Preparation of boron trifluoride and sulfuric acid from boron trifluoride hydrate

A technology of boron trifluoride and hydrate, applied in the direction of boron halide compounds, sulfur trioxide/sulfuric acid, sulfur compounds, etc.

Inactive Publication Date: 2003-09-17
ELF ATOCHEM SA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, the sulfuric acid obtained from this treatment is yellow or b

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A setup consisting of two reactors in series was used. The first reactor has a volume of 400 ml (200 ml is the effective volume of the reaction medium) and is equipped with a helical stirrer (4 blades) with a diameter of 4 cm; the rotational speed of the stirrer head is 500 revolutions per minute. The temperature was maintained at 104-107°C in order to extract the heat of reaction and the reactor was jacketed with a heat transfer fluid flow.

[0039] Continuous weighing of two reactants - Industrial BF 3 Hydrate and 65% oleum were added to the reactor which initially contained 200 ml of 100% sulfuric acid. Industrial BF powered by peristaltic pumps 3 The hydrate and the fuming sulfuric acid provided by the piston metering pump enter the reaction medium through two dip tubes installed side by side. The overflow of this reactor flows to a second reactor having the same characteristics (volume, agitation, etc.) as the first reactor. Industrial BF 3 Hydrates have the f...

Embodiment 2

[0050] Example 2 (Compared)

[0051] The same procedure as in Example 1 was followed except that no hydrogen peroxide was added to the second reactor. BF recovered in the first reactor 3 Has commodity BF 3 characteristics (organic carbon content less than 5 mg / kg BF 3 , did not detect any trace CO 2 ), but the sulfuric acid discharged from the second reactor was black and contained 20 mg organic carbon / kg H 2 SO 4 .

Embodiment 3

[0052] Example 3 :(Compared)

[0053] Use an industrial BF with the following characteristics 3 Hydrate:

[0054] BF 3 =47.7%

[0055] h 2 O = 52.3%

[0056] Density = 1.38

[0057] Organic carbon content: 620 mg / kg industrial BF 3 Hydrate Repeat the method of Example 2.

[0058] Industrial BF 3 The feed rate of hydrate was 188 g / hour and the feed rate of oleum was 681 g / hour. The residual sulfuric acid flow from the second reactor overflow was 784 g / h. Before blowing off the sulfuric acid, BF 3 The mass concentration is 1.3%. blowing off BF with air 3 After that, the sulfuric acid concentration was 98.4% H 2 SO 4 and 1.6% H 2 O.

[0059] BF released is recovered in a trap at the top of the first reactor 3 , analyzing the BF trapped with water 3 , to determine its organic and inorganic carbon (CO 2 ) content; it per kilogram BF 3 contains less than 10 mg of organic carbon.

[0060] The sulfuric acid recovered in the overflow of the second reactor co...

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PUM

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Abstract

The present invention relates to the preparation of commercial grade BF from boron trifluoride hydrate waste liquor containing organic impurities 3 and H 2 SO 4 . The method mainly consists in reacting the waste liquid with oleum, recovering the boron trifluoride gas released thereby, treating with hydrogen peroxide and blowing off sulfuric acid by-products with air.

Description

technical field [0001] The invention relates to the fields of boron trifluoride and sulfuric acid, and more particularly relates to converting industrial waste liquid of boron trifluoride hydrate into boron trifluoride and sulfuric acid. Background technique [0002] Boron trifluoride is a gas mainly used industrially as a catalyst in a large number of reactions: polymerization, esterification, alkylation and isomerization. Usually, after boron trifluoride is used, it is treated with an aqueous sodium hydroxide solution, and the waste liquid thus obtained consisting of fluorine-containing boron derivatives is discharged. [0003] In order to avoid discharging these fluorine-containing boron wastes, boron trifluoride can be converted to BF at the end of the reaction after use 3 to be recovered in the form of hydrate solution, the BF 3 On the one hand, the hydrate solution can be obtained by BF 3 obtained by contact with water, on the other hand washed with water in BF 3 o...

Claims

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Application Information

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IPC IPC(8): B01J27/12C01B35/06C02F1/40C08F4/06C01B17/74C01B17/90
CPCC01B17/74C01B17/905C01B35/061B01J19/18B01J2219/0059
Inventor J·-P·沙利厄克斯C·普拉卢斯
Owner ELF ATOCHEM SA
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