Method and device for purifying by-product potassium fluoroborate in synthesis of pharmaceutical intermediates

A technology for by-product potassium fluoroborate and a purification method is applied in the field of purification of by-product potassium fluoroborate in the synthesis of pharmaceutical intermediates, and can solve the problem of quenching the catalytic activity of boron trifluoride-acetonitrile complex, secondary pollution and disposal costs Advanced problems, to achieve the effect of rapid and efficient degradation, reduced consumption, and high selectivity

Active Publication Date: 2022-07-26
QILU UNIV OF TECH
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Boron trifluoride-acetonitrile complex (molecular formula is BF 3 -CH 3 CN) is a highly active catalyst, which is widely used in the production process of pharmaceutical intermediates such as zoline and cefpiramide. When the reaction reaches the end, in order to ensure the purity of the intermediate, it is necessary to quench the boron trifluoride-acetonitrile The catalytic activity of the complex is mainly achieved by adding an alkaline solution to the reaction system, turning boron trifluoride into a sodium fluoroborate solution, and pharmaceutical companies usually convert sodium fluoroborate into potassium fluoroborate, so that potassium fluoroborate is crystallized Separated from the mother liquor, because the obtained potassium fluoroborate usually contains unreacted organic matter, cyanide, fluoroboric acid and other toxic impurities, the current environmental protection department requires it to be disposed of as a hazardous waste, and it is generally disposed of by incineration. The disposal cost is high and easy. lead to secondary pollution
[0004] However, the potassium fluoride borate produced in the existing intermediate production process contains some antibiotics, organic matter, solvent and other impurities. When it is directly used as a by-product, these impurities will be transferred to the waste water in the secondary processing and utilization process. , waste gas and waste residue, causing indirect secondary pollution

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method and device for purifying by-product potassium fluoroborate in synthesis of pharmaceutical intermediates
  • Method and device for purifying by-product potassium fluoroborate in synthesis of pharmaceutical intermediates
  • Method and device for purifying by-product potassium fluoroborate in synthesis of pharmaceutical intermediates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]Under constant stirring, the reaction temperature was controlled at 40 °C, and 1 mol / L sodium carbonate solution was added to the final solution system of the 2000 mL pharmaceutical intermediate reaction (the synthesis reaction of pharmaceutical intermediates using boron trifluoride acetonitrile complex as a catalyst). , adjust the pH to 6.0 to obtain the intermediate crystallization solution, centrifuge to obtain the intermediate wet product, and further refine and process; the centrifugal filtrate mainly contains sodium fluoroborate solution, add 200-300 mL of saturated potassium chloride solution, and keep the temperature at 20 ℃ Next, the potassium fluoroborate granular solid is crystallized under stirring, and the crystallization time is controlled to be no less than 60 minutes, and then centrifuged, and 200 mL of deionized water alternately washes the potassium fluoroborate crystals multiple times to obtain potassium fluoroborate wet solids, which are transferred to ...

Embodiment 2

[0033] Under the condition of constant stirring, control the reaction temperature at 40 ° C, add 1 mol / L sodium carbonate passivator to the 2000 L pharmaceutical intermediate reaction final solution system, adjust the pH to 6.5-7, add 200 L of saturated potassium chloride solution to obtain The intermediate crystal solution is centrifuged to obtain the intermediate wet product, which is further refined and processed; the centrifuge filtrate mainly contains sodium fluoroborate solution, and the potassium fluoroborate crystals are alternately washed with 200L deionized water, and then sent to the fluidized bed oxidation by an automatic screw machine Impurity removal reactor, through enzymatic hydrolysis and oxidation technology, add 10g compound enzyme solution (Ganoderma lucidase laccase: cyanohydrolase: bromoperoxidase = 1:2:1, compound enzyme activity 20000-50000IU), reaction control 20-30°C, reaction time 2h, 2L hydrogen peroxide (added in two stages, the first stage is enzym...

Embodiment 3

[0038] A purification device for by-product potassium fluoroborate in the synthesis of pharmaceutical intermediates, comprising a primary treatment system and a secondary purification system, the discharge port of the primary treatment system is connected with the feed port of the secondary purification system, and the primary treatment system is connected with the feed port of the secondary purification system. The primary treatment system is used for crystallization and primary centrifugal treatment, and the secondary refining system is used for enzymatic hydrolysis, oxidation and secondary centrifugal treatment. The primary treatment system includes a crystallization tank and a primary centrifuge.

[0039] like image 3 As shown, the secondary refining system includes a potassium fluoroborate silo 1, the outlet of the potassium fluoroborate silo is connected with the feed port of the fluidized bed impurity removal reactor 2, and the fluidized bed impurity removal The air i...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of pharmaceutical synthesis wastewater treatment, and in particular relates to a method and a device for purifying by-product potassium fluoroborate in the synthesis of pharmaceutical intermediates. Saturated KCL aqueous solution is added to the mother liquor to generate a mixed aqueous solution of potassium fluoroborate crystals, and the filter cake is washed with deionized water to obtain the first-grade purified product of potassium fluoroborate, and then the first-grade purified potassium fluoroborate is transferred to the potassium fluoroborate refining tank , add deionized water to soak, stir and wash, add high-selectivity, high-activity compound enzyme preparation and hydrogen peroxide for enzymatic hydrolysis and oxidation, and then separate, dehydrate by a secondary centrifuge, continuously wash with deionized water, and spin dry to obtain fluorine Potassium borate refined product. The application of the method and device can by-produce potassium fluoroborate refined products, effectively reuse fluorine-containing compounds, reduce pollution disposal and consumption of natural fluorine resources, reduce carbon emissions, and have important social and economic benefits.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis wastewater treatment, and in particular relates to a method and a device for purifying by-product potassium fluoroborate in the synthesis of pharmaceutical intermediates. Background technique [0002] Boron trifluoride-acetonitrile complex (molecular formula BF 3 -CH 3 CN) is a highly active catalyst, which is widely used in the production process of pharmaceutical intermediates such as zoline and cefpiramide. The catalytic activity of the complex is mainly achieved by adding an alkaline solution to the reaction system to turn boron trifluoride into a sodium fluoroborate solution. Pharmaceutical companies usually convert sodium fluoroborate into potassium fluoroborate, so that potassium fluoroborate is crystallized. It is separated from the mother liquor. Since the obtained potassium fluoroborate usually contains unreacted organic matter, cyanide, fluoroboric acid and other toxi...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & AuthorityPatents(China)
IPC IPC(8): C01B35/06B01J8/38
CPCC01B35/066B01J8/386Y02W10/37
Inventor杨云军张庆建
OwnerQILU UNIV OF TECH