CN100355761C - Production of boric carbonic acid dimethyl ester complex trifluoride - Google Patents
Production of boric carbonic acid dimethyl ester complex trifluoride Download PDFInfo
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- CN100355761C CN100355761C CNB2006100098382A CN200610009838A CN100355761C CN 100355761 C CN100355761 C CN 100355761C CN B2006100098382 A CNB2006100098382 A CN B2006100098382A CN 200610009838 A CN200610009838 A CN 200610009838A CN 100355761 C CN100355761 C CN 100355761C
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Abstract
The present invention provides a production method of boron trifluoride methyl carbonate complex compounds. In the method, 20% of fuming sulfuric acid, boron oxide and fluorite are added to gas making kettles in the quality proportion of 9:1:3, react at 130DEGC and generate boron trifluoride gas; gas expelled from the gas making kettles enters a buffer tank which is connected with a complexing kettle through a pipeline; methyl carbonate is filled in the complexing kettle, and the proportion of the filling quantity of methyl carbonate and the mass of the boron trifluoride gas generated in each gas making kettle is 5:1 to 10:1; the upper part of the complexing kettle is provided with a circulation pipe which is connected with a circulation pump; the circulation pump is connected with a water conservancy jet pump arranged above a gas inlet; mother solutions and precipitates obtained after complexing are led out from the bottom of the complexing kettle and enter a pressure filter; filtered crystals are the products of the present invention; the mother solutions expelled from the pressure filter are circulated to the complexing kettle. The method of the present invention can be used for producing boron trifluoride methyl carbonate complex compounds which have the advantages of stable performance, high effective component content and convenient use.
Description
(1) technical field
That the present invention relates to is a kind of preparation method of complex compound.
(2) background technology
Boric carbonic acid dimethyl ester complex trifluoride appears in the production of cephalosporins medicine, has changed the situation that original cephalosporins medicine becomes production art to take as the leading factor with liquid phase reaction, and original product yield has been improved nearly 8 percentage points.Simultaneously owing to all must use expensive raw material such as 7-ACA, 7-ADCA, 6-APA, GCLE in the production process of cephalosporins medicine, and reaction process relates to the alkyl isomerization mostly, makes that the application prospect of boric carbonic acid dimethyl ester complex trifluoride is very wide.
At present the production technique of boric carbonic acid dimethyl ester complex trifluoride is that reaction generates boron triflouride gas under 130 ℃ of conditions with 20% oleum, boron oxide, the fluorite mass ratio with 9: 1: 3; The boron triflouride gas that generates behind the persulfuric acid gas washing, directly is passed in the bucket that dimethyl carbonate solvent is housed complexing under gas phase condition.Because the solubleness of boric carbonic acid dimethyl ester complex trifluoride in methylcarbonate is lower, in the time of 25 ℃ in the saturated solution content be about 10% (in boron trifluoride), and application requiring content is about 22%, so finished product state is liquid phase, solid-phase mixture, (liquid phase is the saturated mother liquor of methylcarbonate, and solid phase is the boric carbonic acid dimethyl ester complex trifluoride crystal).Under this kind state, liquid phase boron trifluoride content is lower than solid phase, in use often causes the amount of adding to be difficult to control.Because the volatilization of saturated mother liquor makes finished product that certain loss be arranged in storage process, along with the growth in storage time, the content of boron trifluoride reduces (the normal temperature and pressure opening is placed content reduction about 35% after three days) greatly again.Photochemical reaction easily takes place in the boron trifluoride owing to free state in the methylcarbonate simultaneously, make prolongation finished color with the storage time change (flavescence), quality product and result of use have been influenced greatly, make the yield of synthetic Kefzol reduce (, store 2-3 percentage point of finished product yield reduction in use after three days) in Kefzol raw material 7ACA.
Along with the requirement in the medicine production process improves constantly, the requirement of the detection of quality product is also more and more stricter.Because the detection means difference of liquid phase, solid-phase mixture is very unsound on detection method with the boric carbonic acid dimethyl ester complex trifluoride that this kind process means is produced, and can only estimate the wherein content of boron trifluoride with the effect of practical application.
Because the viscosity of liquid, solid biphase boric carbonic acid dimethyl ester complex trifluoride is bigger, the finished product that in use is difficult to will be stored in the bucket pumps fully, causes a certain amount of waste simultaneously, causes no small loss for producer and user.
(3) summary of the invention
The object of the present invention is to provide a kind of can be so that the stable performance of the boric carbonic acid dimethyl ester complex trifluoride product that arrives, the effective component content height in the product, the production method of boric carbonic acid dimethyl ester complex trifluoride easy to use.
The object of the present invention is achieved like this: with 20% oleum, boron oxide, fluorite joins in the gas making still with 9: 1: 3 mass ratio, reaction generates boron triflouride gas under 130 ℃ of conditions, the gas that goes out the gas making still enters surge tank, surge tank links to each other with the complexing still by pipeline, be filled with methylcarbonate in the complexing still, the mass ratio of the boron triflouride gas that every still produces in the loading level of methylcarbonate and the gas making still is 5: 1-10: 1, complexing still top is provided with circulation tube, connect recycle pump on the circulation tube, recycle pump links to each other with the water conservancy squirt pump that the inlet mouth top is provided with, mother liquor after the complexing and precipitate are drawn from the bottom of complexing still and are entered pressure filter, the crystal that filters out is a product of the present invention, and the Recycling Mother Solution that goes out pressure filter is to the complexing still.
The present invention can also comprise: add Glacial acetic acid in methylcarbonate, the mass ratio of methylcarbonate and Glacial acetic acid is 900: 80.
Need heating when producing boron triflouride gas, and it is less at reaction later stage aerogenesis, owing to expand with heat and contract with cold the phenomenon that boron triflouride gas flows backward to surge tank can take place, produce negative pressure in the complexing still, with methylcarbonate steam suck-back and in pipeline complexing form needle-like crystal blocking pipeline gradually.The present invention places a recycle pump by the complexing still, and piping insulation to being connected with recycle pump, draw the lower mother liquor of relative content on complexing still top, hydraulic jet pump by the inlet mouth top is thrown mother liquor in the complexing still into by inlet mouth, because mother liquor and boron triflouride gas still can complexings, boron triflouride gas can be sucked back to the complexing still, thereby address this problem.Fully after the complexing mother liquor and the boric carbonic acid dimethyl ester complex trifluoride crystal of separating out are injected in the pressure filter together, feed two atmospheric pressurized air and carry out press filtration, mother liquor is returned in the complexing still recycled.Collect resulting dried crystals and be finished product, finished product of the present invention is simple crystalline structure, and the effective component content height in the product, stable performance, metering are conveniently.
In dimethyl carbonate solvent, add a certain amount of Glacial acetic acid, can improve the ability that mother liquor absorbs boron trifluoride, increase the stability of complex compound.Because the change of solvent polarity, the complex compound crystal becomes particulate state by needle-like.
(4) description of drawings
Accompanying drawing is a process flow diagram of the present invention.
(5) embodiment
For a more detailed description to the present invention for example below in conjunction with accompanying drawing:
1,20% oleum, boron oxide, fluorite are joined in the gas making still 1 with 9: 1: 3 mass ratio, reaction generates boron triflouride gas under 130 ℃ of conditions.The gas that goes out the gas making still enters surge tank 2, and surge tank links to each other with complexing still 4 by pipeline.Be filled with methylcarbonate in the complexing still, the mass ratio of the boron triflouride gas that every still produces in the loading level of methylcarbonate and the gas making still is 5: 1-10: 1.Complexing still top is provided with circulation tube, connects recycle pump 8 on the circulation tube, and recycle pump links to each other with the water conservancy squirt pump 3 that the inlet mouth top is provided with.Mother liquor after the complexing and precipitate are drawn from the bottom of complexing still and are entered pressure filter 5, feed 2 atmospheric pressurized air in the pressure filter, and the crystal that filters out is a product of the present invention.The mother liquor that goes out pressure filter enters mother liquor tank 6 by recycle pump 7, is circulated to complexing still 4 by recycle pump 9 again.
2,20% oleum, boron oxide, fluorite are joined in the gas making still 1 with 9: 1: 3 mass ratio, reaction generates boron triflouride gas under 130 ℃ of conditions.The gas that goes out the gas making still enters surge tank 2, and surge tank links to each other with complexing still 4 by pipeline.Be filled with methylcarbonate and Glacial acetic acid in the complexing still, the mass ratio of methylcarbonate and Glacial acetic acid is 900: 80, and the mass ratio of the boron triflouride gas that every still produces in the loading level of the mixture of methylcarbonate and Glacial acetic acid and the gas making still is 8: 1.Complexing still top is provided with circulation tube, connects recycle pump 8 on the circulation tube, and recycle pump links to each other with the water conservancy squirt pump 3 that the inlet mouth top is provided with.Mother liquor after the complexing and precipitate are drawn from the bottom of complexing still and are entered pressure filter 5, feed 2 atmospheric pressurized air in the pressure filter, and the crystal that filters out is a product of the present invention.The mother liquor that goes out pressure filter enters mother liquor tank 6 by recycle pump 7, is circulated to complexing still 4 by recycle pump 9 again.
Claims (2)
1, a kind of production method of boric carbonic acid dimethyl ester complex trifluoride, with 20% oleum, boron oxide, fluorite joins in the gas making still with 9: 1: 3 mass ratio, reaction generates boron triflouride gas under 130 ℃ of conditions, it is characterized in that: the gas that goes out the gas making still enters surge tank, surge tank links to each other with the complexing still by pipeline, be filled with methylcarbonate in the complexing still, the mass ratio of the boron triflouride gas that every still produces in the loading level of methylcarbonate and the gas making still is 5: 1-10: 1, complexing still top is provided with circulation tube, connect recycle pump on the circulation tube, recycle pump links to each other with the water conservancy squirt pump that the inlet mouth top is provided with, mother liquor after the complexing and precipitate are drawn from the bottom of complexing still and are entered pressure filter, the crystal that filters out is a product of the present invention, and the Recycling Mother Solution that goes out pressure filter is to the complexing still.
2, the production method of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that: add Glacial acetic acid in methylcarbonate, the mass ratio of methylcarbonate and Glacial acetic acid is 900: 80.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100098382A CN100355761C (en) | 2006-03-22 | 2006-03-22 | Production of boric carbonic acid dimethyl ester complex trifluoride |
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| CNB2006100098382A CN100355761C (en) | 2006-03-22 | 2006-03-22 | Production of boric carbonic acid dimethyl ester complex trifluoride |
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| CN1817886A CN1817886A (en) | 2006-08-16 |
| CN100355761C true CN100355761C (en) | 2007-12-19 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103044474A (en) * | 2012-12-31 | 2013-04-17 | 东营合益化工有限公司 | Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound |
| CN115197255B (en) * | 2022-08-02 | 2023-05-02 | 山东合益气体股份有限公司 | Low-moisture solid boron trifluoride methyl ethyl carbonate complex and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594321A (en) * | 2004-06-23 | 2005-03-16 | 哈药集团制药总厂 | Process for preparing cephazoline three-position intermediate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594321A (en) * | 2004-06-23 | 2005-03-16 | 哈药集团制药总厂 | Process for preparing cephazoline three-position intermediate |
Non-Patent Citations (2)
| Title |
|---|
| 三氟化硼乙醚络合物的合成与应用 康军.上海化工，第24卷第9期 1999 * |
| 第三代头孢菌素头孢哌酮钠的合成工艺研究 金石，黄金花，徐泽龙，郭云波，文毅.中国药物化学杂志，第14卷第3期 2004 * |
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Assignee: Heilongjiang Haoyun Fine Chemical Co., Ltd. Assignor: Heilongjiang Haoyun Trade Co., Ltd. Contract record no.: 2010230000036 Denomination of invention: Production of boric carbonic acid dimethyl ester complex trifluoride Granted publication date: 20071219 License type: Exclusive License Open date: 20060816 Record date: 20100623 |
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Effective date of registration: 20160920 Address after: 151400 Suihua city in Heilongjiang province Anda City of Hadaqi industrial corridor anda Petrochemical area Patentee after: Heilongjiang Hao Yun Pharmaceutical Co., Ltd. Address before: 151400 Suihua city in Heilongjiang province Anda City of Hadaqi industrial corridor anda Petrochemical area Patentee before: Heilongjiang Haoyun Fine Chemical Co., Ltd. |