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Electronic-grade chlorine trifluoride rectification purification system control method

A chlorine trifluoride, electronic-grade technology is applied in the control field of the rectification and purification system of electronic-grade chlorine trifluoride, which can solve the problems of not using an efficient extraction agent, application, and inability to meet actual needs, and improve the reflux ratio. The effect of parameter stability

Active Publication Date: 2021-06-08
FUJIAN DEER TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this prior art has a low boiling tower and a high boiling tower, this technical solution is not a rectification device for preparing electronic-grade chlorine trifluoride, nor does it elaborate on the specific structure of the high and low boiling towers and whether an extractant is used (It is clearly recorded in the background technology of this prior art description: there are the following defects: (1) adopt the method of chemical removal of impurities
Make the purified solvent difficult to recycle and reuse
(2) Methylal will be generated in the methanol circulating in the process due to the presence of the extractant, which will lead to catalyst poisoning and rectification process with huge energy consumption and very little recycling and serious waste), thus failing to improve the reflux of the vapor-liquid phase equilibrium system Effects such as stability of ratio parameters
[0006] 中国专利申请或专利:CN104262082 A、CN105481640 A、CN109651067 A、CN109651110 A、CN110240536 A、CN211050938U、CN202270376U、CN203355329U、CN209537349U、CN209575807U、CN209940867U、CN209940868U等现有技术,虽然上述现有技术,其领域与本发明 Similar, but, those skilled in the art believe that through practice research, above-mentioned prior art can not reach the effect of reflux ratio parameter stability of vapor-liquid (chlorine trifluoride-hydrogen fluoride) phase equilibrium system, and then can not realize under various working conditions Wide dynamic balance operation; not to mention the purification of electronic grade chlorine trifluoride
[0007] Another example, Chinese patent application, such as: application number: CN2015108752487, publication number: CN105367410 A discloses a kind of hydrogenation refining system for producing chloroacetic acid, application number: CN2018114865024, publication number: CN109293529 A, discloses a kind of production hexachlorobenzene not Purification device and method for chlorothalonil exceeding 10 ppm, application number: CN201910990199x, publication number: CN110590604 A, discloses a continuous rectification and purification device for isophthalonitrile, application number: CN2018220464337, announcement number: CN209352805U discloses a production The purification device of chlorothalonil with hexachlorobenzene not exceeding 10ppm, although the above-mentioned prior art is a purification device or method applied to a certain compound, the above-mentioned disclosed technical scheme is designed for a certain compound. The technical means are relatively complicated, and those skilled in the art cannot apply their technical solutions to the rectification and purification system and method for producing electronic-grade chlorine trifluoride according to actual needs. That is to say, the above-mentioned prior art will not have any technical inspiration Applied to rectification purification system and method for preparing electronic grade chlorine trifluoride
[0008] In addition, Chinese patent applications: CN101979364 A discloses a preparation method of 2,3,3,3-tetrafluoropropene, CN105111351 A discloses a preparation method of a special fluoroether surfactant, and CN105111352 A discloses a special fluoroether low The preparation method of the polymer, although the preparation method of the above-mentioned prior art compound adopts fluoroether oil, but those skilled in the art cannot refer to the above content to give the technical enlightenment of applying it to the rectification device of electronic grade chlorine trifluoride
[0009] As another example, the prior art: CN101914001 A, CN102633597 A, CN102701941 A, CN103739454A, CN107382682 A, CN108103585 A, CN109096033 A, CN109678668 A, CN111217676 A, CN202610130U, etc. Although the extraction techniques such as distillation tower and other methods are used to prepare Or extraction compound method, but, above-mentioned prior art all does not adopt high-efficiency extraction agent, also does not adopt high-efficiency rectifying device, thinks through the experiment of those skilled in the art, analysis: above-mentioned common knowledge can not be realized by the tray temperature control method It can effectively improve the stability of the reflux ratio parameter of the vapor-liquid (chlorine trifluoride-hydrogen fluoride) phase equilibrium system to achieve wide dynamic equilibrium operation under various working conditions; through deep rectification technology, chlorine trifluoride and various impurity components can be realized Effective separation, the purpose of purifying electronic grade chlorine trifluoride

Method used

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Effect test

Embodiment 1

[0042] A rectification device for electronic grade chlorine trifluoride, comprising: a two-stage low-temperature rectification device, the two-stage low-temperature rectification device includes a low-boiling tower and a high-boiling tower, and the two-stage low-temperature rectification device is equipped with An extractant that associates molecules of discrete hydrogen fluoride and chlorine trifluoride to meet electronic grade chlorine trifluoride requirements. The low boiling column includes a first reboiler, a first low boiling column packing section, a second low boiling column packing section and a first condenser from bottom to top. The high boiling column includes a second reboiler, a first high boiling column packing section, a second high boiling column packing section, a third high boiling column packing section and a second condenser from bottom to top. An extraction agent is provided in each packing section for further separating the associated molecules of hydrog...

Embodiment 2

[0045] The present invention further provides the rectification method of the rectification device of above-mentioned electronic grade chlorine trifluoride, this rectification device comprises the technical feature in embodiment 1, and this method comprises the following steps:

[0046] S1, controlling the temperature of the second tray at the upper end of the first reboiler to be 10-12°C, and controlling the temperature of the second tray at the lower end of the first condenser to be -22.5-24°C;

[0047] S2, controlling the temperature at the upper end of the second reboiler to be 11-12°C, and controlling the temperature at the lower end of the second condenser to be -6--4°C.

Embodiment 3

[0049] refer to figure 1 As shown, the present invention provides a purification system for electronic grade chlorine trifluoride, comprising: a sequentially connected first Hastelloy condenser 11, a first Hastelloy heating tank 12, and a Hastelloy pressure heating tank 13. Three-stage metal adsorbent layer bed 14 , rectification device for electronic grade chlorine trifluoride in Example 1, liquefaction tank 16 and pressure stabilizing tank 17 .

[0050] The feed end of the first Hastelloy condenser 11 is arranged at its top and communicates with the reactor 10, and the discharge end of the first Hastelloy condenser 11 is arranged at its bottom and connected with the first Hastelloy condenser 11. The feed end of a Hastelloy heating tank body 12 is connected. The first Hastelloy condenser 11 is used to condense the crude chlorine trifluoride produced by the reactor 10, so as to provide power to the outlet gas of the reactor 10 through temperature difference (generating negati...

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Abstract

The invention provides an electronic-grade chlorine trifluoride rectification purification system control method and an electronic-grade chlorine trifluoride rectification device. The electronic-grade chlorine trifluoride rectification device comprises a secondary low-temperature rectification device which comprises a low-boiling tower and a high-boiling tower, and the econdary low-temperature rectification device comprises anextraction agent which is used for further dispersing hydrogen fluoride and chlorine trifluoride associated molecules, so that the requirements of electronic-grade chlorine trifluoride are met; the stability of reflux ratio parameters of a vapor-liquid (chlorine trifluoride-hydrogen fluoride) phase equilibrium system can be effectively improved through a tower plate temperature control method, and wide dynamic equilibrium operation under various working conditions is realized; according to the tower plate temperature control method, effective separation of chlorine trifluoride and various impurity components can be realized through a deep rectification technology, and electronic-grade chlorine trifluoride is purified.

Description

technical field [0001] The invention relates to a control method for a rectification purification system of electronic grade chlorine trifluoride. Background technique [0002] At present, chlorine trifluoride has the special properties that its boiling point is close to that of hydrogen fluoride and that it is easy to form polymers between molecules and its impurity system. The concentration of hydrogen fluoride impurities is controlled below 500ppmv, and it is difficult to purify electronic grade chlorine trifluoride. [0003] Prior art, such as Chinese patent application (application number: CN2019112490911, publication number: CN110975315A) discloses an energy-saving rectification and purification system for high-purity propylene oxide. The middle part of the high-boiling tower is equipped with a crude propylene oxide inlet. The steam outlet at the top is connected to the first compressor and the first heat exchanger in turn, the first heat exchanger is connected to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/24B01D3/14B01D3/32B01D3/42
CPCC01B7/24B01D3/143B01D3/324B01D3/322B01D3/42Y02P20/10Y02P20/50C07C17/389C07C17/386C07C19/10
Inventor 李向如李嘉磊陈施华申黎明于睿洁吴强
Owner FUJIAN DEER TECH CORP
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