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Oxa perfluorocarboxylic acid dipentaerythritol ester and preparation and application thereof

A technology of dipentaerythritol ester and dipentaerythritol, which is applied in the field of dipentaerythritol oxaperfluorocarboxylate and its preparation and application, and achieves the effects of simple preparation method, high surface activity and broad application prospects

Active Publication Date: 2014-02-05
菏泽奕普新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But take dipentaerythritol as raw material, carry out esterification reaction with hexafluoropropylene oxide oligomer, make the fluorocarbon surfactant of oxa perfluorocarboxylic acid dipentaerythritol ester mixture and also have no report

Method used

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  • Oxa perfluorocarboxylic acid dipentaerythritol ester and preparation and application thereof
  • Oxa perfluorocarboxylic acid dipentaerythritol ester and preparation and application thereof
  • Oxa perfluorocarboxylic acid dipentaerythritol ester and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Equipped with a stirrer, a thermometer, a dropping funnel and a reflux condenser (an anhydrous CaCl 2 Drying tube) In a dry 250mL four-necked flask, add 5.08g (0.02mol) of dipentaerythritol, 25mL of DMF, and 4.1g (0.04mol) of triethylamine. Stir, heat to 55°C, add 15.54g (0.04mol) hexafluoropropylene oxide oligomer mixture (HFPO) dropwise while stirring n . After the dropwise addition was completed, the temperature was continued to rise to 80°C, and the reaction was stirred for 8h. The resulting product was first washed twice with 25mL5%HCl solution, and then washed with 50mL5%NaHCO 3 The solution was washed once, extracted with 25mL ether after washing with water, and the upper organic layer was obtained by liquid separation, and the solvent was distilled off under reduced pressure to obtain a light yellow solid with a yield of 76.1% (based on hexafluoropropylene oxide oligomer mixture) .

[0031] FTIR analysis: 3300cm -1 ~3500cm -1 (residual O-H stretching vibra...

Embodiment 2

[0034] The experimental method is the same as in Example 1, however, the 15.54 g hexafluoropropylene oxide oligomer mixture is changed to 13.28 g (0.04 mol) hexafluoropropylene oxide dimer. The yield was 72.0% (based on hexafluoropropylene oxide dimer).

Embodiment 3

[0036] The experimental method is the same as in Example 1, but the 15.54 g hexafluoropropylene oxide oligomer mixture is changed to 19.92 g (0.04 mol) hexafluoropropylene oxide trimer. The yield was 77.8% (based on hexafluoropropylene oxide trimer).

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Abstract

The invention discloses oxa perfluorocarboxylic acid dipentaerythritol ester and preparation and application thereof. The oxa perfluorocarboxylic acid dipentaerythritol ester is one compound shown as a structural formula (I) or is a mixture of two or more compounds shown as the structural formula (I), in the structural formula (I), R<1>, R<2>, R<3>, R<4>, R<5> and R<6> are respectively and independently H or F(CF3CFCF2O)nCF(CF3)CO-, n is a natural number, and R<1>, R<2>, R<3>, R<4>, R<5> and R<6> are not all H. A synthetic method of the oxa perfluorocarboxylic acid dipentaerythritol ester is shown as the following reaction equations (in the specification). The invention also provides the application of the oxa perfluorocarboxylic acid dipentaerythritol ester as a surfactant, and the oxa perfluorocarboxylic acid dipentaerythritol ester is high in surface activity, can be directly used as a fluorocarbon surfactant, and can be widely used in the fields of brightening agents, waterproof and oilproof agents of fiber fabrics including leather and paper, waterproof and oilproof agents of hard surfaces, and the like.

Description

(1) Technical field [0001] The invention relates to dipentaerythritol oxaperfluorocarboxylate, a preparation method thereof and an application as a surfactant. (2) Background technology [0002] Fluorocarbon surfactants have "three highs" and "two rejections" properties, namely high surface activity, high heat resistance, high chemical resistance and water and oil repellency [Fluorocarbon surfactants, Beijing: Chemical Industry Press, 2001], and thus received widespread attention. Since the 1950's, research on fluorocarbon surfactants has been in the ascendant, and it is used in fabrics and papers [Fluorinated surfactants and their applications. Hangzhou Chemical Industry, 2001, 31 (2): 6-10.] and leather waterproof and oil-proof [Synthesis and application of fluorosurfactant [J]. Leather and Chemical Industry, 2008, 25(1): 25-28.], AFFF fire extinguishing agent [Fluorocarbon surfactant and AFFF fire extinguishing agent Chemical Research and Application, 2002,14(4):391-393...

Claims

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Application Information

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IPC IPC(8): C07C67/14C07C69/708B01F17/44B01F17/38C09K23/38C09K23/44
CPCC07C67/14C07C69/708C09K23/007
Inventor 史鸿鑫沈海民魏文俊
Owner 菏泽奕普新材料有限公司
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