CN103360415A - Preparation method of boron trifluoride acetonitrile - Google Patents
Preparation method of boron trifluoride acetonitrile Download PDFInfo
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- CN103360415A CN103360415A CN2013102963945A CN201310296394A CN103360415A CN 103360415 A CN103360415 A CN 103360415A CN 2013102963945 A CN2013102963945 A CN 2013102963945A CN 201310296394 A CN201310296394 A CN 201310296394A CN 103360415 A CN103360415 A CN 103360415A
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- acetonitrile
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Abstract
The invention discloses a preparation method of boron trifluoride acetonitrile. The preparation method comprises the following steps: mixing fuming sulfuric acid with boric acid to react to generate diboron trioxide, reacting the diboron trioxide with hydrogen fluoride to generate a boron trifluoride gas, filtering the boron trifluoride gas through sulfuric acid to obtain a pure gas, and adding acetonitrile for complexing to obtain a finished product. The preparation method disclosed by the invention has the advantages that the fuming sulfuric acid and the boric acid react, so that the safety is high and no waste residue is generated, the sulfuric acid can be recycled in phosphate fertilizer plants, and meanwhile, the labor intensity of the staff is reduced, and physical and mental health of the staff are benefitted; moreover, the product produced by the preparation method disclosed by the invention is stable and high in yield.
Description
Technical field
The present invention relates to a kind of preparation method of boron trifluoride acetonitrile, belong to the compound preparation field.
Background technology
Boron trifluoride complex is the very strong catalyzer of a kind of activity, can be used in the multiple organic synthesis, especially in cephalosporins antibacterials synthesis technique, owing to introducing boron trifluoride complex, having shortened the reaction times of existing product, is that the yield of existing product improves greatly.And the catalytic effect of boron trifluoride acetonitrile complex compound more is better than boron trifluoride ethyl ether complex, so the boron trifluoride acetonitrile complex compound has with wide market outlook.
At present, the domestic fluorite borate method that adopts is produced boron triflouride gas more, the method is in process of production take fluorite as reaction raw materials, can produce a large amount of calcium sulphate solid waste residues after the reaction, environment is caused very serious pollution, use simultaneously the method production, work personnel's labour intensity is large, affects the healthy of producers; In addition, the fluorite borate method is intermittent reaction, yields poorly.
Summary of the invention
The present invention is directed to deficiency of the prior art, provide a kind of output high, pollute the preparation method of few boron trifluoride acetonitrile.
For solving the problems of the technologies described above, the present invention adopts following technical scheme to realize:
A kind of preparation method of boron trifluoride acetonitrile is characterized in that: technological process is as follows:
(1) nitration mixture: generate boron trioxide take oleum and boric acid as raw material reaction;
(2) gas making reaction: the fluoridation tower is carried out preheating, when temperature arrives 250 ℃, begin to advance tower with measuring the pump delivery mixed acid solution, open simultaneously the hydrogen fluoride steel cylinder and pass into hydrogen fluoride and react the production boron triflouride gas, the equation of fluoridation is:
3H
2S
2O
7+H
3BO
3+3HF→BF
3+6H
2SO
4
(3) purify: in the purification container, the boron triflouride gas that obtains is filtered purification through sulfuric acid;
(4) complex reaction: acetonitrile is carried out preheating stand-by, preheating temperature is 60 ℃, begins to add acetonitrile and carry out complexing when producing boron triflouride gas arrival complexing tank, and the boron trifluoride acetonitrile complex compound that complexing is good is fed directly in the finished product receiving tank and makes finished product.
The weight ratio of oleum and boric acid is 1:8 in the described mixed acid solution.
Preferably, per hour add 200～250kg nitration mixture in the fluoridation tower.
Preferably, passing into hydrofluoric speed is 25～26kg/h.
The complexing temperature is 70～80 ℃ when complexing, and proportion is greater than 0.855, and the acetonitrile flow rate control is at 100kg/h, and content is 18～20%.
Beneficial effect of the present invention: react with oleum and boric acid, produce boron trioxide, then boron trioxide and hydrogen fluoride reaction are produced boron triflouride gas, and be safe, do not have waste residue, sulfuric acid is to phosphate fertilizer plant's second stage employ, reduce simultaneously staff labor intensity, favourable employee is physically and mentally healthy, in addition, the product that the present invention produces is stable, and yield is high.
Description of drawings
Fig. 1 is the process flow sheet of preparation boron trifluoride acetonitrile.
Embodiment
Below in conjunction with specific embodiment the present invention is elaborated.
Embodiment 1
1800kg sulfuric acid and 250kg boric acid are mixed, reaction tower is carried out preheating, treat that the tower temperature reaches 250 degree, advance tower with measuring the pump delivery nitration mixture, speed is 200Kg/h, opens simultaneously the hydrogen fluoride steel cylinder and passes into hydrogen fluoride and react, and passing into hydrofluoric speed is 25kg/h; In the purification container, the boron triflouride gas that obtains is filtered purification through sulfuric acid; Acetonitrile is preheating to 60 degree stand-by, when producing boron triflouride gas arrival complexing tank, begin to add acetonitrile and carry out complexing, the complexing temperature must remain on 70 ℃ when complexing, proportion is greater than 0.855, the acetonitrile flow rate control was at 100/ hour, the boron trifluoride acetonitrile complex compound that complexing is good is fed directly in the finished product receiving tank, and content is being 18%.
Embodiment 2
1800kg sulfuric acid and 250kg boric acid are mixed, reaction tower is carried out preheating, treat that the tower temperature reaches 250 degree, advance tower with measuring the pump delivery nitration mixture, speed is 200kg/h, opens simultaneously the hydrogen fluoride steel cylinder and passes into hydrogen fluoride and react, and passing into hydrofluoric speed is 25kg/h; In the purification container, the boron triflouride gas that obtains is filtered purification through sulfuric acid; Acetonitrile is preheating to 60 degree stand-by, when producing boron triflouride gas arrival complexing tank, begin to add acetonitrile and carry out complexing, the complexing temperature must remain on 80 ℃ when complexing, proportion is greater than 0.89, the acetonitrile flow rate control was at 100/ hour, the boron trifluoride acetonitrile complex compound that complexing is good is fed directly in the finished product receiving tank, and content is being 20%.
Above-described embodiment is only in order to illustrate technical scheme of the present invention; but not design of the present invention and protection domain are limited; those of ordinary skill of the present invention is made amendment to technical scheme of the present invention or is equal to replacement; and not breaking away from aim and the scope of technical scheme, it all should be encompassed in the claim scope of the present invention.
Claims (5)
1. the preparation method of a boron trifluoride acetonitrile, it is characterized in that: technological process is as follows:
(1) nitration mixture: generate boron trioxide take oleum and boric acid as raw material reaction;
(2) gas making reaction: the fluoridation tower is carried out preheating, when temperature arrives 250 ℃, begin to advance tower with measuring the pump delivery mixed acid solution, open simultaneously the hydrogen fluoride steel cylinder and pass into hydrogen fluoride and react the production boron triflouride gas, the equation of fluoridation is:
3H
2S
2O
7+H
3BO
3+3HF→BF
3+6H
2SO
4
(3) purify: in the purification container, the boron triflouride gas that obtains is filtered purification through sulfuric acid;
(4) complex reaction: acetonitrile is carried out preheating stand-by, preheating temperature is 60 ℃, begins to add acetonitrile and carry out complexing when producing boron triflouride gas arrival complexing tank, and the boron trifluoride acetonitrile complex compound that complexing is good is fed directly in the finished product receiving tank and makes finished product.
2. the preparation method of a kind of boron trifluoride acetonitrile according to claim 1, it is characterized in that: the weight ratio of oleum and boric acid is 1:8 in the described mixed acid solution.
3. the preparation method of a kind of boron trifluoride acetonitrile according to claim 1 is characterized in that: per hour add 200～250kg nitration mixture in the fluoridation tower.
4. the preparation method of a kind of boron trifluoride acetonitrile according to claim 1, it is characterized in that: passing into hydrofluoric speed is 25～26kg/h.
5. the preparation method of a kind of boron trifluoride acetonitrile according to claim 1, it is characterized in that: the complexing temperature is 70～80 ℃ when complexing, and proportion is greater than 0.855, and the acetonitrile flow rate control is at 100kg/h, and content is 18～20%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891757A (en) * | 2009-05-22 | 2010-11-24 | 于景东 | Preparation method of catalyst for producing cephalosporin |
| CN102249256A (en) * | 2011-06-10 | 2011-11-23 | 格兰特医药科技(南通)有限公司 | Process for preparing boron trifluoride gas |
| CN103012454A (en) * | 2012-12-31 | 2013-04-03 | 东营合益化工有限公司 | Method for preparing solid boron trifluoride acetonitrile complex and application thereof |
-
2013
- 2013-07-16 CN CN2013102963945A patent/CN103360415A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891757A (en) * | 2009-05-22 | 2010-11-24 | 于景东 | Preparation method of catalyst for producing cephalosporin |
| CN102249256A (en) * | 2011-06-10 | 2011-11-23 | 格兰特医药科技(南通)有限公司 | Process for preparing boron trifluoride gas |
| CN103012454A (en) * | 2012-12-31 | 2013-04-03 | 东营合益化工有限公司 | Method for preparing solid boron trifluoride acetonitrile complex and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 孙福楠: "瓶装三氟化硼的大规模生产", 《低温与特气》, vol. 22, no. 1, 29 February 2004 (2004-02-29), pages 24 - 27 * |
| 韩瑞雄等: "高纯三氟化硼制备技术研究", 《舰船科学技术》, vol. 32, no. 5, 15 May 2010 (2010-05-15), pages 99 - 102 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20131023 |