CN102249256A - Process for preparing boron trifluoride gas - Google Patents
Process for preparing boron trifluoride gas Download PDFInfo
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- CN102249256A CN102249256A CN2011101545172A CN201110154517A CN102249256A CN 102249256 A CN102249256 A CN 102249256A CN 2011101545172 A CN2011101545172 A CN 2011101545172A CN 201110154517 A CN201110154517 A CN 201110154517A CN 102249256 A CN102249256 A CN 102249256A
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Abstract
The invention relates to a process for preparing boron trifluoride gas. The process comprises the following steps of: a, mixing, and generating gas, namely mixing boric acid and 20 percent fuming sulphuric acid under normal pressure, mixing the mixed acid of boric acid and fuming sulphuric acid, and hydrogen fluoride gas in a reaction tower, contacting and reacting in the mass ratio of the mixed acid of boric acid and fuming sulphuric acid to the hydrogen fluoride gas of 9:(0.8-0.9) to generate fluoboric acid, and performing decomposition reaction of fluoboric acid at the presence of the fuming sulphuric acid at the temperature of between 80 and 120 DEG C to generate boron trifluoride gas; b, reacting in an absorption column, namely drying and purifying the boron trifluoride gas and byproduct sulfuric acid which are produced in the gas making process; and c, utilizing the byproduct sulfuric acid, namely adding sodium sulfate into a reaction kettle, adding the byproduct sulfuric acid, and reacting in the mass ratio of sodium sulfate to byproduct sulfuric acid of 1:(4-6), and reacting at normal temperature to generate sodium acid sulfate. The process has the advantages of low reaction temperature, high safety, no waste residue or waste gas, and environment-friendliness, and the waste liquor can be recycled.
Description
Technical field
The present invention relates to the preparation technology of boron triflouride gas, belong to chemical field.
Background technology
Produce at present boron trifluoride general adopt 20% oleum, boric anhydride, fluorite joined in the gas making reactor with the 9:1:3 mass ratio under 130 ° of conditions, react the production boron triflouride gas with hydrogen fluoride, the gas of producing complex reaction in above solvent gets product; The shortcoming of this reaction process is to adopt the fluorite powder to do raw material need carry out under higher temperature, can cause the waste of the energy, high temperature also can aggravate the corrosion and the damage of equipment, and workshop condition is relatively poor in process of production, can contain in the boron triflouride gas that a large amount of impurity has certain influence to the derived product quality and be batch production, the last production capacity power of project has certain restriction; Another technology is exactly to feed sulphur trioxide add boric acid in the vitriol oil after, feeds hydrogen fluoride generation boron triflouride gas and solvent complex at last and obtains product; It is exactly the sulphur trioxide of using severe toxicity that there is insufficient place in this reaction, and operational difficulty has the leakage meeting that environment is caused bigger pollution slightly, the higher not good utilisation of the spent acid sulfur trioxide content that is produced, contaminate environment.
Summary of the invention
The preparation technology who the purpose of this invention is to provide a kind of boron triflouride gas.
For achieving the above object, the technical solution used in the present invention is:
The preparation technology of boron triflouride gas may further comprise the steps:
A, mixing, gas making step:
Under normal pressure, with boric acid with after 20% oleum mixes, in reaction tower, carry out mixing and contacting reaction then with hydrogen fluoride gas, reaction is excessive for boric acid, and according to the quality of boric acid and oleum nitration mixture: the quality of hydrogen fluoride gas is 9:0.8-0.9, the generation fluoroboric acid, fluoroboric acid is in the presence of oleum, under 80-120 ° of conditions, decomposition reaction takes place, thereby generated boron triflouride gas;
B, absorption tower reactions steps:
Above-mentioned gas-making process come out boron triflouride gas and by-product sulfuric acid, boron triflouride gas is handled by dry decontamination;
C, by-product vitriolic utilize step:
Sodium sulfate is added reactor, and then add by-product sulfuric acid, sodium sulfate and by-product sulfuric acid are the 1:4-6 reaction according to mass ratio, and normal temperature reaction down generates sodium pyrosulfate, and controlled temperature 15-35 ° of sodium pyrosulfate crystallization promptly obtains sodium pyrosulfate through centrifugation.
Advantage of the present invention: temperature of reaction is low, safe; No waste residue, no waste gas is good to environment; The waste liquid recycle, the by-product sodium pyrosulfate has certain market economy; Continuity easy and simple to handle is strong, characteristics such as easy control.
Embodiment
Following examples are intended to illustrate the present invention rather than to the bright further qualification of we.
Embodiment 1
The preparation technology of boron triflouride gas may further comprise the steps:
A, mixing, gas making step:
Under normal pressure, with boric acid with after 20% oleum mixes, carry out mixing and contacting reaction with hydrogen fluoride gas then in reaction tower, react excessive for boric acid, the mass ratio of boric acid and oleum is 8:1, quality according to boric acid and oleum nitration mixture: the quality of hydrogen fluoride gas is 9:0.8, generate fluoroboric acid, fluoroboric acid is in the presence of oleum, under 80 ° of conditions, decomposition reaction takes place, thereby has generated boron triflouride gas;
B, absorption tower reactions steps:
Above-mentioned gas-making process come out boron triflouride gas and by-product sulfuric acid, boron triflouride gas is handled by dry decontamination;
C, by-product vitriolic utilize step:
Sodium sulfate is added reactor, and then add by-product sulfuric acid, sodium sulfate and by-product sulfuric acid are the 1:4 reaction according to mass ratio, and normal temperature reaction down generates sodium pyrosulfate, and 15 ° of sodium pyrosulfate crystallizations of controlled temperature promptly obtain sodium pyrosulfate through centrifugation.
Embodiment 2
The preparation technology of boron triflouride gas may further comprise the steps:
A, mixing, gas making step:
Under normal pressure, with boric acid with after 20% oleum mixes, carry out mixing and contacting reaction with hydrogen fluoride gas then in reaction tower, react excessive for boric acid, the mass ratio of boric acid and oleum is 7:2, quality according to boric acid and oleum nitration mixture: the quality of hydrogen fluoride gas is 9:0.85, generate fluoroboric acid, fluoroboric acid is in the presence of oleum, under 100 ° of conditions, decomposition reaction takes place, thereby has generated boron triflouride gas;
B, absorption tower reactions steps:
Above-mentioned gas-making process come out boron triflouride gas and by-product sulfuric acid, boron triflouride gas is handled by dry decontamination;
C, by-product vitriolic utilize step:
Sodium sulfate is added reactor, and then add by-product sulfuric acid, sodium sulfate and by-product sulfuric acid are the 1:5 reaction according to mass ratio, and normal temperature reaction down generates sodium pyrosulfate, and 25 ° of sodium pyrosulfate crystallizations of controlled temperature promptly obtain sodium pyrosulfate through centrifugation.
Embodiment 3
The preparation technology of boron triflouride gas may further comprise the steps:
A, mixing, gas making step:
Under normal pressure, with boric acid with after 20% oleum mixes, carry out mixing and contacting reaction with hydrogen fluoride gas then in reaction tower, react excessive for boric acid, the mass ratio of boric acid and oleum is 5:4, quality according to boric acid and oleum nitration mixture: the quality of hydrogen fluoride gas is 9:0.9, generate fluoroboric acid, fluoroboric acid is in the presence of oleum, under 120 ° of conditions, decomposition reaction takes place, thereby has generated boron triflouride gas;
B, absorption tower reactions steps:
Above-mentioned gas-making process come out boron triflouride gas and by-product sulfuric acid, boron triflouride gas is handled by dry decontamination;
C, by-product vitriolic utilize step:
Sodium sulfate is added reactor, and then add by-product sulfuric acid, sodium sulfate and by-product sulfuric acid are the 1:6 reaction according to mass ratio, and normal temperature reaction down generates sodium pyrosulfate, and 35 ° of sodium pyrosulfate crystallizations of controlled temperature promptly obtain sodium pyrosulfate through centrifugation.
Reaction is excessive for boric acid, and the mass ratio of boric acid and oleum is to be 6:3,
Advantage of the present invention: temperature of reaction is low, safe; No waste residue, no waste gas is good to environment; The waste liquid recycle, the by-product sodium pyrosulfate has certain market economy; Continuity easy and simple to handle is strong, characteristics such as easy control.
Claims (1)
1. the preparation technology of boron triflouride gas is characterized in that, may further comprise the steps:
A, mixing, gas making step:
Under normal pressure, with boric acid with after 20% oleum mixes, in reaction tower, carry out mixing and contacting reaction then with hydrogen fluoride gas, reaction is excessive for boric acid, and according to the quality of boric acid and oleum nitration mixture: the quality of hydrogen fluoride gas is 9:0.8-0.9, the generation fluoroboric acid, fluoroboric acid is in the presence of oleum, under 80-120 ° of conditions, decomposition reaction takes place, thereby generated boron triflouride gas;
B, absorption tower reactions steps:
Above-mentioned gas-making process come out boron triflouride gas and by-product sulfuric acid, boron triflouride gas is handled by dry decontamination;
C, by-product vitriolic utilize step:
Sodium sulfate is added reactor, and then add by-product sulfuric acid, sodium sulfate and by-product sulfuric acid are the 1:4-6 reaction according to mass ratio, and normal temperature reaction down generates sodium pyrosulfate, and controlled temperature 15-35 ° of sodium pyrosulfate crystallization promptly obtains sodium pyrosulfate through centrifugation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101545172A CN102249256A (en) | 2011-06-10 | 2011-06-10 | Process for preparing boron trifluoride gas |
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| CN2011101545172A CN102249256A (en) | 2011-06-10 | 2011-06-10 | Process for preparing boron trifluoride gas |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432030A (en) * | 2011-12-16 | 2012-05-02 | 天津市泰亨气体有限公司 | Preparation method of boron trifluoride |
| CN103360415A (en) * | 2013-07-16 | 2013-10-23 | 如皋市众昌化工有限公司 | Preparation method of boron trifluoride acetonitrile |
| CN105803480A (en) * | 2016-05-09 | 2016-07-27 | 上海应用技术学院 | Preparation method of boron trifluoride gas |
| CN106248520A (en) * | 2016-07-19 | 2016-12-21 | 苏州金宏气体股份有限公司 | A kind of detect the method and device of hydrogen fluoride content in boron trifluoride unstripped gas |
| CN112850731A (en) * | 2021-02-01 | 2021-05-28 | 山东合益气体股份有限公司 | Method and device for recovering boron trifluoride from wastewater containing boron trifluoride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1188758A (en) * | 1967-09-08 | 1970-04-22 | U S S Agri Chemicals Inc | Manufacture of Boron Trifluoride. |
| US3690821A (en) * | 1971-03-23 | 1972-09-12 | United States Steel Corp | Manufacture of boron trifluoride |
| CN1231214A (en) * | 1997-12-08 | 1999-10-13 | 埃勒夫阿托化学有限公司 | Preparation of boron trifluoride and sulfuric acid from boron trifluoride hydrate |
| CN101219798A (en) * | 2007-11-14 | 2008-07-16 | 李可宏 | Method for extracting sodium bisulfate from sodium chlorite waste acid |
-
2011
- 2011-06-10 CN CN2011101545172A patent/CN102249256A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1188758A (en) * | 1967-09-08 | 1970-04-22 | U S S Agri Chemicals Inc | Manufacture of Boron Trifluoride. |
| US3690821A (en) * | 1971-03-23 | 1972-09-12 | United States Steel Corp | Manufacture of boron trifluoride |
| CN1231214A (en) * | 1997-12-08 | 1999-10-13 | 埃勒夫阿托化学有限公司 | Preparation of boron trifluoride and sulfuric acid from boron trifluoride hydrate |
| CN101219798A (en) * | 2007-11-14 | 2008-07-16 | 李可宏 | Method for extracting sodium bisulfate from sodium chlorite waste acid |
Non-Patent Citations (1)
| Title |
|---|
| 《舰船科学技术》 20100531 韩瑞雄，周俊波 高纯三氟化硼制备技术研究 第100页 1 第32卷, 第5期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432030A (en) * | 2011-12-16 | 2012-05-02 | 天津市泰亨气体有限公司 | Preparation method of boron trifluoride |
| CN103360415A (en) * | 2013-07-16 | 2013-10-23 | 如皋市众昌化工有限公司 | Preparation method of boron trifluoride acetonitrile |
| CN105803480A (en) * | 2016-05-09 | 2016-07-27 | 上海应用技术学院 | Preparation method of boron trifluoride gas |
| CN106248520A (en) * | 2016-07-19 | 2016-12-21 | 苏州金宏气体股份有限公司 | A kind of detect the method and device of hydrogen fluoride content in boron trifluoride unstripped gas |
| CN112850731A (en) * | 2021-02-01 | 2021-05-28 | 山东合益气体股份有限公司 | Method and device for recovering boron trifluoride from wastewater containing boron trifluoride |
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Application publication date: 20111123 |