Method of treating surface of fibre glass-filled polytetrafluoroethylene

FIELD: chemistry.

SUBSTANCE: surface of fibre glass-filled polytetrafluoroethylene is treated with a sodium-naphthalene complex in tetrahydrofuran. The surface is washed and dried. 2-4 wt % solution of 3-aminopropyl triethoxy silane in ethanol is deposited and the surface is dried at 70-90°C.

EFFECT: method ensures high adhesion strength of acrylate and fluoride rubber to the surface of fibre glass-filled polytetrafluoroethylene.

2 tbl, 4 ex

 

The invention relates to the development of the adhesive composition for attaching rubber to steklovolokonnogo the polytetrafluoroethylene (PS: fluoroplastic-4 containing 25 wt.% fiberglass) during vulcanization and can be used in the manufacture of rubber products for the automotive industry.

Polytetrafluoroethylene (PTFE), due to their specific chemical and physical structure, has an exceptional chemical inertness, wide operating temperature range from -269°to +260°C), low coefficient of friction, poor adhesive property.

To increase the adhesion of PTFE commonly used methods of modification of its surface by plasma (Danilin BS the Use of low-temperature plasma for etching and cleaning materials. - M.: Energoatomizdat, 1987, 264 S. Trofimenko K.A., Kucheeva E.A. plasma Chemical surface modification of PTFE. XXX Gagarin readings. Abstracts of the international youth scientific conference, Vol.6, M.: LALMAS, 2004, p.23-24).

Know the use of carbofunctional silicon-organic derivatives, in particular 3-aminopropyltriethoxysilane (AGM-9), for the preparation of adhesives and surface treatment (Lazarev GV, Sobolevsky MV, Rosenberg V.R. Carbofunctional organosilane and organosiloxane. - Moscow: Hee the Oia, 1990, p.124; Novitskaya S. p., Nudelman Z.N., Dontsov AA Forecaster. Moscow: Chemistry, 1988, s). Such adhesives may contain resin (rezol, phenolic), 3-amino-propyltriethoxysilane (AGM-9), the solvent (methyl ethyl ketone). The water content of the organic solvent is methylethylketone (TU 6-09-782-76) limited regulatory document and does not exceed 0.8 wt.%. An organic solvent such adhesives is the main water - secondary. Upon dilution with methyl ethyl ketone water in such Klee significantly decreases the adhesive strength of the rubber to the metal.

Famous water company Henkel adhesives XW 7484 and XW7856, which is an aqueous dispersion, cholesteremia on the surface of the heated metal in a solid film (Y. Morozov, Reznichenko S. Recent advances in the chemistry and technology of elastomers - international conference on rubber and rubber IRC'98, Rubber & rubber, No. 1, 1999, p.46). Such adhesives comparable to systems containing the solvent, although somewhat inferior to them in strength of attachment of the rubber to the metal. However, there are no data on the basis of any of the elastomers is used to mount rubbers and compounds of these elastomers (Beiersdorf D. Mount rubbers to metal with the help of middleware systems "Henkel". Rubber & rubber, No. 6, 1996, p.3 7...).

Known adhesives and adhesives for fastening rubber products based on acrylate ka is Chukov to metal surfaces during vulcanization: Hemosil 350 and 360 (dry residue 38-42 wt.% and 42-45 wt.%, respectively) of the firm Henkel, water-emulsion adhesive BA-1 (TU 2294-330-12654617-95, dry residue of at least 12 wt.%).

The composition of the adhesives Hemosil 350 and 360 (by analogy with Chemosil 211) includes soluble organic polymers and dispersed solids in organic solvents (ethanol/ethyl acetate). This product is included in the group flammable substances (Henkel KGaA, SPK 04/90).

The main disadvantages are the use in the manufacture of various solvents and high dry matter content, which is a collection of various soluble polymers, dispersed solids.

The composition of water-based glue VA-1 is a water-soluble phenolic resin, the polymer (polybutadiene) and dispersed solids. The concrete structure is not given.

Known introduction in the rubber composition of the modifying additive R-152 (Quaternary ammonium salt of 1,8-diazabicyclo[5,4,0]-undecene-7 and Novolac resin) to increase the adhesion of rubbers on the basis of fluorine - and epichlorhydrine (Nudelman Z. Florkowski: fundamentals, processing, application. M: LLC MIF RIAS, 2007, 364 S.).

Also known adhesive composition (Golfarb VI, Lapaeva N.A., Gorban VI, Pichhadze SJ Patent No. 2180675. The adhesive composition), which is an aqueous adhesive for fluoride rubbers, suitable for mounting acrylate rubbers to metal Seating the second surface of the valve cuff. The main disadvantage of the adhesive is necessary when it is used to observe the homogeneity of the composition, which is a set of various soluble polymers and dispersed solids.

Closest to the claimed method is a chemical method of processing the surface of a PTFE (Kovacic L. Bonding metals and plastics: transl. from Slovac. Ed. Astradyne. - M.: Chemistry, 1985, 240 C.), which ensures uniformity of processing and high adhesive strength (prototype). The method consists in the processing of PTFE for 5-15 minutes at 20°C. a solution prepared as follows: 128 grams of naphthalene dissolved in 1 l of tetrahydrofuran, add 23 g of metallic sodium and stirred for 2 hours. Then PTFE washed with acetone, water and dried.

The technical result of the invention is to achieve a high strength acrylic and fluorinated rubbers to the surface steklovolokonnogo polytetrafluoroethylene.

This technical result is achieved by sequential processing of the surface steklovolokonnogo PTFE-sodium-naphthalene complex in tetrahydrofuran and 3-aminopropyltriethoxysilane in ethyl alcohol followed by drying at a temperature of 70-90°C.

Example. Adhesion steklovolokonnogo PTFE akrilatna and fluorine rubbers.

In the claimed technical solution uses a chemical method of surface modification steklovolokonnogo PTFE, which consists in the successive immersion of the sample for 5 minutes in a sodium-naphthalene complex in tetrahydrofuran, followed by washing, drying, application of 2-4 wt.% solution of 3-aminopropyltriethoxysilane in ethanol and drying at a temperature of 70-90°C.

The optimal concentration of 3-aminopropyltriethoxysilane in ethyl alcohol is 2-4 wt.%. Concentrations of less than 2 wt.% and more than 4 wt.%, as the experiments showed, reducing the strength of adhesion of rubbers and steklovolokonnogo PTFE.

The connection of rubber-modified samples FS (fluoroplastic-4 containing 25 wt.% glass fiber) was produced in the vulcanizing press.

Determination of the strength of the adhesive interaction of rubbers and steklovolokonnogo PTFE was carried out according to GOST 6768-75.

It was determined the force required to separate the layers of rubber and FS. Tested sample width (25±0,5) mm, thickness 4 mm and a length for the stratification in the area at least 100 mm, the Tests were carried out on a tensile testing machine Zwick/Roell with the speed of movement of the rolling grip 100 mm/min

The results of the study are given in table 1. Transcript of the rubber compositions of the mixtures are given in table 2.

p>
Table 1
The bond strength, kgf/cm, when stratification "rubber-FS"
№ p/pRubber compoundThe processing of PTFE
sodium-naphthalene complex (prototype)sodium-naphthalene complex, then AGM-9AGM-9, then a sodium-naphthalene complex
12803-9 based on acrylate rubber Akron XF-5140 (product emulsion copolymerization of acrylic acid with vinyl monomers, the Mooney viscosity ML (1+4) 100°C=40%)1,591,890,64
22803-23 based on acrylate rubber Akron XF-51400,550,840,40
3420-35 on the basis of fluoride rubbers SCF-26 (a copolymer of vinylidenefluoride and hexaferrite, top grade. The Mooney viscosity ML (1+10) 150°C=95-105%) and GFR-26 OHM (copolymer of vinylidenefluoride and hexaferrite is a, OHM is a very low molecular weight. The Mooney viscosity ML (1+4)120°C=20%)0,510,820,47
4420-67-based fluorine rubber G-752 (a copolymer of vinylidenefluoride and hexaferrite, with vulcanizing system consisting of Bisphenol AF and postnasal salt chloride. The Mooney viscosity ML (1+10)121°C=30)1,602,01the 1.44

The analysis of the results showed that the bond strength "rubber-FS" after chemical treatment FS solution of sodium-naphthalene complex in tetrahydrofuran, followed by the application of AGM-9 in ethanol at 1.18 to 1.60 times the value of the bond strength at the surface FS only solution of sodium-naphthalene complex in tetrahydrofuran. AGM-9, as bifunctional compound, provides chemical interaction between the matrix rubber (rubber) and the surface FS, thereby increasing the bond strength "rubber-FS". Moreover, this fact is observed for all investigated rubber blends are given in table 2.

Processing of AGM-9, then chemical modification adversely affects the bond strength "rubber-FS". Surface color FS changes to light brown is O. This is because the presence of AGM-9 on the surface FS prevents a more complete detonirovanie polymer and, accordingly, the acquisition of a dark brown color.

When the surface treatment FS solution of sodium-naphthalene complex is defluorination of the polymer chain and the formation of double bonds in the macromolecule PTFE, which is confirmed by the appearance in the infrared spectrum of absorption bands (νs=1592,0 cm-1, νas=1417,7 cm-1), corresponding to vibrations of the C=C, missing the unmodified PS. On multiple bonds can communicate steklovolokonnogo PTFE with the amino group of the diamine carbamate, part of the acrylate rubber, and the amino group of 3-aminopropyltriethoxysilane can interact with the oxygen of the carbonyl and ester groups of the acrylate.

It is not excluded that residual ethoxy-group AGM-9 in the vulcanization process at high temperature and pressure continue to communicate with components of rubber, namely Si-OH groups of mineral fillers (white carbon black BS-100, hard-shelled land Celite-219 and others) acrylate rubber.

Thus, the bond strength steklovolokonnogo PTFE with rubber-based fluoride and acrylate rubbers can be improved further modification of the surface of the fluoropolymer whom is the osita FS 3-aminopropyltriethoxysilane in ethyl alcohol, pre-treated with a solution of sodium-naphthalene complex in tetrahydrofuran.

The consumption of the compositions of the first and second stages of surface treatment FS is 2900±50 300±10 ml/m2respectively.

240,7
Table 2
The investigated compounds acrylate and fluorinated rubbers
№ p/pCompositionCipher rubber
2803-9 (per 100 mass parts of the rubber)2803-23 (per 100 mass parts of the rubber)420-35 (per 100 mass parts of the rubber)420-67 (per 100 mass parts of the rubber)
1Rubber Akron XF-5140100100
2Deafen AF2
3Stearic acid T-32 1
4Silica Carplex 1120507,6
5White carbon black BS-10050
6Hard-shelled land Celite 2193525
7The wollastonite FW 32550408
8Graphite Superrior 502620,31
9AGM-90,40,4
10Carbon black T-900/iron Oxide -/23/3-/0,22/2
11Tetrastearate pentaerythritol/Wax SV-N-/12/1-/0,2-/0,3
12Dibutylsebacate/low-Molecular-weight polyethylene/Amines taly2/-/-1,5/2/1,2
13Diphenylguanidine11
14Hexamethylendiamine0,70,7
15Rubber SCF-26/SCF-26 OHM/G-75266/34/--/-/100
16Magnesium oxide RA-200/burnt magnesia -/83/-
17Calcium hydroxide Caldic 200066
18Barium sulphate1535
19Calcium fluoride735
20Lacquer ruby0,2
21Bisphenol a, diphenylolpropane)1,6
22Octadecyltrichlorosilane0,3
Amount240,1151,5184,3
Viscosity, ML (1+4)120°C, Mooney units6060103,589

The method of surface treatment steklovolokonnogo polytetrafluoroethylene for attachment to him resins based on acrylate or fluorinated rubber, which consists in the fact that steklovoloknistye polytetrafluoroethylene processed sodium-naphthalene complex in tetrahydrofuran, followed by washing, drying, application of 2-4 wt.% solution of 3-aminopropyltriethoxysilane in ethanol and drying at a temperature of 70-90°C.



 

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