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Method for producing a composition containing a perfluoropolyether compound containing a hydroxyl group at one end and a method for increasing the content of the compound

A technology of perfluoropolyether and its manufacturing method, which is applied in the direction of chemical instruments and methods, separation methods, chemical/physical processes, etc., to achieve the effect of reducing the amount of use and the impact of environmental load

Active Publication Date: 2018-07-06
SHIN ETSU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the case of this method, a large amount of non-functional polymers are also produced at the same time

Method used

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  • Method for producing a composition containing a perfluoropolyether compound containing a hydroxyl group at one end and a method for increasing the content of the compound
  • Method for producing a composition containing a perfluoropolyether compound containing a hydroxyl group at one end and a method for increasing the content of the compound
  • Method for producing a composition containing a perfluoropolyether compound containing a hydroxyl group at one end and a method for increasing the content of the compound

Examples

Experimental program
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Effect test

Embodiment 1

[0134] Make 10g of composition F60 in supercritical carbon dioxide as mobile phase, and filled with silica gel 60-NH 2 (manufactured by Kanto Chemical Co., Ltd., particle size: 40 μm to 50 μm, weakly alkaline: pH 9.5 (25° C., value in the state of 10% by weight aqueous suspension), dry-filled) in a 25 mL high-pressure vessel. The flow rate of the mobile phase was 5ml / min, and the temperature was 40°C. Change the pressure from 11MPa to 25MPa. In detail, first flow carbon dioxide adjusted to a supercritical state at 40°C and 11 MPa, fractionate components for 60 minutes at a mobile phase pressure of 11 MPa, then set the mobile phase pressure to 15 MPa and fractionate The components were separated for 60 minutes, then the pressure of the mobile phase was set to 25 MPa and the components were fractionated for 60 minutes. The ratio of the components contained in each component is shown in Table 2 below. The composition ratio is utilized 19 F-NMR to confirm.

[0135] [Table 2] ...

Embodiment 2

[0138] Make 10g of composition F70 in supercritical carbon dioxide as mobile phase, and filled with silica gel 60-NH 2 (manufactured by Kanto Chemical Co., Ltd., particle size: 40 μm to 50 μm, weakly alkaline: pH 9.5 (25° C., value in the state of 10% by weight aqueous suspension), dry-filled) in a 25 mL high-pressure vessel. The flow rate of the mobile phase was 5ml / min, and the temperature was 40°C. Change the pressure from 11MPa to 25MPa. Specifically, first, carbon dioxide adjusted to a supercritical state was passed through at 40° C. and 11 MPa, fractionated for 60 minutes at a mobile phase pressure of 11 MPa, and then the mobile phase pressure was set to 15 MPa and separated. The components were taken for 60 minutes, then the pressure of the mobile phase was set to 25 MPa and the components were taken for 60 minutes. The ratio of the components contained in each component is shown in Table 3 below. The composition ratio is utilized 19 F-NMR to confirm. In addition, ...

Embodiment 3

[0142] Make 10g of composition F80 in supercritical carbon dioxide as mobile phase, and filled with silica gel 60-NH 2 (manufactured by Kanto Chemical Co., Ltd., particle size: 40 μm to 50 μm, weakly alkaline: pH 9.5 (25° C., value in the state of 10% by weight aqueous suspension), dry-filled) in a 25 mL high-pressure vessel. The flow rate of the mobile phase was 5ml / min, and the temperature was 40°C. Change the pressure from 11MPa to 25MPa. In detail, first flow carbon dioxide adjusted to a supercritical state at 40°C and 11 MPa, fractionate components for 60 minutes at a mobile phase pressure of 11 MPa, then set the mobile phase pressure to 15 MPa and fractionate The components were separated for 60 minutes, then the pressure of the mobile phase was set to 25 MPa and the components were fractionated for 60 minutes. The ratio of the components contained in each component is shown in Table 4 below. The composition ratio is utilized 19 F-NMR to confirm. In addition, the co...

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Abstract

The present invention provides a method for producing a composition containing a single-terminal hydroxyl-containing perfluoropolyether compound at a high concentration with high efficiency and high selectivity. The present invention provides a method for increasing the content rate of a perfluoropolyether compound containing a hydroxyl group at a single terminal, which increases the content rate of a perfluoropolyether compound containing a hydroxyl group at a single terminal through the following steps: For perfluoropolyether compounds containing a hydroxyl group at a single terminal The composition of the fluoropolyether compound and the perfluoropolyether compound containing hydroxyl groups at both ends is used for chromatographic analysis using supercritical or subcritical carbon dioxide as the mobile phase and silica gel as the stationary phase. At this time, the mobile phase is set Determined to be in a state of a temperature (T) between 25°C and below 150°C and a pressure (P) between 7MPa and below 30MPa, carry out chromatographic analysis, and fractionate the single-terminal hydroxyl-containing compound at a high concentration. Procedure for components of perfluoropolyether compounds.

Description

technical field [0001] The present invention relates to a method for producing a composition containing a single-terminal hydroxyl-containing perfluoropolyether compound at a high concentration and a method for increasing the content of the compound. Background technique [0002] Perfluoropolyether compounds having functional groups at one end (hereinafter referred to as single-terminal derivatives), or perfluoropolyether compounds having functional groups at both ends (hereinafter referred to as both-terminal derivatives) (hereinafter collectively referred to as Functional polymers) are often used as precursors for various derivatives such as surfactants or surface treatment agents. For example, precursors of surfactants useful for polymerization of polymers include acrylic acid derivatives, amine derivatives, and isocyanate derivatives of the above-mentioned functional polymers. In addition, examples of the precursor of the surface treatment agent include alkoxy derivativ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/08C08G65/00
CPCC08G65/007C08G65/30C08G65/46B01D15/12Y02P20/54C08L71/00
Inventor 山根祐治松田高至小池则之
Owner SHIN ETSU CHEM CO LTD