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Fluoroelastomers

An elastomer, monomer technology, applied in the field of VDF-based fluoroelastomers, can solve problems such as poor productivity, and achieve the effect of improving mechanical and compression set properties

Active Publication Date: 2006-02-01
SOLVAY SOLEXIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From an industrial point of view this means a disadvantage due to poor productivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0163] The preparation of adducts is described in European patent application EP 684277 in the name of the applicant, which is hereby incorporated by reference.

[0164] The blend for ion curing additionally contains:

[0165] i) One or more inorganic acid acceptors selected from those known in the ionic curing of vinylidene fluoride copolymers, in an amount of 1-40 parts per 100 parts of fluoroelastomer copolymer;

[0166] ii) One or more basic compounds selected from those known in the ionic curing of vinylidene fluoride copolymers, in an amount of 0.5-10 parts per 100 parts of the fluoroelastomer copolymer.

[0167] The basic compound of point ii) is usually selected from Ca(OH) 2 , Sr(OH) 2 , Ba(OH) 2 , Weak acid metal salts, such as carbonates, benzoates, oxalates and phosphites of Ca, Sr, Ba, Na and K, and mixtures of the above-mentioned hydroxides and the above-mentioned metal salts; compounds of type i) MgO can be mentioned in.

[0168] The stated amounts of compounding co...

Embodiment

[0197] Analytical method

[0198] Determination of polymer Tg

[0199] Tg is determined by DSC analysis according to ASTM D 3418 method. The Tg value reported in the examples is the midpoint Tg.

[0200] Determination of intrinsic viscosity

[0201] The intrinsic viscosity was measured in perfluoroheptane at a temperature of 30°C.

[0202] -COF Determination of polar end groups

[0203] At the end of the polymerization, the polymer is separated by coagulation by freezing at -20°C and then defrosting at room temperature until a slurry in which the polymer is deposited at the bottom is obtained; it is washed twice with demineralized water and heated at 90°C in an oven. Dry at ℃ until constant weight (about 12 hours); by using Nicolet  Nexus FT-IR device (256 scans, 2cm resolution -1 ) Determination of -COF end groups by FT-IR spectroscopy, in which 4000cm is first carried out on a polymer film with a thickness of 50-300 microns -1 And 400cm -1 Then the film was kept in an en...

Embodiment A

[0213] CF is prepared by thermal reaction at 170℃ in a glass reactor 3 OCOF

[0214] A tubular glass reactor with an inner diameter of 55.6 mm and a length of 510 mm, filled with 6×6 glass Raschig rings (free internal volume 842 ml), and maintained at a constant temperature by electrical resistance was used.

[0215] At the same time, CF synthesized as described in USP 4400872 3 OF gas flow (1.5 liters / hour) and CO flow (1.5 liters / hour) were added to the reactor kept at 170°C for 5 hours. The flow from the reactor is continuously analyzed by on-line gas chromatography analysis.

[0216] The stream from the reactor except CO is condensed in a trap kept at -110°C containing 15gCFCl=CFCl(A 1112), so that residual CF 3 OF reacts with olefin to obtain CF 3 OCFClCF 2 Cl.

[0217] After fractional distillation of the resulting mixture, 33.9 g of 99.8% pure CF was obtained 3 OCOF (for feed CF 3 The molar yield of OF is 76.5%), 12.3g of CF 3 OCFClCF 2 Cl, 3.4g COF 2 .

[0218] Relative fe...

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Abstract

The present invention provides a VDF-based curable fluoroelastomers having glass transition temperature lower than -35 DEG C. and an amount of -COF end groups in the polymer lower than the sensitivity limit of the method using the FT-IR spectroscopy described in the present application.

Description

[0001] An industrial invention specification in the name of SOLVAY SOLEXISS.p.A. with Italian nationality and headquartered in Milano, via Turati 12. Technical field [0002] The present invention relates to a VDF-based fluoroelastomer with an improved combination of Tg (glass transition temperature) lower than -35°C and having mechanical and compression set properties in a wide temperature range at high and low temperatures. [0003] More specifically, the present invention relates to a fluoroelastomer with a Tg lower than -35°C and substantially no -COF end groups, which are undetectable by the method described below. The fluoroelastomer of the present invention shows an improved molecular weight as shown by an improved intrinsic viscosity and can be obtained by a polymerization method with improved productivity. Background technique [0004] It is well known that fluoroelastomers are particularly useful polymers in the automotive, aerospace, petroleum, petrochemical and electro...

Claims

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Application Information

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IPC IPC(8): C08F14/18C08L27/12C07C21/18
CPCC07C68/00C07C43/313C08F14/18C07C41/48C07C41/54C07C69/96C08F2/02C07C21/18
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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