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INVENTION
Patent of the Russian Federation RU2087509
COMPOSITION FOR PRODUCING ADHESIVES WITH CONSTANT FLEXIBILITY
Applicant's name: V.Kargin State Research Institute of Polymer Chemistry and Polymer Technology with pilot plant
The name of the inventor: Kuryzhova LV; Klyuzhin ES; Zavin BG; Pryakhina TA; Kotov V.M .; Kashintseva GN; Pavlov V.Yu .; Kravchenko V.S.
The name of the patentee: State Research Institute of Polymer Chemistry and Technology named after V. Kargin with an experimental plant
Address for correspondence:
Date of commencement of the patent: 1994.06.07
The invention relates to the creation of compositions for the preparation of a glue with a permanent tack, intended for adhering heat-resistant film materials and articles thereof to metal surfaces. The invention solves the problem of increasing the heat resistance of the glue and simplifying the technology of its production. The composition includes, by weight: butylacrylate 88-65; Butyl methacrylate 32-5; Methacrylic acid 3-7; Benzoyl peroxide as an initiator of free-radical polymerization 0.35-0.55; 1,5-divinyl-1,3,5,7-tetramethyl-3,7-diphenylcyclotetrasiloxane 6-15; Tetramethyldisilylbenzene 6-15; Platinum hydrochloric acid as a catalyst (3-15) · 10 -4 ; Ethyl acetate as solvent 300-400. The last five components are taken for 100 wt. H. Mixture of monomers. When using the adhesive, the strength at detachment of the polyimide film from the aluminum surface is: at room temperature, 1.08-1.93 kgf / cm 2 ; At a temperature of 150 ° C after holding at this temperature for 2 hours - 0.17-0.39 kgf / cm 2 ; At a temperature of 250 ° C after holding at this temperature for 2 minutes - 0.08-0.15 kgf / cm 2 .
DESCRIPTION OF THE INVENTION
The invention relates to a composition of adhesives based on high molecular weight polymerization products, in particular to acrylic adhesives with a permanent tack, intended for bonding heat-resistant film materials (eg polyimides) and articles thereof to metal surfaces of steel, aluminum, etc.
These adhesives are used for temporary fastening of small devices, sensors, sometimes sealed in polyimide film, etc. on the metal surfaces of machines, mechanisms that are heated during operation or under extreme conditions up to 150-250 o C.
Due to the constant stickiness of the adhesive layer, installation work is greatly accelerated, and at the right time the instruments and sensors are easily dismantled.
Adhesive with constant tackiness should meet the following requirements. The strength at detachment of a polyimide film from an aluminum or steel surface at room temperature should be not less than 1.00 kgf / cm 2 , at a temperature of 150 ° C after holding for at least 2 hours at least 0.15 kgf / cm 2 at a temperature of 250 ° C after holding at this temperature for 2 min not less than 0.05 kgf / cm 2 . Do not activate the adhesive layer by heating or any radiation to increase the strength and thermal stability of the adhesive bond.
Known adhesive composition with a constant tack and increased heat resistance [1] for gluing a polyester film to steel, aluminum.
According to Example (parts by weight): 60 2-ethylhexyl acrylate (2-EGA), 40 butyl acrylate (BA), 1 4,4'-azobisianovaleric acid, 1 thioglycolic acid in 75 methyl ethyl ketone and 75 toluene are aged 8 hours at 70 ° C In a stream of nitrogen with stirring. The oligomer is isolated with a water-methanol mixture. In 100 wt. H. Oligomer is added 4 parts by weight. Glycidyl methacrylate, 0.5 parts by weight Tributylamine, 0.5 wt. H. Hydroquinone and 150 parts by weight. Xylene and held for 6 hours at 140 ° C., after which a macromonomer is similarly isolated.
10 wt. H. Macromonomer, 51 ml. H 2-EGA, 34 parts by weight BA, 0.5 parts by weight 2,2'-azobisisobutyronitrile in 150 wt. H of ethyl acetate is held at 60 ° C. for 8 hours to obtain a graft copolymer (PSPL). Adhesion of the adhesive from this copolymer applied to a 25 micron polyester film to steel is 1280 g / 20 mm, the adhesion retention time (sample 20 x 10 mm at 40 ° C and 400 g load) is 630 minutes, the heat resistance when bonding aluminum and Tests at 20 ° C for 1 hour, 60 ° C for 1 hour and 20 ° C for 1 hour and 0 ° C for 1 hour remains high.
However, the described adhesive is not heat-resistant at higher temperatures: at a temperature of 150 ° C., it is destroyed without load. In addition, the drawbacks include the complexity of the technology for obtaining glue (3-stage graft polymerization).
In [2], a method for manufacturing polyacrylate dispersions in aliphatic hydrocarbons with a thermal stability of up to 50 ° C is described.
The polymer is prepared with stirring under a nitrogen atmosphere, parts by weight. 100 hexane (I), 97.5 2-EGA, 17.5 methyl acrylate (II), 2.5 acrylic acid (AA), 0.1 azoisobutyronitrile (III), the mixture is polymerized at 70 ° C for 20 minutes, then Cooled. A product containing 73.2% of the polymer is obtained. The apparatus is charged, parts by weight. 219 of the manufactured polymer and for 1.5 hours a mixture consisting of 1805 isodecyl acrylate, 170 vinyl acetate, 10 N-butoxymethyl methacrylamide, 22.5 oxymethacrylate and 1.2 benzoyl peroxide (PB) was added. Within 3 hours, 241 parts by weight were added to the mixture. I and 10 parts by weight. PB and polymerized at 70.degree . C., then cooled and a dispersion with a solid content of 54.2% was obtained. The shear strength of the adhesive compound, estimated over time, during which the films from the polyethylene terephthalate glued together with the composition were separated at a load of 1 kg and temperatures of 23 And 50 ° C for more than 24 s. The disadvantage of this method is its complexity (graft polymerization) and the fact that the heat resistance of the adhesive is below 150 ° C (it breaks down at this temperature without load).
As a prototype, a pressure-sensitive acrylate adhesive composition with increased heat resistance based on 70-95 parts by weight was taken. Polyalkyl (meth) acrylate with T glass. = 90-0 ° C and 5-30 hours. 
2 compounds selected from metal salts with rosin-modified phenolic resin [3]
According to an example, the composition includes, by weight. 80 copolymer synthesized from 73 BA, 25 2-EGA and 2 AA in the presence of 0.2 PB and 100 ethyl acetate at the boiling point of the solvent, 10 lithium salt of the rosin-modified phenolic resin (MFFS) with a softening temperature of 185 ° C., synthesized per hour for 80 ° C from 100 MKFS (Tamanol-803) and 4 lithium hydroxide in 150 toluene, 10 ester (MCPS and G) with a softening point of 176.5 ° C, synthesized for 3 hours at 240 ° from 100 by the phenol modified by colophony Resin and 3 glycerol (D), and 8.2 polyisocyanate (Coronet L) are applied to a polyethylene sheet having a thickness of 38 μm, dried and an adhesive sheet with a glue layer thickness of 30 μm and a peel strength of 180 ° from stainless steel Tearing off of 300 mm / min.) 1.76 (20 ° ) or 1.18 kg / 25 mm (80 ° ).
The disadvantage of the composition of the prototype is the complexity of the technology for its production. In addition, the adhesive compositions are not sufficiently heat-resistant and do not have the necessary strength at temperatures of 150-250 ° C (they break down at the indicated temperatures without load).
The technical result of the proposed invention is to increase the heat resistance of the adhesive with constant tack and simplify the technology for its preparation.
This is achieved by the fact that the composition for producing a glue with a permanent tack including butyl acrylate, butyl methacrylate, methacrylic acid, benzoyl peroxide as a free radical initiator and ethyl acetate as solvent, in addition to the known one, additionally contains 1,5-divinyl-1,3 , 5,7-tetramethyl-3,7-diphenylcyclotetrasiloxane, tetramethyldisilylbenzene and chloroplatinic acid as the catalyst, with the following ratio of components, parts by weight.
Butyl acrylate (BA) 88-65
Butyl methacrylate (BMA) 32-5
Methacrylic acid (MAA) 3-7
The novelty of the claimed adhesive is the use of 1,5-divinyl-1,3,5,7-tetramethyl-3,7-diphenylcyclotetrasiloxane and tetramethyldisilylbenzene.
These compounds were synthesized in INEOS, Moscow, and in adhesive compositions with permanent stickiness were not used. Adhesives have a heat resistance at short-term exposure to temperatures of 150 ° C (2 h), 250 ° C (2 min). The strength at detachment of a polyimide film from aluminum on samples of the "fungus" type according to GOST 14760-69 at temperatures 150-250 ° C is not less than 0.15 kgf / cm 2 and 0.05 kgf / cm 2, respectively.
EXAMPLES OF THE INVENTION
Example 1
The adhesive composition obtained by polymerizing the mixture at 75 ° C., H. 85 BA; 10.5 BMA; 4.5 MAC; 0,45 PB; 9 1,5-divinyl-1,3,5,7-t-tetramethyl-3,7-diphenylcyclotetrasiloxane (CO-1), 9 tetramethyldisilylbenzene (CO-II), 1 × 10 -3 chloroplatinic acid (II-I), 300 Ethyl acetate, brush or roller is applied to the surface of the polyimide film on both sides and to the surface of the aluminum fungus. After holding at room temperature for 15-30 minutes, the surfaces to be bonded are joined at contact pressure.
The strength at the detachment of the adhesive at temperatures of 20, 150 and 250 ° C is 1.08; 0.17; 0.15 kgf / cm 2 (see the table).
Example 2
The adhesive composition obtained by polymerization at 75 ° C. of a mixture consisting of, 65 BA, 32 BMA, 3 MAK, 0.35 PB, 6 КО-I, 6 КО-II, 3 × 10 -4 П-I, 300 ethyl acetate are applied from both sides to the polyimide film and to the surface of the aluminum fungus. After holding at room temperature for 15-30 minutes, the surfaces to be bonded are joined at contact pressure. The strength at separation of the adhesive at temperatures of 20, 150 and 250 ° C is 1.93; 0.33; 0.08 kgf / cm 2 .
Example 3
An adhesive prepared from a solution of a copolymer synthesized by polymerization at 75 ° C. of the mixture, 88 BA, 5 BMA, 7 MAK, 0.55 PB, 400 ethyl acetate, and 15 KO-I, 15 KO-II, 15 × 10 -4 PI-I, is applied from both sides to the polyimide film and to the surface of the aluminum fungus. After holding at room temperature for 15-30 minutes, the surfaces to be bonded are joined at contact pressure. The strength at separation of the adhesive at temperatures of 20, 150 and 250 ° C is 1.37; 0.39; 0.12 kgf / cm 2 .
Under similar conditions, the bond strength based on the adhesive at the prototype at 20 ° C is 2.0 kgf / cm 2 , and at temperatures of 150 and 250 ° C the adhesive compound is destroyed without load.
From the examples and table, it can be seen that the proposed technical solution makes it possible to obtain an adhesive with the desired thermal stability. At the same time, the technology of obtaining it is much simpler.
The advantages of the claimed adhesive composition include the fact that, in order to impart heat resistance, it is not necessary to activate the adhesive layer by heating, irradiation, or the like, as is usually done in the manufacture of heat-resistant adhesive tapes.
The specified technical result is not achieved beyond the stated intervals of content of the components.
CLAIM
A composition for producing an adhesive with a permanent tack on the basis of alkyl (meth) acrylate, comprising benzoyl peroxide as a free radical initiator and ethyl acetate as a solvent, characterized in that as an alkyl (meth) acrylate it contains butyl acrylate and butyl methacrylate and additionally methacrylic acid, 1,5-divinyl-1,3,5,7-tetramethyl-3,7-diphenylcyclotetrasiloxane, tetramethyldisilylbenzene and the catalyst, chloroplatinic acid, in the following ratio, parts by weight.
Butyl acrylate 65 88
Butyl methacrylate 5 32
Methacrylic acid 3 7
By 100 parts by weight. Mixture of monomers
Benzoyl peroxide 0.35 0.55
1,5-Divinyl-1,3,5,7-tetramethyl-3,7-diphenylcyclotetrasiloxane 6 15
Tetramethyldisilylbenzene 6 15
Hydrochloric acid (3 15) · 10 -4
Ethyl acetate 300 400 tons
print version
Date of publication 18.12.2006гг
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