Method for preparing perfluoroelastomers

一种单体、氟甲酸酯的技术，应用在全氟弹性体领域，能够解决机械性能未改进等问题，达到改进机械和压缩永久变形性能的效果

Active Publication Date: 2011-01-19
SOLVAY SOLEXIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However the mechanical properties were not improved after this treatment, so they did not solve the technical problem of providing perfluoroelastomers with an improved combination of mechanical and compression set properties over a wide temperature range, at high and low temperatures

Method used

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  • Method for preparing perfluoroelastomers
  • Method for preparing perfluoroelastomers
  • Method for preparing perfluoroelastomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0184] Analytical method

[0185] Determination of polymer Tg

[0186] Tg is determined by DSC analysis according to ASTM D 3418 method. Tg values ​​reported in the examples are midpoint Tg.

[0187] Determination of intrinsic viscosity

[0188] Intrinsic viscosity was measured in perfluoroheptane at a temperature of 30°C.

[0189] -Determination of polar end groups of COF

[0190] At the end of the polymerization, the polymer was isolated from coagulation by freezing at -20° C. and subsequently defrosting at room temperature until a slurry was obtained in which the polymer settled at the bottom; it was washed twice with demineralized water and heated in an oven at 90 Dry at °C until constant weight (about 12 hours); by using Nexus FT-IR equipment (256 scans, resolution 2cm -1 )-COF end groups determined by FT-IR spectroscopy, where first 4000 cm -1 and 400cm -1 between scans, the film was then kept for 12 hours in an environment saturated with ammonia vapor, a...

Embodiment A

[0200] Preparation of CF in a glass reactor by thermal reaction at 170 °C 3 OCOF

[0201] A tubular glass reactor with an internal diameter of 55.6 mm, a length of 510 mm, filled with 6x6 glass Raschig rings (free internal volume 842 ml), thermostatted by an electric resistance was used.

[0202] Simultaneously the CF synthesized as described in USP 4400872 3 OF flow (1.5 L / h) and CO flow (1.5 L / h) were fed into the reactor maintained at 170°C for 5 hours. The stream from the reactor was continuously analyzed by on-line gas chromatographic analysis.

[0203] The stream from the reactor except CO was condensed in a trap kept at -110 °C containing 15 g CFCl=CFCl (A 1112) such that residual CF 3 Reaction of OF with alkenes to give CF 3 OCFClCF 2 Cl.

[0204] After fractional distillation of the resulting mixture, 33.9 g of 99.8% pure CF were obtained 3 OCOF (for feed CF 3 The molar yield of OF 76.5%), the CF of 12.3g 3 OCFClCF 2 Cl, 3.4 g COF 2 .

[0205] relative fee...

Embodiment B

[0207] Preparation of CF in a PTFE reactor by thermal reaction at 170 °C 3 OCOF

[0208] A PTFE tubular thermostatic reactor with an inner diameter of 4 mm and a length of 13.2 m was used.

[0209] CF 3 OF gas flow (1.5 liters / hour) and CO flow (2.0 liters / hour) were fed into the reactor maintained at 170°C.

[0210]The stream from the reactor was analyzed by gas chromatography to have the following molar composition: 7.3% CF 3 OF, 54.2% CF 3 OCOF, 9.1% COF 2 and 29.4% CO.

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Abstract

The invention relates to a method of preparing perfluoroelastomers. Perfluoroelastomers curable by peroxidic way having glass transition temperature lower than -10 DEG C. and an amount of -COF end groups in the polymer lower than the sensitivity limit of the method using the IR spectroscopy in Fourier transform described in the present application.

Description

[0001] This application is a divisional application of an application with a filing date of August 1, 2005, an application number of 200510087886.9, and an invention title of "perfluoroelastomer". [0002] Specification of an industrial invention in the name of SOLVAY SOLEXISS.p.A. of Italian nationality, headquartered in Milano, via Turati 12. technical field [0003] The present invention relates to perfluoroelastomers having a Tg (glass transition temperature) below -10°C and an improved combination of mechanical and compression set properties over a wide temperature range, at high and low temperatures. [0004] More specifically, the present invention relates to perfluoroelastomers having a Tg below -10°C and having substantially no -COF end groups which are not detectable by the methods described below. The perfluoroelastomers of the present invention show improved molecular weight as shown by improved intrinsic viscosity and are obtainable by a polymerization process wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/313C07C41/48
CPCC08F14/18C08F2/02C08F6/00C08F6/10C08F291/02
Inventor M·阿波斯托洛F·特留尔兹V·托尔特利M·加林贝蒂
Owner SOLVAY SOLEXIS
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