Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for producing fluorine-containing ether with high purity

A manufacturing method and technology of fluorine-containing ethers, which are applied in the field of manufacture of fluorine-containing ethers, and can solve problems such as inability to separate fluorine-containing alkyl alcohols and increase in the number of processes

Active Publication Date: 2012-11-28
DAIKIN IND LTD
View PDF16 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, in addition to being unable to separate the fluorine-containing alkyl alcohol, light and high temperature are required, so in addition to requiring equipment such as a high-pressure mercury lamp, there is also a problem that the number of steps will increase.

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 for producing fluorine-containing ether with high purity
  • Method for producing fluorine-containing ether with high purity
  • Method for producing fluorine-containing ether with high purity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0078] Next, the present invention will be described based on examples and comparative examples, but the present invention is not limited to the examples.

[0079] In addition, the measuring method used in this invention is as follows.

[0080] (1) Composition analysis

[0081] NMR method: AC-300 manufactured by BRUKER was used.

[0082] 19 F-NMR:

[0083] Measuring conditions: 282MHz (trichlorofluoromethane = 0ppm)

[0084] 1 H-NMR:

[0085] Measuring conditions: 300MHz (tetramethylsilane = 0ppm)

[0086] (2) Concentration (GC%) analysis

[0087] Gel chromatography (GC) method: GC-17A manufactured by Shimadzu Corporation was used. Column: DB624 (Length 60, I.D 0.32, Film 1.8 μm). Determination limit: 0.001%

[0088] (3) Moisture content (mass % or ppm)

[0089] Karl Fischer method: MKC-501 manufactured by Kyoto Denshi Kogyo Co., Ltd. was used. Catholyte: Aquamicron CXU manufactured by Mitsubishi Chemical Co., Ltd. Anolyte: Aquamicron AKX manufactured by Mitsubishi...

Synthetic example 1

[0090] Synthesis Example 1 (Manufacture of Fluorinated Ether Crude Liquid)

[0091] The inside of the 6L autoclave made of stainless steel was vacuumed, and 401 g of potassium hydroxide (7.15 mol. The ratio to 1 mole of fluorine-containing alkyl alcohol was 0.55 mole), water (1604 mL), and fluorine-containing 2,2,3,3-tetrafluoro-1-propanol (boiling point: 109°C, specific gravity: 1.4) of alkyl alcohol: HCF 2 CF 2 CH2 OH (1716 g, 13 mol), followed by 20 vacuum-nitrogen displacements at room temperature. After vacuuming the inside of the system, tetrafluoroethylene was filled so that the pressure was 0.1 MPa, and heating was performed so that the inside of the reaction system was 85°C. After the internal temperature reached 85° C., tetrafluoroethylene was added little by little to keep the reaction pressure at 0.5 MPa to 0.8 MPa. Adjust the internal temperature of the system to keep it at 75°C to 95°C.

[0092] When the amount of tetrafluoroethylene added reached 0.5 mole re...

Synthetic example 2

[0095] A fluorine-containing ether was synthesized in the same manner as in Synthesis Example 1 except that the added amount of tetrafluoroethylene was changed to 780 g (7.8 mol). Table 1 shows the composition of the obtained fluorine-containing ether production liquid.

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

PropertyMeasurementUnit
boiling pointaaaaaaaaaa
boiling pointaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for producing a fluorine-containing ether with a high purity that has a largely reduced fluorine-containing alkyl alcohol concentration. This method, which can be efficiently carried out and is suitable for scale-up, is characterized by comprising subjecting a crude fluorine-containing ether solution, which contains a fluorine-containing alkyl alcohol as an impurity, to countercurrent extraction using water.

Description

technical field [0001] The present invention relates to a method for producing fluorine-containing ethers with high purity by an easy purification method. Background technique [0002] As a method for synthesizing fluorine-containing ethers, a method of reacting a fluorine-containing alkyl alcohol with a fluorinated olefin in the presence of a basic compound such as an alkali metal compound is known (Patent Documents 1 to 6). However, a small amount of fluorine-containing alkyl alcohol as a raw material and by-products remain in the reaction product of these reactions (crude fluorine-containing ether reaction liquid). [0003] Separation (purification) of impurities (especially fluorine-containing alkyl alcohols) from fluorine-containing ether reaction crude liquid is carried out by, for example, washing with water, distillation (rectification or simple distillation) or a combination thereof, but the above-mentioned patent documents roughly According to calculation, it can ...

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 & Authority Applications(China)
IPC IPC(8): C07C41/05C07C41/58C07C43/12C07B61/00
CPCC07C41/38Y02P20/582C07C43/123C07B61/00C07C41/05C07C41/58C07C43/12
Inventor 贺川米基璐中园葵仙波靖英本山均吉沢透高明天
Owner DAIKIN IND LTD