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Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound

A technology of dimethyl carbonate and boron trifluoride, which is applied in the field of low-temperature preparation of boron trifluoride dimethyl carbonate complex, can solve the problems of high risk, high energy consumption, etc. Reaction temperature, safe and controllable effect of production process

Inactive Publication Date: 2013-04-17
SHANDONG HEYI GAS CO LTD DONGYING CITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that both the gas-making reaction and the complexation reaction need to be carried out at a relatively high temperature, the energy consumption is large and the risk is high. In order to overcome the above shortcomings, a boron trifluoride dimethyl carbonate complex is provided. Low temperature preparation method of compound

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add sulfur trioxide, boric acid, and anhydrous hydrofluoric acid into the gas generator at a weight ratio of 4:1:1, and react at 18°C ​​for 15 hours. The vacuum pump evacuates the boron trifluoride gas, The degree of vacuum is 0.07MPa.

[0025] The derived boron trifluoride gas enters the purification tank filled with 85% concentrated sulfuric acid for purification, and the gauge pressure of the purification tank is 0.2MPa.

[0026] The purified boron trifluoride gas enters the complexing kettle, which is filled with dimethyl carbonate, and the mass ratio of the filling amount of dimethyl carbonate to the boron trifluoride gas produced by each kettle in the gas making kettle is 6 : 3, the complexation reaction temperature is 20°C, and the reaction time is 4 hours.

[0027] The complexation reaction liquid circulates in the complexation tank and the filter, the temperature of the filter is 8°C lower than the temperature of the complexation tank, and the reaction liquid ...

Embodiment 2

[0036] Add sulfur trioxide, boric acid, and anhydrous hydrofluoric acid into the gas generator at a mass ratio of 8:1:1, and react at 30° C. for 8 hours to generate boron trifluoride gas. The vacuum pump evacuates the boron trifluoride gas, and the vacuum degree is 0.08MPa.

[0037] The exported boron trifluoride gas enters the purification tank filled with concentrated sulfuric acid with a concentration of 93% for purification, and the gauge pressure of the purification tank is 0.4MPa.

[0038] The purified boron trifluoride gas enters the complexing kettle, which is filled with dimethyl carbonate, and the mass ratio of the filling amount of dimethyl carbonate to the boron trifluoride gas produced by each kettle in the gas making kettle is 6 : 4, the complexation reaction temperature is 30 DEG C, and the reaction time is 8 hours.

[0039] The filter temperature is 10° C. lower than the complexation reaction temperature, and the rest refer to Example 1. The product is a whit...

Embodiment 3

[0041] Add sulfur trioxide, boric acid, and anhydrous hydrofluoric acid into the gas generator at a weight ratio of 12:2:3, and react at 48° C. for 4 hours to generate boron trifluoride gas. The vacuum pump pumps out the boron trifluoride gas with a vacuum degree of 0.098MPa.

[0042] The exported boron trifluoride gas enters the purification tank filled with 98% concentrated sulfuric acid for purification, and the gauge pressure of the purification tank is 0.5MPa.

[0043] The purified boron trifluoride gas enters the complexing kettle, which is filled with dimethyl carbonate, and the mass ratio of the filling amount of dimethyl carbonate to the boron trifluoride gas produced by each kettle in the gas making kettle is 6 : 6, the complexation reaction temperature is 40 DEG C, and the reaction time is 12 hours.

[0044] The filter temperature is 15° C. lower than the complexation reaction temperature, and the rest refer to Example 1. The product is a white crystal with a boro...

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PUM

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Abstract

The invention belongs to a chemical engineering product, a boron trifluoride dimethyl carbonate complex compound, in particular relates to a low temperature preparation method of the boron trifluoride dimethyl carbonate complex compound. The preparation method comprises the following steps: in a gas generating container, using boric acid and anhydrous hydrofluoric acid as raw materials, dehydrating and generating boron trifluoride gas, and sulfur trioxide is used as an dehydrating agent; in a purification container, purifying the boron trifluoride gas generated through concentrated sulphuric acid; in a complexing container, performing a complexing reaction of the purified boron trifluoride gas and the dimethyl carbonate; and in a filter, cooling down and crystallizing the liquid reactant of the complexing reaction, and the solid gathered is the boron trifluoride dimethyl carbonate complex compound. The technical scheme provided by the invention enables the temperature of the gas generating reaction and complexing reaction to be close to the room temperature, decreases energy consumption during production process and is low-carbon and environment friendly; the production process is safer and more controllable; and the boron trifluoride dimethyl carbonate complex compound is a solid white crystal, wherein the content of boron trifluoride is 40-43 percent in weight and the property of the boron trifluoride is stable.

Description

technical field [0001] The invention belongs to chemical product boron trifluoride dimethyl carbonate complex, in particular to a low-temperature preparation method of boron trifluoride dimethyl carbonate complex. Background technique [0002] Boron trifluoride complex is a very active catalyst, which can be used in various organic synthesis reactions, especially in the synthesis process of cephalosporin antibacterial drugs, because the introduction of boron trifluoride complex shortens the The reaction time of the original product greatly increases the yield of the original product. The boron trifluoride dimethyl carbonate complex is currently the most effective catalyst in the chemical synthesis process of cephalosporins modified at the C3 position, and is safe and convenient to use and has no pollution to the environment. [0003] The production process of boron trifluoride dimethyl carbonate complex is at present: [0004] Sulfuric acid, boric acid and hydrofluoric aci...

Claims

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Application Information

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IPC IPC(8): C07F5/02
Inventor 刘喜民于景东张斌周士蒿孙刚强马西胜
Owner SHANDONG HEYI GAS CO LTD DONGYING CITY
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