Preparation method of boron trifluoride complex

A technology of boron trifluoride and preparation process, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, chemical/physical processes, etc., and can solve problems such as energy waste, severe environmental pollution, etc.

Inactive Publication Date: 2011-06-08
于志红
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production process of boron trifluoride complex is to react 20% oleum, boric anhydride, and fluorite at a mass ratio of 9:1:3 to generate boron trifluoride gas at 130°C. Due to the use of fluorite as the reaction raw material, a large amount of waste liquid and waste residue mixed with sulfuric acid and calcium sulfate will appear after the reaction, and these waste liquid and waste residue will seriously pollute the environment
Moreover, the temperature of the reaction is 130°C, which needs to be heated to reach this temperature, which will inevitably cause a waste of energy, and also accelerate the corrosion rate of sulfuric acid to equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0009] Example 1, first add sulfuric acid to the reaction tank, then add boric anhydride, pass into sulfur trioxide, and finally pass into hydrogen fluoride; the ratio of parts is: 2 sulfuric acid, 0.4 boric anhydride, 2 sulfur trioxide, 5 hydrogen fluoride, if the production Boron trifluoride dimethyl carbonate complex, the parts of boron trifluoride and dimethyl carbonate are 1.5 boron trifluoride, 10 dimethyl carbonate, and the solid boron trifluoride dimethyl carbonate complex is separated by centrifugation The compound is put into the transport bag, and the mother liquor is returned to the complexing tank for re-complexation; if the boron trifluoride-acetonitrile complex is produced, 0.8 parts of boron trifluoride and 4 parts of acetonitrile are directly poured into the packaging barrel. When passing sulfur trioxide and hydrogen fluoride, the temperature is controlled at 50°C.

example 2

[0010] Example 2, first add fuming acid to the reaction tank, then add boric acid, feed sulfur trioxide, and finally feed hydrogen fluoride; the proportion of parts is 3 fuming acid, 0.4 boric acid, 2 sulfur trioxide, and 2 hydrogen fluoride. Boron trifluoride dimethyl carbonate complex, the ratio of boron trifluoride and dimethyl carbonate is 1.5 boron trifluoride, 10 dimethyl carbonate, solid boron trifluoride dimethyl carbonate is separated by centrifugation The complex is packed into the transport bag, and the mother liquor is returned to the complexing tank for re-complexation; if the boron trifluoride acetonitrile complex is produced, the parts of boron trifluoride and acetonitrile are 0.8 parts of boron trifluoride and 4 parts of acetonitrile, which can be directly Pour into shipping barrels. When passing sulfur trioxide and hydrogen fluoride, the temperature is controlled at 50°C.

example 3

[0011] Example 3, first add sulfuric acid to the reaction tank, then add boric anhydride, feed sulfur trioxide, and finally feed hydrogen fluoride; the ratio of parts is: 5 sulfuric acid, 1.5 boric anhydride, 4 sulfur trioxide, 7 hydrogen fluoride, if the production Boron trifluoride dimethyl carbonate complex, the number of parts of boron trifluoride and dimethyl carbonate is 1.25 boron trifluoride, 5 dimethyl carbonate, and the solid boron trifluoride dimethyl carbonate complex is separated by centrifugation The compound is put into the transport bag, and the mother liquor is returned to the complexing tank for re-complexation; if the boron trifluoride-acetonitrile complex is produced, 1 part of boron trifluoride and 5 parts of acetonitrile are directly poured into the packaging barrel. When passing sulfur trioxide and hydrogen fluoride, the temperature is controlled at 60°C.

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PUM

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Abstract

The invention relates to a catalyst applied to the manufacturing technique of cephalo-type products, comprising the steps of firstly adding sulphuric acid or fuming acid in a reaction kettle, and then adding boron anhydrous or boric acid, infusing sulphur trioxide in the reaction kettle, and finally infusing hydrogen fluoride in the reaction kettle, the contents of the components are respectively2-5 parts of sulphuric acid or 3-5 parts of fuming acid, 0.4-1.5 parts of boron anhydrous or 0.4-1.5 parts of boric acid, 2-4 parts of sulphur trioxide and 2-7 parts of hydrogen fluoride. For the production of boron trifluoride-dimethyl carbonate complex, the raw materials comprise 1.25-1.5 parts of boron trifluoride and 5-10 parts of dimethyl carbonate, and solid boron-trifluoride dimethyl carbonate complex is separated by centrifuging and then packed into a transportation bag, and finally returning the mother liquor to a complexing kettle to carry out complexation again. For the production of boron trifluoride-acetonitrile complex, the raw materials comprise 0.8-1 part of boron trifluoride and 4-5 parts of acetonitrile, and the raw materials are directly put into a package bucket. The invention has the advantages of low reaction temperature, moderate reaction and high safety. The invention does not generate waste slag and waste liquor, avoids environmental pollution and saves energysource. The product of the invention is stable and has high yield. The method is simply operated and suitable for mass production.

Description

Technical field: [0001] The invention relates to a catalyst used in the production process of cephalosporin products. Background technique: [0002] With the research and development of cephalosporin products, the international processing capacity of cephalosporin products has reached a new level, and now it can produce more than 50 kinds of products, especially in ceftazidime, cefotaxime sodium, ceftriaxone sodium, cefazolin sodium , ceftezole sodium, cefradine and other products such as boron trifluoride complexes have been fully utilized. In particular, cephalosporin products are widely used clinically and become indispensable for antibacterial and anti-inflammatory. Boron trifluoride complexes appear as catalysts in the production of cephalosporin drugs, which shortens the reaction time of the original products and converts the original products. The yield of some products has increased by nearly 10 percentage points. At the same time, resources are used reasonably and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02B01J31/14
Inventor 于志红杨金平
Owner 于志红
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