CN210764357U

CN210764357U - Purification device of boron trichloride

Info

Publication number: CN210764357U
Application number: CN201920706222.3U
Authority: CN
Inventors: 赵毅; 赵趫; 王天源; 裴凯; 赵银凤; 计燕秋; 张琳
Original assignee: Dalian Kelide Optoelectronic Mat Co ltd
Current assignee: Dalian Kelide Optoelectronic Mat Co ltd
Priority date: 2019-05-16
Filing date: 2019-05-16
Publication date: 2020-06-16
Anticipated expiration: 2029-05-16

Abstract

The utility model provides a purification device of boron trichloride. The method is characterized in that: the low-purity boron trichloride raw material is vaporized by a raw material reboiler, continuously passes through a first-stage adsorption bed, a second-stage adsorption bed, a reaction bed and a filter, then is introduced into a rectifying tower from the bottom of the tower, flows into a buffer tank through a tower top condenser, and one part of the material in the buffer tank returns to the rectifying tower and the other part of the material is extracted to a product storage tank. Has the advantages of simple structure, safety, reliability and the like.

Description

Purification device of boron trichloride

Technical Field

The utility model relates to a chemical industry separation technology field, concretely relates to purification device of boron trichloride.

Background

The high-purity boron trichloride is mainly used in a Chemical Vapor Deposition (CVD) film forming process and a plasma dry etching process which have high technical requirements in an IC manufacturing process and greatly influence the yield of circuits, can bring a very critical effect on the quality of IC products, and other electronic gases cannot be replaced. At present, the purity of the electronic grade boron trichloride is required to be more than 99.999 percent. Because the impurity content and purity of the boron trichloride directly affect the quality, performance, technical index and yield of IC and electronic components, the requirement of the electronic grade boron trichloride on gas phase, metal and other impurities is extremely high.

In the practical application of electronic grade high-purity boron trichloride, the requirement on the purity of gas is very high, the purity of boron trichloride is generally required to be more than 99.999%, a rectifying tower is generally used for rectification and purification in the process, and impurities with high boiling point and low boiling point in boron trichloride are removed, but because boron trichloride belongs to low-temperature liquefied gas, the removal efficiency of impurities with low boiling point (such as oxygen and nitrogen) is not high only by a rectification method, and the method of adopting a high reflux ratio and a high theoretical plate is generally a well-known high-energy consumption process.

Meanwhile, in the production process of boron trichloride, chlorine is used for reaction, the chlorine has certain solubility in the boron trichloride, and the purification requirement is difficult to meet by rectification purification, and Japanese patent JP patent publication No. 2013 144644A discloses that a corrosion-resistant device filled with boron carbide is used for purifying phosgene and chlorine in the boron trichloride, so that the content of the chlorine in the boron trichloride can be less than 1ppm, but the method needs to be carried out at a high temperature of 500-720 ℃, and is also a high-energy consumption process.

Disclosure of Invention

The utility model aims at providing a can get rid of more than 90% low boiling impurity and chlorine impurity in the boron trichloride at lower temperature within range (20 ~ 70 ℃), reach the boron trichloride purity through the rectification and > 99.999% to reduce the high-purity boron trichloride purification device of energy consumption.

The utility model discloses purpose technical solution does: the utility model provides a purification device of boron trichloride, is formed by connecting raw materials reboiler, one-level adsorption bed, second grade adsorption bed, reaction bed, filter, rectifying column reboiler, condenser, buffer tank, product storage tank, its characterized in that: vaporizing a low-purity boron trichloride raw material by a raw material reboiler, continuously passing through a first-stage adsorption bed, a second-stage adsorption bed, a reaction bed and a filter, introducing into a rectifying tower from the bottom of the tower, flowing into a buffer tank through a tower top condenser, returning part of the material in the buffer tank to the rectifying tower, and extracting part of the material to a product storage tank;

the first-stage adsorption bed is filled with an adsorbent X1 modified by 10-25% nitric acid;

the second-stage adsorption bed has pore volume of 0.45-0.70mL/g and micropore surface area of 1000-²Coconut shell activated carbon per gram;

the reaction bed adopts metal titanium with the diameter of phi 2-8 mm and ceramic ring mixed packing with the diameter of phi 5, and the ratio is 3.5:1 (volume ratio).

Compared with the prior art, the utility model have following advantage: the process adopts the process of adsorption, filtration and rectification, and is modified in the structure of a rectifying tower, so that the purification filler is added, and the unit energy consumption is reduced. Meanwhile, the adsorbers can be activated and regenerated, and the reaction bed packing is replaced periodically, so that the production cost is greatly reduced, and the device is simple in structure, safe and reliable.

Drawings

FIG. 1 is a schematic view of the purification process of high purity boron trichloride.

In the figure: 1. the system comprises a raw material reboiler, 2, a first-stage adsorption bed, 3, a second-stage adsorption bed, 4, a reaction bed, 5, a filter, 6, a rectifying tower, 7, a rectifying tower reboiler, 8, a condenser, 9, a buffer tank, 10 and a product storage tank.

Detailed Description

The embodiments are described below with reference to the accompanying drawings:

example 1

Take the production scale equipment of 100T high-purity boron trichloride produced every year as an example. The production device comprises a raw material reboiler 1, a primary adsorption bed 2, a secondary adsorption bed 3, a reaction bed 4, a filter 5, a rectifying tower 6, a rectifying tower reboiler 7, a condenser 8, a buffer tank 9 and a product storage tank 10. Wherein, the temperature of the raw material reboiler 1 is set to 55 ℃, the gas velocity flowing through the first-stage adsorption bed 2, the second-stage adsorption bed 3 and the reaction bed 4 after the material is vaporized is 250L/min, the theoretical plate number of the rectifying tower 6 is 30, and the reflux ratio is 5. The boron trichloride purification effect is as follows:

high temperature (500-720 ℃) is not used for removing chlorine impurities, the theoretical plate number is low, the reboiler power is low, and the electricity charge (according to 0.8 yuan/Kwh) is saved by about 56 ten thousand yuan per year.

Example 2

Take the production scale equipment of annual 500T high-purity boron trichloride as an example. The production device comprises a raw material reboiler 1, a primary adsorption bed 2, a secondary adsorption bed 3, a reaction bed 4, a filter 5, a rectifying tower 6, a rectifying tower reboiler 7, a condenser 8, a buffer tank 9 and a product storage tank 10. Wherein, the temperature of the raw material reboiler 1 is set to be 70 ℃, the gas velocity flowing through the first-stage adsorption bed 2, the second-stage adsorption bed 3 and the reaction bed 4 after the material is vaporized is 350L/min, the theoretical plate number of the rectifying tower is 28, and the reflux ratio is 5. The boron trichloride purification effect is as follows:

high temperature (500-720 ℃) is not used for removing chlorine impurities, the theoretical plate number is low, the reboiler power is low, and the electricity charge (according to 0.8 yuan/Kwh) is saved by about 260 ten thousand yuan per year.

Claims

1. The utility model provides a purification device of boron trichloride, is formed by connecting raw materials reboiler (1), one-level adsorption bed (2), second grade adsorption bed (3), reaction bed (4), filter (5), rectifying column (6), rectifying column reboiler (7), condenser (8), buffer tank (9), product storage tank (10), its characterized in that: after being vaporized by a raw material reboiler (1), the low-purity boron trichloride continuously passes through a first-stage adsorption bed (2), a second-stage adsorption bed (3), a reaction bed (4) and a filter (5), then is introduced into a rectifying tower (6) from the bottom of the tower, flows into a buffer tank (9) through a tower top condenser (8), and a part of materials in the buffer tank (9) returns to the rectifying tower (6) and a part of materials are extracted to a product storage tank (10);

the secondary adsorption bed (3) has pore volume of 0.45-0.70mL/g and micropore surface area of 1000-²Coconut shell activated carbon per gram.