: 16 ℃, flow rate: 0.020Nm 3 Gas phase fraction/h: 1, a step of;
step 6: the second rectification and extraction in the second rectification column 24 in the step 3 The pure liquid phase enters the adsorption tower 31 through a liquid phase outlet 48 at the bottom of the second rectifying tower 24, a sixth regulating valve 6 and a third end of the second tee 16; the liquid phase temperature of the liquid phase outlet 48 at the bottom of the second rectifying column 24 is: 18 ℃, the flow is: 0.8Nm 3 And (3) gas phase fraction: 0;
step 7: liquid ammonia from the liquid ammonia storage tank 29 enters the second tube side of the first heat exchanger 22 and the second tube side of the second heat exchanger 23 through the third tee joint 33 respectively, and enters the air conditioning ice maker 30 through the second tube side of the first heat exchanger 22, the second tube side outlet of the second heat exchanger 23, the fourth tee joint 15 and the eleventh regulating valve 11; the temperature at the inlet of the air conditioner working condition ice machine 30 is as follows: 10 ℃, liquid ammonia composition: 100%, gas phase fraction: 100%.
Step 8: circulating water in the circulating water return tank 32 respectively enters a first reboiler 20 at the bottom of the first rectifying tower 19 and a second reboiler 25 at the bottom of the second rectifying tower 19 through a fifth tee joint 12, and respectively enters a circulating water upper water tank 28 through a sixth tee joint 14 from an outlet of the first reboiler 20 and an outlet of the second reboiler 25; the circulating water is hot water, and the mole fraction of the hot water is as follows: 100%; the outlet circulation liquid temperature of the first reboiler 20 is: 35 ℃, gas phase fraction: 0; the temperature of the circulating liquid at the outlet of the second reboiler 25: 35 ℃, gas phase fraction: 0.
In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "end," "inner wall," "front end," etc. are based on the orientation or positional relationship shown in the drawings, and are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element in question must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. In the description of the present invention, it should be noted that, unless explicitly stated and limited otherwise, the terms "provided with," "mounted to," "connected to," and the like are to be construed broadly, and may be, for example, fixedly connected, integrally connected, or detachably connected; or the communication between the two components is also possible; may be directly connected or indirectly connected through an intermediate medium, and the specific meaning of the above terms in the present invention will be understood by those skilled in the art according to the specific circumstances. Finally, it is noted that the above-mentioned preferred embodiments are only intended to illustrate rather than limit the invention, and that, although the invention has been described in detail by means of the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (8)
1. A production method of a device for producing high-purity boron trichloride is characterized by comprising the following steps: the production method comprises the following steps:
step 1: the raw material liquid in the raw material liquid buffer tank (17) sequentially passes through a first regulating valve (1), a raw material liquid pump (18) and a first raw material liquid inlet (34) at the upper middle part of the first rectifying tower to enter the first rectifying tower (19); the main composition of the raw material liquid is as follows: boron trichloride, silicon tetrachloride, hydrogen chloride, chlorine, carbon monoxide, oxygen, carbon dioxide, nitrogen, methane, argon and moisture; temperature of raw material liquid: 35-40 ℃, pressure: 0.2Mpa, flow: 5-7 Nm 3 Gas phase fraction/h: 0, BCL 3 Mole fraction: 98% -99.5%;
step 2: the raw material liquid entering the first rectifying tower (19) in the step 1 is subjected to primary rectification purification, and the liquid phase after primary rectification purification enters the second rectifying tower (24) through a liquid phase outlet (41) at the bottom of the first rectifying tower, a second regulating valve (2) and a first raw material liquid inlet (42) of the second rectifying tower; liquid phase product temperature at the bottom liquid phase outlet (41) of the first rectification column: 34-38 ℃, flow: 4-8 Nm 3 /h，BCL 3 Mole fraction: 99.5 to 99.9 percent;
step 3: the liquid phase entering the second rectifying tower (24) in the step 2 is subjected to secondary rectifying purification, the gas phase after the secondary rectifying purification enters the first tee (13) through a gas phase outlet at the top of the second rectifying tower (24), a second tube pass inlet (43) of a second heat exchanger and a second tube pass outlet (44) of the second heat exchanger, the liquid phase entering the first tee (13) is divided into two streams, and one stream of liquid phase passes through a fifth regulating valve (5) of the first tee (13), a product pump (26) and a first outlet of the second heat exchanger The fourth regulating valve (4) enters the product tank (27), and the other liquid phase flows back into the second rectifying tower (24) through the third end of the first tee joint (13) and the second raw material liquid inlet (45) of the second rectifying tower; gas phase temperature at the top gas phase outlet of the second rectifying column (24): 14-18 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid inlet (45) of the second rectifying column: 14-18 ℃, gas phase fraction: 0; liquid phase temperature at the inlet of the product pump (26): 14-18 ℃, BCL 3 The purity of the product is not lower than 99.9995%;
step 4: the gas phase after primary rectification and purification in the step 2 enters a first gas-liquid separator (21) through a gas phase outlet at the top of a first rectifying tower (19), a second tube side inlet (35) of a first heat exchanger and a second tube side outlet (36) of the first heat exchanger to carry out gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower (19) through a liquid phase outlet of the first gas-liquid separator (21) and a second raw material liquid inlet (38) at the upper middle part of the first rectifying tower (19); gas phase temperature at the top gas phase outlet of the first rectifying column (19): 33-37 ℃, BCL 3 Mole fraction: 99 to 99.5 percent; the liquid phase temperature of the liquid phase entering the first rectifying tower (19) through a second raw material liquid inlet (38) at the upper middle part of the first rectifying tower (19) is 14-18 ℃, and the liquid phase temperature of the liquid phase is BCL 3 Mole fraction: 99.1 to 99.5 percent, gas phase fraction: 0;
step 5: in the step 4, the gas phase after gas-liquid separation in the first gas-liquid separator (21) sequentially passes through a gas phase outlet of the first gas-liquid separator (21), a fifth regulating valve (5) and a second tee joint (16) to enter an adsorption tower (31); gas phase temperature of the gas phase outlet of the first gas-liquid separator (21): 14-18 ℃, flow: 0.015 to 0.025Nm 3 Gas phase fraction/h: 1, a step of;
step 6: in the step 3, the liquid phase after the secondary rectification purification in the second rectifying tower (24) enters the adsorption tower (31) through a liquid phase outlet (48) at the bottom of the second rectifying tower, a sixth regulating valve (6) and a third end of a second tee joint (16); the liquid phase temperature of the liquid phase outlet (48) at the bottom of the second rectifying tower is as follows: 16-20 ℃, the flow is: 0.6 to 1Nm 3 And (3) gas phase fraction: 0;
step 7: liquid ammonia from a liquid ammonia storage tank (29) respectively enters a second tube side of the first heat exchanger (22) and a second tube side of the second heat exchanger (23) through a third tee joint (33), and enters an air conditioner working condition ice machine (30) through the second tube side of the first heat exchanger (22), a second tube side outlet of the second heat exchanger (23), a fourth tee joint (15) and an eleventh regulating valve (11); the temperature at the inlet of the air conditioner working condition ice machine (30) is as follows: 8-12 ℃, and liquid ammonia: 100%, gas phase fraction: 100%;
Step 8: circulating water in the circulating water return tank (32) respectively enters a first reboiler (20) at the bottom of the first rectifying tower (19) and a second reboiler (25) at the bottom of the second rectifying tower (24) through a fifth tee joint (12), and respectively enters a circulating water upper tank (28) through a sixth tee joint (14) from an outlet of the first reboiler (20) and an outlet of the second reboiler (25); the circulating water is hot water, and the mole fraction of the hot water is as follows: 100%; the outlet circulating liquid temperature of the first reboiler (20) is as follows: 33-37 ℃, gas phase fraction: 0; temperature of the circulating liquid at the outlet of the second reboiler (25): 33-37 ℃, gas phase fraction: 0.
2. the method for producing an apparatus for producing high purity boron trichloride according to claim 1, wherein: the device for producing the high-purity boron trichloride comprises a raw material liquid buffer tank (17), a product tank (27), a liquid ammonia storage tank (29) and a circulating water return tank (32), and is characterized in that: the raw material liquid buffer tank (17) is connected with a first raw material liquid inlet (34) at the upper part in the first rectifying tower through the raw material liquid pump (18), a liquid phase outlet (41) at the bottom of the first rectifying tower is connected with a first raw material liquid inlet (42) of the second rectifying tower, and a top gas phase outlet of the second rectifying tower (24) is sequentially connected with the product tank (27) through a first tube side inlet (43) of the second heat exchanger, a first tube side outlet (44) of the second heat exchanger, a first tee joint (13) and the product pump (26).
3. The production method of the device for producing high-purity boron trichloride according to claim 2, wherein: the gas phase outlet at the top of the first rectifying tower (19) is connected with the inlet of the first gas-liquid separator (21) through a first tube side inlet (35) of the first heat exchanger and a first tube side outlet (36) of the first heat exchanger, the liquid phase outlet of the first gas-liquid separator (21) is connected with a second raw material liquid inlet (37) at the upper middle part of the first rectifying tower, and the gas phase outlet of the first gas-liquid separator (21) is connected with the adsorption tower (31) through a fifth regulating valve (5) and a second tee joint (16).
4. The production method of the device for producing high-purity boron trichloride according to claim 2, wherein: the liquid phase outlet (48) at the bottom of the second rectifying tower is connected with the adsorption tower (31) through a sixth regulating valve (6) and a third end of the second tee joint (16).
5. The production method of the device for producing high-purity boron trichloride according to claim 2, wherein: the third end of the first tee joint (13) is connected with a second raw material liquid inlet (45) of the second rectifying tower.
6. The production method of the device for producing high-purity boron trichloride according to claim 2, wherein: the liquid ammonia outlet of the liquid ammonia storage tank (29) is respectively connected with a second tube side inlet (39) of the first heat exchanger and a second tube side inlet (47) of the second heat exchanger through a third tee joint (33), a second tube side outlet (46) of the first heat exchanger and a second tube side outlet (40) of the second heat exchanger are respectively connected with a fourth tee joint (15), and a third end of the fourth tee joint (15) is connected with an air conditioner working condition ice machine (30);
A ninth regulating valve (9) is arranged between the third tee joint (33) and the second tube side inlet (39) of the first heat exchanger, a tenth regulating valve (10) is arranged between the third tee joint (33) and the second tube side inlet (47) of the second heat exchanger, and an eleventh regulating valve (11) is arranged between the third end of the fourth tee joint (15) and the air conditioner ice machine (30).
7. The production method of the device for producing high-purity boron trichloride according to claim 2, wherein: the water outlet of the circulating water return tank (32) is respectively connected with a first reboiler (20) at the bottom of the first rectifying tower (19) and a second reboiler (25) at the bottom of the second rectifying tower (24) through a fifth tee joint (12), and the outlets of the first reboiler (20) and the second reboiler (25) are respectively connected with a circulating water feeding tank (28) through a sixth tee joint (14);
a seventh regulating valve (7) is arranged between the fifth tee joint (12) and the first reboiler (20), and an eighth regulating valve (8) is arranged between the fifth tee joint (12) and the second reboiler (25).
8. The production method of the device for producing high-purity boron trichloride according to claim 2, wherein: install first governing valve (1) between feed liquor buffer tank (17) and feed liquor pump (18), be equipped with second governing valve (2) between liquid phase export (41) of first rectifying column bottom and first feed liquor import (42) of second rectifying column, be equipped with third governing valve (3) between first tee bend (13) and product pump (26), be equipped with fourth governing valve (4) between product pump (26) and product tank (27).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910221456.3A CN110065951B (en) | 2019-03-20 | 2019-03-20 | Device and method for producing high-purity boron trichloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910221456.3A CN110065951B (en) | 2019-03-20 | 2019-03-20 | Device and method for producing high-purity boron trichloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110065951A CN110065951A (en) | 2019-07-30 |
| CN110065951B true CN110065951B (en) | 2023-05-12 |
Family
ID=67366488
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910221456.3A Active CN110065951B (en) | 2019-03-20 | 2019-03-20 | Device and method for producing high-purity boron trichloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110065951B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115072733A (en) * | 2022-07-27 | 2022-09-20 | 安徽艾佩科电子材料有限公司 | Purification method of high-purity boron trichloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661654A (en) * | 2012-05-02 | 2012-09-12 | 北京华宇同方化工科技开发有限公司 | Method and system for preparing high purity gas by rectification method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB875899A (en) * | 1959-04-24 | 1961-08-23 | Dow Chemical Co | Recovery and purification of boron trichloride |
| CN105731379A (en) * | 2015-12-31 | 2016-07-06 | 上海正帆科技股份有限公司 | Purifying method of electronic grade chlorine |
-
2019
- 2019-03-20 CN CN201910221456.3A patent/CN110065951B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661654A (en) * | 2012-05-02 | 2012-09-12 | 北京华宇同方化工科技开发有限公司 | Method and system for preparing high purity gas by rectification method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110065951A (en) | 2019-07-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104817110B (en) | A kind of zircon sand fluidizing chlorination method produces high-purity zirconium oxychloride and the method for coproduction Silicon chloride. | |
| CN101791487B (en) | Method for recycling hydrogen chloride in tail gas of polysilicon production | |
| CN101538044B (en) | System for separating and purifying trichlorosilane in production process of polysilicon and operation method thereof | |
| CN101254921B (en) | Method for preparing trichlorosilane and polycrystalline silicon by transforming silicon tetrachloride | |
| CN102874814B (en) | Polycrystalline-silicon reducing and producing process and device | |
| CN109867262B (en) | Synthesis system and synthesis method of diborane | |
| CN104437295A (en) | Device and method for preparing tetramethoxysilane | |
| CN104725191A (en) | Ethylene glycol refining and separating method and system | |
| CN204434297U (en) | Prepare the system of trichlorosilane | |
| CN113120862A (en) | Method for continuously producing high-purity diborane | |
| CN110065951B (en) | Device and method for producing high-purity boron trichloride | |
| CN217313451U (en) | Tower type continuous preparation device for bis (fluorosulfonyl) imide | |
| CN101531367B (en) | Process for producing silicane | |
| CN110240165B (en) | Method and device for recovering dichlorosilane from polycrystalline silicon reduction tail gas | |
| CN113772625A (en) | High-efficiency hydrogen production process by using methanol | |
| CN109867263B (en) | Two-section type tubular continuous reaction system for diborane synthesis and diborane synthesis method | |
| CN210103472U (en) | Device for producing high-purity boron trichloride | |
| CN202072477U (en) | Polycrystalline silicon production system | |
| CN209778297U (en) | synthesis system of diborane | |
| CN204380655U (en) | Prepare the device of tetramethoxy-silicane | |
| CN215439670U (en) | Reduction circulation hydrogen cryogenic impurity removal device for producing high-quality polycrystalline silicon | |
| CN104163761A (en) | Method for refining dimethyl succinate by rectification | |
| CN210332179U (en) | System for obtaining by-product hydrogen by pressure swing adsorption method in ethylene preparation process | |
| CN105036137B (en) | Method for preparing silane by disproportionation of dichlorosilane as raw material | |
| CN102092720B (en) | Continuous preparation device for high-purity silane gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |