CN102276638A - Process for producing boron trifluoride complex - Google Patents
Process for producing boron trifluoride complex Download PDFInfo
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- CN102276638A CN102276638A CN2011101540060A CN201110154006A CN102276638A CN 102276638 A CN102276638 A CN 102276638A CN 2011101540060 A CN2011101540060 A CN 2011101540060A CN 201110154006 A CN201110154006 A CN 201110154006A CN 102276638 A CN102276638 A CN 102276638A
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Abstract
The invention relates to a process for producing a boron trifluoride complex. The process comprises the following steps of: a, making gas, namely slowly dripping an organic solvent into a caustic soda flake kettle and absorbing water to generate an organic solvent with vapor, leading the organic solvent with the vapor into a complexing device, leading boron trifluoride gas and performing a complexing reaction, and controlling the temperature to 30 to 50 DEG C and the reaction time to 2 to 5 hours; b, crystallizing, namely after the reaction is finished, stirring for 1 to 2 hours, reducing the temperature to 15 to 20 DEG C, centrifuging, collecting centrifugate and applying; and c, drying under reduced pressure, namely allowing crystals obtained after centrifugation to enter a double cone dryer, controlling the temperature to 35 to 45 DEG C, and drying for 3 to 5 hours to obtain the boron trifluoride complex. The process has the characteristics that: aqueous solution is adopted, the cost is low, liquid caustic soda generated after water is absorbed by using caustic soda flakes can be used for other working sections, and the pollution is avoided; and the reaction temperature is normal temperature or a little higher than the normal temperature and is easy to control, the vacuum drying is adopted, the cost for the application of the centrifugate is low and the like.
Description
Technical field
The present invention relates to the production technique of boron trifluoride complex, belong to chemical field.
Background technology
The production technology of the Japan and the U.S. all is to react with boron trifluoride and acetonitrile liquid, sherwood oil liquid, mono aminoethane liquid or ethyl acetate liquid at present, obtain flaky boron trifluoride complex with magnesium drum drying, this reaction has the following disadvantages: boron trifluoride mono aminoethane for example, reaction will be used the higher liquid mono aminoethane of purity, mono aminoethane is a kind of lower boiling, highly toxic liquid, thermopositive reaction when boiling point has only 16.6 ° of reactions, carry out so must be controlled under the cold condition, and product drying cost height.Therefore, need provide a kind of new production technique to solve the problems referred to above.
Summary of the invention
The production technique that the purpose of this invention is to provide a kind of boron trifluoride complex.
For achieving the above object, the technical solution used in the present invention is:
The production technique of boron trifluoride complex is characterized in that, may further comprise the steps:
A, gas making step:
Organic solvent slowly is added drop-wise in the sheet alkali still, suction produces the organic solvent that has steam, the organic solvent that will have steam imports in the complexing device, import boron triflouride gas simultaneously and carry out complex reaction, mass ratio by organic solvent and boron triflouride gas is that 1:2-4 reacts, temperature is controlled between 30-50 °, reaction times 2-5 hour;
B, crystallisation step:
Above-mentioned reaction finishes, stirred 1-2 hours, temperature drop to 15-20 ° centrifugal, apply mechanically again after centrifugate is collected;
C, drying under reduced pressure step:
Above crystal after centrifugal is entered in the double cone dryer, and controlled temperature dry 3-5 hours, obtains boron trifluoride complex at 35-45 °.
Described organic solvent is a kind of in acetonitrile, sherwood oil, mono aminoethane, the ethyl acetate.
Advantage of the present invention: this process using be the aqueous solution, cost is low, can use other workshop sections with the liquid caustic soda that generates after the sheet alkali planar water, does not pollute; Temperature of reaction normal temperature or slightly relative superiority or inferiority control easily, vacuum-drying, centrifugate are applied mechanically characteristics such as cost is low.
Embodiment
Following examples are intended to illustrate the present invention rather than to the bright further qualification of we.
Embodiment 1
The production technique of boron trifluoride complex may further comprise the steps:
A, gas making step:
Acetonitrile slowly is added drop-wise in the sheet alkali still, and suction produces acetonitrile steam, and acetonitrile steam is imported in the complexing device, import boron triflouride gas simultaneously and carry out complex reaction, mass ratio by acetonitrile and boron triflouride gas is that 1:2 reacts, and temperature is controlled between 30 °, 2 hours reaction times;
B, crystallisation step:
Above-mentioned reaction finishes, stirred 1 hour, temperature drop to 15 ° centrifugal, apply mechanically again after centrifugate is collected;
C, drying under reduced pressure step:
Above crystal after centrifugal is entered in the double cone dryer, and controlled temperature dry 3 hours, obtains boron trifluoride acetonitrile at 35 °.
Embodiment 2
The production technique of boron trifluoride complex may further comprise the steps:
A, gas making step:
Sherwood oil slowly is added drop-wise in the sheet alkali still, suction produces sherwood oil steam, sherwood oil steam is imported in the complexing device, import boron triflouride gas simultaneously and carry out complex reaction, mass ratio by sherwood oil and boron triflouride gas is that 1:2.5 reacts, temperature is controlled between 40 °, 3.5 hours reaction times;
B, crystallisation step:
Above-mentioned reaction finishes, stirred 1.5 hours, temperature drop to 18 ° centrifugal, apply mechanically again after centrifugate is collected;
C, drying under reduced pressure step:
Above crystal after centrifugal is entered in the double cone dryer, and controlled temperature dry 5 hours, obtains the boron trifluoride sherwood oil at 40 °.
Embodiment 3
The production technique of boron trifluoride complex may further comprise the steps:
A, gas making step:
Mono aminoethane slowly is added drop-wise in the sheet alkali still, suction produces mono aminoethane steam, mono aminoethane steam is imported in the complexing device, import boron triflouride gas simultaneously and carry out complex reaction, mass ratio by mono aminoethane and boron triflouride gas is that 1:4 reacts, temperature is controlled between 50 °, 5 hours reaction times;
B, crystallisation step:
Above-mentioned reaction finishes, stirred 2 hours, temperature drop to 20 ° centrifugal, apply mechanically again after centrifugate is collected;
C, drying under reduced pressure step:
Above crystal after centrifugal is entered in the double cone dryer, and controlled temperature dry 5 hours, obtains the boron trifluoride mono aminoethane at 45 °.
This process using be the aqueous solution, cost is low, can use other workshop sections with the liquid caustic soda that generates after the sheet alkali planar water, does not pollute; Temperature of reaction normal temperature or slightly relative superiority or inferiority control easily, vacuum-drying, centrifugate are applied mechanically characteristics such as cost is low.
Claims (2)
1. the production technique of boron trifluoride complex is characterized in that, may further comprise the steps:
A, gas making step:
Organic solvent slowly is added drop-wise in the sheet alkali still, suction produces the organic solvent that has steam, the organic solvent that will have steam imports in the complexing device, import boron triflouride gas simultaneously and carry out complex reaction, mass ratio by organic solvent and boron triflouride gas is that 1:2-4 reacts, temperature is controlled between 30-50 °, reaction times 2-5 hour;
B, crystallisation step:
Above-mentioned reaction finishes, stirred 1-2 hours, temperature drop to 15-20 ° centrifugal, apply mechanically again after centrifugate is collected;
C, drying under reduced pressure step:
Above crystal after centrifugal is entered in the double cone dryer, and controlled temperature dry 3-5 hours, obtains boron trifluoride complex at 35-45 °.
2. the production technique of boron trifluoride complex according to claim 1 is characterized in that: described organic solvent is a kind of in acetonitrile, sherwood oil, mono aminoethane, the ethyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201110154006.0A CN102276638B (en) | 2011-06-09 | 2011-06-09 | Process for producing boron trifluoride complex |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110154006.0A CN102276638B (en) | 2011-06-09 | 2011-06-09 | Process for producing boron trifluoride complex |
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| CN102276638A true CN102276638A (en) | 2011-12-14 |
| CN102276638B CN102276638B (en) | 2014-03-26 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108409768A (en) * | 2018-05-14 | 2018-08-17 | 东营合益化工有限公司 | A kind of preparation method of boron trifluoride benzylamine complex compound |
| CN108640938A (en) * | 2018-04-26 | 2018-10-12 | 江西瑞合精细化工有限公司 | A kind of preparation method of high-melting-point boron chloride tertiary amines complex compound |
| CN108707161A (en) * | 2018-05-14 | 2018-10-26 | 东营合益化工有限公司 | A kind of preparation method of Boron Trifluoride Ethylamine complex compound |
| CN108864163A (en) * | 2018-09-06 | 2018-11-23 | 珠海市格特生物科技有限公司 | Boron trifluoride acetonitrile solid mixt manufacturing technique method |
| CN111825705A (en) * | 2019-04-19 | 2020-10-27 | 东营合益化工有限公司 | Preparation method of boron trifluoride dimethyl sulfide complex |
| CN113150021A (en) * | 2021-04-08 | 2021-07-23 | 上海化工研究院有限公司 | Method for synthesizing boron trifluoride complex by using microchannel reactor |
| CN113860257A (en) * | 2021-11-04 | 2021-12-31 | 浙江容跃环保科技有限公司 | Method and system for regenerating and recycling glass thinning waste acid liquor |
| CN116162104A (en) * | 2023-02-23 | 2023-05-26 | 山东合益气体股份有限公司 | Preparation method of boron trifluoride isopropylamine complex |
Citations (1)
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| CN101891757A (en) * | 2009-05-22 | 2010-11-24 | 于景东 | Preparation method of catalyst for producing cephalosporin |
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2011
- 2011-06-09 CN CN201110154006.0A patent/CN102276638B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101891757A (en) * | 2009-05-22 | 2010-11-24 | 于景东 | Preparation method of catalyst for producing cephalosporin |
Non-Patent Citations (1)
| Title |
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| 康军: "三氟化硼***络合物的合成与应用", 《上海化工》, vol. 24, no. 09, 8 May 1999 (1999-05-08) * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640938A (en) * | 2018-04-26 | 2018-10-12 | 江西瑞合精细化工有限公司 | A kind of preparation method of high-melting-point boron chloride tertiary amines complex compound |
| CN108409768A (en) * | 2018-05-14 | 2018-08-17 | 东营合益化工有限公司 | A kind of preparation method of boron trifluoride benzylamine complex compound |
| CN108707161A (en) * | 2018-05-14 | 2018-10-26 | 东营合益化工有限公司 | A kind of preparation method of Boron Trifluoride Ethylamine complex compound |
| CN108409768B (en) * | 2018-05-14 | 2019-09-17 | 东营合益化工有限公司 | A kind of preparation method of boron trifluoride benzylamine complex compound |
| CN108707161B (en) * | 2018-05-14 | 2019-11-26 | 东营合益化工有限公司 | A kind of preparation method of Boron Trifluoride Ethylamine complex compound |
| CN108864163A (en) * | 2018-09-06 | 2018-11-23 | 珠海市格特生物科技有限公司 | Boron trifluoride acetonitrile solid mixt manufacturing technique method |
| CN111825705A (en) * | 2019-04-19 | 2020-10-27 | 东营合益化工有限公司 | Preparation method of boron trifluoride dimethyl sulfide complex |
| CN113150021A (en) * | 2021-04-08 | 2021-07-23 | 上海化工研究院有限公司 | Method for synthesizing boron trifluoride complex by using microchannel reactor |
| CN113860257A (en) * | 2021-11-04 | 2021-12-31 | 浙江容跃环保科技有限公司 | Method and system for regenerating and recycling glass thinning waste acid liquor |
| CN113860257B (en) * | 2021-11-04 | 2022-04-22 | 浙江容跃环保科技有限公司 | Method and system for regenerating and recycling glass thinning waste acid liquor |
| CN116162104A (en) * | 2023-02-23 | 2023-05-26 | 山东合益气体股份有限公司 | Preparation method of boron trifluoride isopropylamine complex |
| CN116162104B (en) * | 2023-02-23 | 2024-03-15 | 山东合益气体股份有限公司 | Preparation method of boron trifluoride isopropylamine complex |
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|---|---|
| CN102276638B (en) | 2014-03-26 |
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Address after: 226400 chemical industry park, Rudong, Jiangsu Patentee after: Ruentex chemical Nantong Co. Ltd. Address before: 226407 the Yellow Sea two road, Nantong chemical industry park, Rudong, Jiangsu Patentee before: Glad Pharmaceutical Technoliges (Nantong) Co.,Ltd. |
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