Method of removing and recovering boron trifluoride with metal fluoride and process for polyolefin production using the same

A technology of boron trifluoride and fluoride, applied in chemical instruments and methods, separation methods, chemical/physical processes, etc.

Inactive Publication Date: 2001-03-28
NIPPON PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, none of the currently proposed schemes is economical and environmentally friendly to recover reusable boron trifluoride

Method used

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  • Method of removing and recovering boron trifluoride with metal fluoride and process for polyolefin production using the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0193] (Absorptive removal of boron trifluoride)

[0194] Under nitrogen flow, 100 g of the dispersion liquid (boron trifluoride 0.25% (weight)) that boron trifluoride diethyl ether complex is dispersed in hexane is put into the Erlenmeyer flask with stirrer, at a constant temperature of 25 ℃ and While maintaining stirring, 1.91 g (equivalent to 20 times the mole of boron trifluoride) of a commercially available special-grade reagent lithium fluoride (purity 99% or more, manufactured by Soegawa Rika Co., Ltd.) was added, and stirred for 30 minutes under nitrogen flow.

[0195] Stop stirring, let the reaction solution stand still, use the difference in specific gravity to separate the adsorbent and the organic liquid into two phases, and separate the organic phase into another container by decantation. An aqueous solution of calcium chloride was added to the above-mentioned organic phase, and the concentration of boron trifluoride remaining in the organic phase was measured by ...

Embodiment 2

[0205] (Absorptive removal of boron trifluoride)

[0206] 18.00 g (694 mmol) of lithium fluoride used in Example 1 was filled in a stainless steel tubular container with a diameter of 20 mm and a length of 200 mm. The above-mentioned tube was kept at a constant temperature of 25° C., and in the same manner as in Example 1, a dispersion solution in which boron trifluoride diethyl ether complex was dispersed in hexane was supplied at a constant flow rate of 10 ml / hour (boron trifluoride 16.5 mg / hour). Liquid (boron trifluoride 0.25% (weight)). The concentration of boron trifluoride in the outlet fluid is 0, indicating that boron trifluoride has been completely removed by adsorption.

[0207] The adsorption operation was continued, and 120 hours after the supply of the dispersion solution was started, the supply of the dispersion solution was stopped when a trace amount of boron trifluoride was detected from the outlet fluid. After the supply of the dispersion solution was stop...

Embodiment 3

[0214] The boron trifluoride diethyl ether complex used in Example 1 is changed into a boron trifluoride phenoxide complex, and the dispersion liquid (boron trifluoride 0.25% (weight)) that is dispersed in hexane is used, Other than that, the adsorption and desorption tests of boron trifluoride were carried out in the same manner as in Example 1, and the results are shown in Table 1.

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Abstract

Boron trifluoride can be recovered in a reusable state by a method that is economical and does not cause environmental pollution, which method comprises the steps of bringing a fluid containing boron trifluoride or its complex into contact with metal fluoride so as to selectively adsorb and remove boron trifluoride in the complex and heating the resultant metal tetrafluoroborate at a temperature in the range of 100 to 600 DEG C to separate it into boron trifluoride and metal fluoride. By applying the method to a process for producing polybutene or olefin oligomer using boron trifluoride complex catalyst, the catalyst can be recovered with retaining its activity and reused effectively.

Description

technical field [0001] The present invention relates to a method for selectively separating and removing boron trifluoride from a fluid containing boron trifluoride or its coordination compound and a method for recovering the boron trifluoride. [0002] In addition, the present invention also relates to a method for producing polyolefin using a boron trifluoride-based complex catalyst composed of boron trifluoride and a complexing agent as a polymerization catalyst. That is, the present invention relates to a method for removing boron trifluoride in a complex catalyst and recovering a complexing agent by contacting a polymer product obtained by polymerizing olefins, including polybutene or olefin oligomers, with metal fluorides , and heat the generated tetrafluoroborate metal salt, separate it into metal fluorides and boron trifluoride gas, and re-prepare the boron trifluoride-based coordination compound catalyst from the recovered boron trifluoride and complexing agent for re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/00B01D15/08C08F2/00C08F4/14C08F6/08C08F10/00C08F10/08C08F10/14
CPCC08F6/02B01J20/046C08F110/10C08F110/14B01D15/08C08F4/14B01D15/00C08L23/22C08F110/08C08F2/04
Inventor 高屿务德本祐一藤村耕治
Owner NIPPON PETROCHEMICAL CO LTD
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