CN101829601A - Method for preparing environmentally-friendly catalyst for producing cephalosporin - Google Patents
Method for preparing environmentally-friendly catalyst for producing cephalosporin Download PDFInfo
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- CN101829601A CN101829601A CN200910047398A CN200910047398A CN101829601A CN 101829601 A CN101829601 A CN 101829601A CN 200910047398 A CN200910047398 A CN 200910047398A CN 200910047398 A CN200910047398 A CN 200910047398A CN 101829601 A CN101829601 A CN 101829601A
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- acid
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- complex
- dimethyl carbonate
- boron trifluoride
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Abstract
The invention discloses a method for preparing an environmentally-friendly catalyst for producing cephalosporin. The method comprises the following steps of: reacting sulfuric acid, boric acid with hydrofluoric acid to obtain boron trifluoride gas; then mixing the boron trifluoride gas and dimethyl carbonate, and performing complex reaction on the mixture to obtain a complex mother liquid; and then cooling and crystallizing the complexation mother liquid, and collecting a solid crystal from the complex mother liquid, namely the environmentally-friendly catalyst for producing the cephalosporin. By using the method, the boron trifluoride dimethyl carbonate complex is the white solid crystal; and the boron trifluoride content is more than or equal to 45 percent, the performance of the complex is stable, the active ingredient content of the product is multiplied, and the defect of the low-concentration product is overcome.
Description
Technical field
The present invention relates to produce the Preparation of catalysts method that cynnematin is used.
Background technology
Cephalosporins (Cephalosporins) is the cephalosporin that separates by in the crown head spore bacteria culture fluid, a series of semisynthetic antibiotics that obtain through transforming side chain.Its advantage is: has a broad antifungal spectrum has efficiently anaerobic bacteria; The allergic reaction that causes is low than PCs; To acid and more stable to various bacteriogenic beta-lactamases; The same penicillin of the mechanism of action also is to suppress the generation of bacteria cell wall and the purpose that reaches sterilization.Belong to bactericide breeding period.Because its bad reaction and toxic and side effect are lower, are current exploitation class antibiotic faster.
The main chemical process that cephalosporins is synthetic: the C7 bit amino is transformed chemical synthesis, 7 α transform the chemical synthesis of methoxyl group, the chemical synthesis that transform the C3 position etc. as.In the chemical synthesis process that transform the C3 position, the boric carbonic acid dimethyl ester complex trifluoride activity is strong, is the most effective catalyst at present, safe in utilization, convenient, environmentally safe.
The production technology of existing boric carbonic acid dimethyl ester complex trifluoride is:
With 20% oleum, boric anhydride, fluorite mass ratio with 9: 1: 3, reaction generates boron triflouride gas under 130 ℃ of conditions, then with the boron triflouride gas that generates behind the persulfuric acid gas washing, be passed in the dimethyl carbonate solvent, complexing under gas phase condition, finished product are liquid phase or Solid complexing thing.Because the solubility of boric carbonic acid dimethyl ester complex trifluoride in dimethyl carbonate is lower, in the time of 25 ℃ in the saturated solution boron trifluoride content only be 10%, the high energy of existing production technology only reaches 25%.Boron trifluoride content is low, and in use dosage is difficult to control.Photochemical reaction easily takes place in the boron trifluoride owing to free state in the dimethyl carbonate simultaneously, and low concentration finished color meeting flavescence has influenced product quality and result of use, makes the yield of synthetic cephazoline reduce.In cephazoline raw material 7ACA, store after three days finished product in use yield reduce 2-3 percentage point.
Summary of the invention
The object of the present invention is to provide a kind of environment-friendly type Preparation of catalysts method that cynnematin is used of producing, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
Sulfuric acid, boric acid and hydrofluoric acid 90-150 ℃ of reaction, reaction time 8-18 hour, are generated boron triflouride gas; Mix with dimethyl carbonate then, carry out complex reaction, the complexing temperature is 40-80 ℃, and the time is 4-12 hour.Obtain the complexing mother liquor, be cooled to 20-50 ℃ of crystallization then, from the complexing mother liquor, collect solid crystal, be the environment-friendly type catalyst that described production cynnematin is used.
Preferably, collected the mother liquor behind the solid crystal, recycled.
The mass ratio of material is:
Sulfuric acid: boric acid: hydrofluoric acid=5-7: 1-3: 1-3;
Dimethyl carbonate: boron triflouride gas 5: 1-10;
Method of the present invention, the boric carbonic acid dimethyl ester complex trifluoride that is obtained is a white crystalline solid, boron trifluoride content 〉=45% wherein, complex compound stable performance, effective component content in the product is significantly improved, and has overcome the above-mentioned shortcoming of low concentration product.
The specific embodiment
Embodiment 1
Sulfuric acid, boric acid, hydrofluoric acid are joined in the gas making still with 6: 1: 1 mass ratio, react under 125 ℃ of conditions, 12 hours reaction time became boron triflouride gas.The gas of gas making still enters the complexing still, is filled with dimethyl carbonate in the complexing still, and the mass ratio of the boron triflouride gas that every still produces in the loading of dimethyl carbonate and the gas making still is 6: 1.The complexing temperature is 40 ℃, and the time is 12 hours.With pump dimethyl carbonate solution is circulated in complexing still and filter during complexing, simultaneously filter is cooled, make the temperature in the filter hang down 16 ℃ than the temperature of complexing still, make the mother liquor that contains boric carbonic acid dimethyl ester complex trifluoride under this temperature, become supersaturated solution, separate out crystal;
Mother liquor is returned in the complexing still usefulness again, and the gained crystal is finished product through the centrifuge drying.Finished product is a white crystal, and boron trifluoride content reaches 45%.
Embodiment 2
Sulfuric acid, boric acid, hydrofluoric acid are joined in the gas making still with 5: 1: 1 mass ratio, and reaction is 15 hours under 150 ℃ of conditions, generates boron triflouride gas.The gas of gas making still enters the complexing still, is filled with dimethyl carbonate in the complexing still, and the mass ratio of the boron triflouride gas that every still produces in the loading of dimethyl carbonate and the gas making still is 5: 1.The complexing temperature is 80 ℃, and the time is 4 hours.All the other are with embodiment 1.Finished product is a white crystal, and boron trifluoride content reaches 46%.
Claims (6)
1. produce the environment-friendly type Preparation of catalysts method that cynnematin is used, it is characterized in that, comprise the steps:, generate boron triflouride gas sulfuric acid, boric acid and hydrofluoric acid; Mix with dimethyl carbonate then, carry out complex reaction, obtain the complexing mother liquor, cooling crystallization is collected solid crystal from the complexing mother liquor then, is the environment-friendly type catalyst that described production cynnematin is used.
2. method according to claim 1 is characterized in that, has collected the mother liquor behind the solid crystal, recycles.
3. method according to claim 1 is characterized in that, with sulfuric acid, boric acid and hydrofluoric acid 90-150 ℃ of reaction, reaction time 8-18 hour.
4. method according to claim 1 is characterized in that, the complexing temperature is 40-80 ℃, and the time is 4-12 hour.
5. method according to claim 1 is characterized in that, the complexing mother liquor is cooled to 20-50 ℃ of crystallization.
6. according to each described method of claim 1～5, it is characterized in that the mass ratio of material is: sulfuric acid: boric acid: hydrofluoric acid=5-7: 1-3: 1-3; Dimethyl carbonate: boron triflouride gas 5: 1-10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910047398A CN101829601A (en) | 2009-03-11 | 2009-03-11 | Method for preparing environmentally-friendly catalyst for producing cephalosporin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910047398A CN101829601A (en) | 2009-03-11 | 2009-03-11 | Method for preparing environmentally-friendly catalyst for producing cephalosporin |
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| Publication Number | Publication Date |
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| CN101829601A true CN101829601A (en) | 2010-09-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200910047398A Pending CN101829601A (en) | 2009-03-11 | 2009-03-11 | Method for preparing environmentally-friendly catalyst for producing cephalosporin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2009
- 2009-03-11 CN CN200910047398A patent/CN101829601A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20100915 |