CN104030249A - Method for purifying hydrogen fluoride - Google Patents
Method for purifying hydrogen fluoride Download PDFInfo
- Publication number
- CN104030249A CN104030249A CN201410297681.2A CN201410297681A CN104030249A CN 104030249 A CN104030249 A CN 104030249A CN 201410297681 A CN201410297681 A CN 201410297681A CN 104030249 A CN104030249 A CN 104030249A
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- China
- Prior art keywords
- hydrogen fluoride
- reaction mixture
- fluoride
- crude product
- mentioned reaction
- 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.)
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910000040 hydrogen fluoride Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title abstract description 10
- 239000011541 reaction mixture Substances 0.000 claims abstract description 32
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 12
- KWVVTSALYXIJSS-UHFFFAOYSA-L silver(ii) fluoride Chemical compound [F-].[F-].[Ag+2] KWVVTSALYXIJSS-UHFFFAOYSA-L 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 6
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 6
- 239000012043 crude product Substances 0.000 claims description 12
- 239000003929 acidic solution Substances 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 6
- 229910021610 Silver(III) fluoride Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 abstract description 9
- 229910052785 arsenic Inorganic materials 0.000 abstract description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 150000003018 phosphorus compounds Chemical class 0.000 abstract 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- -1 phosphorus compound Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for purifying hydrogen fluoride, and belongs to the technical field of chemical product preparation. The method comprises the following steps: firstly, reacting a crude hydrogen fluoride product with a silver difluoride liquid, subsequently adding sodium fluoride for reaction, distilling an obtained reaction mixture, introducing a hydrogen fluoride gas obtained through distillation into an acid solution for reaction, and finally further distilling the obtained reaction mixture, thereby preparing hydrogen fluoride. Due to adoption of the method, impurities, particularly phosphorus compounds and arsenic impurities, in the crude hydrogen fluoride product can be effectively removed, and the purity of hydrogen fluoride can be greater than 99%.
Description
Technical field
The invention belongs to chemical preparing technical field, be specifically related to a kind of hydrofluoric purification process.
Background technology
Hydrogen fluoride be generally the fluorite ore deposit of containing bifluoride calcium be that raw material is prepared from, the hydrogen fluoride crude product that it makes contains plurality of impurities, for example, contain the phosphorus compound existing with various forms, the impurity such as silicon-dioxide, calcium carbonate and arsenic.And the existence of these impurity not only can make hydrofluoric performance be affected, even also can work the mischief.
Wherein, if contain arsenic impurities in hydrogen fluoride, can make utilizing hydrogen fluoride catalyzer produce to be poisoned in preparing the process of cfc, if simultaneously by this hydrogen fluoride for the preparation of semi-conductor, the arsenic wherein containing can be diffused in semiconductor element, thereby has influence on the work of element.
Therefore, conventionally the hydrogen fluoride making further can be purified, remove as much as possible the impurity wherein containing.
Summary of the invention
The invention provides a kind of hydrofluoric purification process, the method can effectively be removed the impurity containing in hydrogen fluoride crude product, particularly phosphorus compound and arsenic impurities.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
A hydrofluoric purification process, the method comprises the following steps:
A, the hydrogen fluoride crude product making is put into reactor, then add 1～2 times of Argentic fluoride liquid of hydrogen fluoride crude product quality, and be heated to 40 ℃～55 ℃ and carry out isothermal reaction 20min～30min, obtain reaction mixture I;
B, to the Sodium Fluoride that adds 0.5～0.8 times of reaction mixture I quality in above-mentioned reaction mixture I, at 40 ℃～55 ℃, continue constant temperature stirring reaction 10min～15min, obtain reaction mixture II;
C, above-mentioned reaction mixture II is distilled, and the flow of hydrogen fluoride that distillation is obtained passes in acidic solution, make; The solution that the ratio that it is 2～3:1 in mass ratio that wherein said acidic solution refers to by hydrogen fluoride and water makes;
D, last, distills above-mentioned reaction mixture III again, makes.
Embodiment
Below in conjunction with specific examples, the invention will be further described:
Embodiment 1
A hydrofluoric purification process, the method comprises the following steps:
A, the hydrogen fluoride crude product making is put into reactor, then add 1 times of Argentic fluoride liquid of hydrogen fluoride crude product quality, and be heated to 55 ℃ and carry out isothermal reaction 20min, obtain reaction mixture I;
B, to the Sodium Fluoride that adds 0.5 times of reaction mixture I quality in above-mentioned reaction mixture I, at 55 ℃, continue constant temperature stirring reaction 10min, obtain reaction mixture II;
C, above-mentioned reaction mixture II is distilled, and the flow of hydrogen fluoride that distillation is obtained passes in acidic solution, make; Wherein said acidic solution refers to the solution being made for the ratio of 2:1 in mass ratio by hydrogen fluoride and water;
D, last, distills above-mentioned reaction mixture III again, makes.
The hydrogen fluoride purity obtaining after the purified processing of the present embodiment is 99.1%.
Embodiment 2
A hydrofluoric purification process, the method comprises the following steps:
A, the hydrogen fluoride crude product making is put into reactor, then add 2 times of Argentic fluoride liquid of hydrogen fluoride crude product quality, and be heated to 40 ℃ and carry out isothermal reaction 30min, obtain reaction mixture I;
B, to the Sodium Fluoride that adds 0.8 times of reaction mixture I quality in above-mentioned reaction mixture I, at 40 ℃, continue constant temperature stirring reaction 15min, obtain reaction mixture II;
C, above-mentioned reaction mixture II is distilled, and the flow of hydrogen fluoride that distillation is obtained passes in acidic solution, make; Wherein said acidic solution refers to the solution being made for the ratio of 3:1 in mass ratio by hydrogen fluoride and water;
D, last, distills above-mentioned reaction mixture III again, makes.
The hydrogen fluoride purity obtaining after the purified processing of the present embodiment is 99.6%.
Embodiment 3
A hydrofluoric purification process, the method comprises the following steps:
A, the hydrogen fluoride crude product making is put into reactor, then add 1.5 times of Argentic fluoride liquid of hydrogen fluoride crude product quality, and be heated to 50 ℃ and carry out isothermal reaction 25min, obtain reaction mixture I;
B, to the Sodium Fluoride that adds 0.6 times of reaction mixture I quality in above-mentioned reaction mixture I, at 50 ℃, continue constant temperature stirring reaction 12min, obtain reaction mixture II;
C, above-mentioned reaction mixture II is distilled, and the flow of hydrogen fluoride that distillation is obtained passes in acidic solution, make; Wherein said acidic solution refers to the solution being made for the ratio of 2.5:1 in mass ratio by hydrogen fluoride and water;
D, last, distills above-mentioned reaction mixture III again, makes.
The hydrogen fluoride purity obtaining after the purified processing of the present embodiment is 99.5%.
Claims (1)
1. a hydrofluoric purification process, is characterized in that comprising the following steps:
A, the hydrogen fluoride crude product making is put into reactor, then add 1～2 times of Argentic fluoride liquid of hydrogen fluoride crude product quality, and be heated to 40 ℃～55 ℃ and carry out isothermal reaction 20min～30min, obtain reaction mixture I;
B, to the Sodium Fluoride that adds 0.5～0.8 times of reaction mixture I quality in above-mentioned reaction mixture I, at 40 ℃～55 ℃, continue constant temperature stirring reaction 10min～15min, obtain reaction mixture II;
C, above-mentioned reaction mixture II is distilled, and the flow of hydrogen fluoride that distillation is obtained passes in acidic solution, make; The solution that the ratio that it is 2～3:1 in mass ratio that wherein said acidic solution refers to by hydrogen fluoride and water makes;
D, last, distills above-mentioned reaction mixture III again, makes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410297681.2A CN104030249B (en) | 2014-06-29 | 2014-06-29 | Hydrofluoric purification process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410297681.2A CN104030249B (en) | 2014-06-29 | 2014-06-29 | Hydrofluoric purification process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104030249A true CN104030249A (en) | 2014-09-10 |
| CN104030249B CN104030249B (en) | 2016-03-30 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410297681.2A Active CN104030249B (en) | 2014-06-29 | 2014-06-29 | Hydrofluoric purification process |
Country Status (1)
| Country | Link |
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| CN (1) | CN104030249B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4668497A (en) * | 1984-12-25 | 1987-05-26 | Hashimoto Chemical Industries Co., Ltd. | Process for purifying hydrogen fluoride |
| US5411726A (en) * | 1993-02-10 | 1995-05-02 | Bayer Ag | Process for purifying hydrogen fluoride |
| CN102232060A (en) * | 2008-11-28 | 2011-11-02 | 国立大学法人京都大学 | Hydrogen fluoride purification method |
-
2014
- 2014-06-29 CN CN201410297681.2A patent/CN104030249B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4668497A (en) * | 1984-12-25 | 1987-05-26 | Hashimoto Chemical Industries Co., Ltd. | Process for purifying hydrogen fluoride |
| US5411726A (en) * | 1993-02-10 | 1995-05-02 | Bayer Ag | Process for purifying hydrogen fluoride |
| CN102232060A (en) * | 2008-11-28 | 2011-11-02 | 国立大学法人京都大学 | Hydrogen fluoride purification method |
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| Publication number | Publication date |
|---|---|
| CN104030249B (en) | 2016-03-30 |
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Address after: 547500 the old Finance Bureau of Bama Yao Autonomous County, Hechi County, the Guangxi Zhuang Autonomous Region Patentee after: Chen Kun Address before: The Guangxi Zhuang Autonomous Region Luzhai County Road 545600 Liuzhou city built in 25 Patentee before: Chen Kun |
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Effective date of registration: 20191121 Address after: Tri village Pingquan 067500 Chengde province Hebei city Pingquan County town Patentee after: CHENGDE YINGKE FINE CHEMICAL CO.,LTD. Address before: 547500 the old Finance Bureau of Bama Yao Autonomous County, Hechi County, the Guangxi Zhuang Autonomous Region Patentee before: Chen Kun |
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Address after: 067500 dongsanjia village, Pingquan Town, Pingquan City, Chengde City, Hebei Province Patentee after: Chengde Yingke Fine Chemical Co.,Ltd. Address before: 067500 dongsanjia village, Pingquan Town, Pingquan County, Chengde City, Hebei Province Patentee before: CHENGDE YINGKE FINE CHEMICAL CO.,LTD. |