CN101423194A - Dewatering process of fluorine hydride - Google Patents
Dewatering process of fluorine hydride Download PDFInfo
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- CN101423194A CN101423194A CNA2008101945544A CN200810194554A CN101423194A CN 101423194 A CN101423194 A CN 101423194A CN A2008101945544 A CNA2008101945544 A CN A2008101945544A CN 200810194554 A CN200810194554 A CN 200810194554A CN 101423194 A CN101423194 A CN 101423194A
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- Prior art keywords
- dewatering
- dewatering agent
- hydrogen fluoride
- hydrofluoric
- fluoride
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Abstract
The invention discloses a dehydration method used for hydrogen fluoride. Metal fluoride which can react with water is used as a dehydrating agent so as to lead the hydrogen fluoride to contact with the dehydrating agent and convert the water in the hydrogen fluoride into vapor-phase fluoride which is discharged into the air, thus finally gaining the hydrogen fluoride meeting the requirement. The method has the advantages that the water content of disposed hydrogen fluoride is less than 10ppm; the fluoride after reaction can be circularly used by regeneration, the method improves the utilization ratio and reduces the disposal expense.
Description
Technical field
The present invention relates to hydrofluoric dewatering.
Background technology
Hydrogen fluoride is used industrial widely because of the physics and the chemical property of uniqueness, as the etching, the organic fluorine that are applied to large-scale integrated circuit in glass etching, the semi-conductor industry are combined to medium of reagent, non-aqueous solvent method chemosynthesis etc.Hydrogen fluoride usually influences its application because of containing various impurity, therefore need carry out suitable processing.Utilizing element fluorine is a kind of highly effective method for reducing various redox impurity and moisture content, but directly use element fluorine often to be difficult to control because of its intensive chemically reactive, thereby equipment has been proposed very high requirement, made cost increase, it is complicated that operation becomes.Under some situation, need the content of moisture in the strict control anhydrous hydrogen fluoride, as reaction medium, moisture content has directly influenced the quality of product as anhydrous hydrogen fluoride in some building-up reactionss, thereby is necessary existing technology is done further research.
Summary of the invention
The purpose of this invention is to provide and a kind ofly make water content in the hydrogen fluoride less than the hydrofluoric dewatering of 10ppm.
For achieving the above object, the technical solution used in the present invention is:
Utilization can with the metal fluoride of water reaction as dewatering agent, hydrogen fluoride is contacted with dewatering agent, be the vapor-phase fluoride emptying with the water transform in the hydrogen fluoride, finally obtain the hydrogen fluoride that suits the requirements;
Described dewatering agent is at least a in the following material:
M
xNiF
y(M＝Li、Na、K、Ru、Cs，x＝2～3，y＝5～7)、MPbF
6(M＝Li、Na、K、Ru、Cs)、XeF
a(a＝2、4、6)、KrF
b(b＝2、4、6)、MMnF
6(M＝Li、Na、K、Ru、Cs)、CoF
3、MnF
c(c＝3、4)、CeF
4、TiF
4、MoF
6、WF
6；
Described dewatering agent is a particulate state or Powdered;
Described dewatering agent the best is a particulate state, and its particle size range is 10～100 orders;
Described hydrogen fluoride contacts with the dewatering agent circulation under the recycle pump effect;
Also comprise the dewatering agent step for regeneration in the described dewatering, that is: after dewatering agent uses for some time to lose dehydration activity, utilize fluorine gas as regenerator, the feeding fluorine gas recovers dehydration activity until dewatering agent in the dewatering agent;
Described hydrofluoric dewatering is characterized in that: when carrying out step for regeneration dewatering agent is heated to 200～320 ℃.
The invention has the beneficial effects as follows:
1, treated hydrogen fluoride water content can be lower than 10ppm.
2, reacted dewatering agent can be recycled by regeneration, has improved utilization ratio, has reduced processing costs.
Description of drawings
Fig. 1 is the dewatering unit that method of the present invention adopted
1, vacuum pumping valve; 2, dewatering agent container; 3, connect the fluorine gas valve; 4 hydrogen fluoride containers; 5, recycle pump, 6, analyser; 7, recycle valve.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described, but the present invention should not only limit to these embodiment.
Embodiment 1:
As shown in Figure 1; at first under nitrogen protection; in dewatering agent container 2, insert 20～30 purpose solid cobaltic fluoride particles; in hydrogen fluoride container 4, add 50 liters of hydrogen fluoride that water content is 100ppm; open recycle valve 7 and vacuum pumping valve 1 then; start recycle pump 5; the pressure of Controlling System is lower than safe design pressure; hydrogen fluoride liquid is mobile linear velocity 0.5 meter per second in dewatering agent container 2; the vapor-phase fluoride that generates in this process is discharged through vacuum pumping valve 1; sampling and measuring water content 50ppm after 3 hours; 5 hours; 10 hours; sampling detection respectively after 15 hours; water content is respectively 42ppm; 12ppm; 5ppm takes a sample to check and can be undertaken by analyser 6.
Employed dewatering agent CoF in the present embodiment
3After operation for some time, dewatering agent can lose reactive behavior, need activating and regenerating to handle, its operation is as follows: open connect fluorine gas valve 3 and vacuum pumping valve 1 and vacuumize after, open the internal heating annex, dewatering agent is heated, 300 ℃ of Heating temperatures of control feed the fluorine gas of 0.2MPa, the changing conditions of observation pressure then in the dewatering agent container 2, after no longer reducing to pressure, stop to feed fluorine gas, close the internal heating annex, naturally cool to room temperature, extract remaining regeneration gas out, finish the regeneration of dewatering agent.
Embodiment 2:
As shown in Figure 1, at first under nitrogen protection, in dewatering agent container 2, insert 20～30 order solid manganese tetrafluoride (MnF
4) particle, in hydrogen fluoride container 4, add 35 liters of hydrogen fluoride that water content is 150ppm, open recycle valve 7 then, start recycle pump 5, the pressure of Controlling System is lower than safe design pressure, hydrogen fluoride liquid is mobile linear velocity 0.5 meter per second in dewatering agent container 2, the vapor-phase fluoride that generates in this process is discharged through vacuum pumping valve 1, sampling and measuring water content 80ppm after 3 hours, 5.5 hour, after 8 hours, 15 hours respectively sampling detect, water content is respectively 45ppm, 15ppm, 7.5ppm, and sampling detects and can be undertaken by analyser 6.
Claims (7)
1, hydrofluoric dewatering is characterized in that: utilization can with the metal fluoride of water reaction as dewatering agent, hydrogen fluoride is contacted with dewatering agent, be the vapor-phase fluoride emptying with the water transform in the hydrogen fluoride, finally obtain the hydrogen fluoride that suits the requirements.
2, hydrofluoric dewatering according to claim 1 is characterized in that: described dewatering agent is at least a in the following material:
M
xNiF
y(M＝Li、Na、K、Ru、Cs，x＝2～3，y＝5～7)、MPbF
6(M＝Li、Na、K、Ru、Cs)、XeF
a(a＝2、4、6)、KrF
b(b＝2、4、6)、MMnF
6(M＝Li、Na、K、Ru、Cs)、CoF
3、MnF
c(c＝3、4)、CeF
4、TiF
4、MoF
6、WF
6。
3, as hydrofluoric dewatering as described in claims 1 or 2, it is characterized in that: described dewatering agent is a particulate state or Powdered.
4, state hydrofluoric dewatering as claims 1 or 2, it is characterized in that: described dewatering agent is a particulate state, and its particle size range is 10～100 orders.
5, state hydrofluoric dewatering as claims 1 or 2, it is characterized in that: described hydrogen fluoride contacts with the dewatering agent circulation under the recycle pump effect.
6, hydrofluoric dewatering according to claim 1 and 2, it is characterized in that: also comprise the dewatering agent step for regeneration in the described dewatering, that is: after dewatering agent uses for some time to lose dehydration activity, utilize fluorine gas as regenerator, feed fluorine gas in the dewatering agent and recover dehydration activity until dewatering agent.
7, hydrofluoric dewatering according to claim 6 is characterized in that: when carrying out step for regeneration dewatering agent is heated to 200～320 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101945544A CN101423194A (en) | 2008-11-17 | 2008-11-17 | Dewatering process of fluorine hydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101945544A CN101423194A (en) | 2008-11-17 | 2008-11-17 | Dewatering process of fluorine hydride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101423194A true CN101423194A (en) | 2009-05-06 |
Family
ID=40614107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101945544A Pending CN101423194A (en) | 2008-11-17 | 2008-11-17 | Dewatering process of fluorine hydride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101423194A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111387A (en) * | 2019-12-25 | 2020-05-08 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for removing water in hydrogen fluoride steel cylinder |
-
2008
- 2008-11-17 CN CNA2008101945544A patent/CN101423194A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111387A (en) * | 2019-12-25 | 2020-05-08 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for removing water in hydrogen fluoride steel cylinder |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090506 |