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INVENTION
Patent of the Russian Federation RU2108357
ADHESIVE FOR GLAZING, SEALING AND PREPARATION OF CONNECTIONS ...
Applicant's name: Closed Joint-Stock Company "Unique technologies for the production of molds"
The name of the inventor: Kulikov GA; Preobrazhensky IM; Akimov BA; Nikitina N.L .; Maltsev G.K .; Shebashova NM; Shebashov Yu.N .; Chesnokova I.V.
The name of the patent owner: Closed Joint-Stock Company "Unique technologies for the production of molds"
Address for correspondence:
Date of commencement of the patent: 1996.10.08
The adhesive is designed for bonding and sealing and impregnating joints, to increase their thermal and mechanical strength. The adhesive includes epoxydian resin, polyethylene polyamine modified with 1,2-di (hydroxymethyl) -ortho-carborane , oligoamide of T-19 grade and carbonyl iron.
DESCRIPTION OF THE INVENTION
The invention relates to cold-cured epoxy-resin-based compositions filled with powdered iron, which are intended for bonding and sealing compounds, impregnating and coating parts to improve their thermal and mechanical strength in repair, industrial work in industry and everyday life.
Among the known analogs of the technical essence and coinciding features of the closest proposed is a composition that contains an epoxy-resin resin, a hardener in the form of a mixture of a modified polyethylene polyamine and a T-19 oligomamide, a polycondensation product of dimerized fatty acid methyl esters of tall oil and triethylenetetraamine, and a carbonyl filler Iron ( Patent of the Russian Federation No. 2041894, cl. C 08 L 63/00, 1995 ).
In the prior art, the polyethylene polyamine is modified with a carborane derivative of general formula R 1 CB 10 H 10 CR 2 , wherein R 1 and R 2 are the same or different organic substituents. In this case, R 1 is hydrogen, acryl, alkyl, alkenyl, simple or ester, acid, and R 2 is acryl, alkyl, alkenyl, simple or ester, acid in an amount of 0.06-100.0 parts by weight. By 100 parts by weight. Epoxy resin.
The direct interaction between amines and the structural formula of ortho-carborane leads to the successive substitution of hydrogen atoms in the carborane nucleus, forming products of varying degrees of substitution, with different materials with markedly different physicomechanical characteristics.
The known composition is universal, providing different service characteristics depending on the combination of constituent components and their quantitative content, and can be used as both an impregnating material, an adhesive, a coating, and a structural material for injection molds and molds.
Thus, as the modifying agent of polyethylene polyamine, prototypes are used in the mixture with the product of polycondensation of dimerized acids of linseed and soybean oil with diethylenetriamine or tetraethylenepentamine, and as a filler, powder of various metals and alloys, non-metallic powders and fibers is introduced.
However, the qualitative composition and the quantitative content of the selected series of ingredients are not optimized in the confidence range of industrial technology, which guarantees the specified repeatability, uniformity of the main service characteristics of the material, in particular glue, such as heat resistance, strength, adhesion.
The object of the invention is to provide a process adhesive with increased heat resistance and strength properties.
The desired technical result is achieved by the fact that in a known glue comprising an epoxydian resin, a curing agent is a mixture of a modified polyethylene polyamine and an oligoamide of the T-19 brand, a polycondensation product of dimerized fatty acid methyl esters of tall oil and triethylenetetraamine, and a carbonyl iron filler, A mixture of a modified polyethylene polyamine, which is the reaction product of 16 parts by weight. 1,2-di- (hydroxymethyl) -ortho-carborane with 100 parts by weight of Polyethylene polyamine, and T-19 oligomamide, with the following ratio of the components of the adhesive, mass parts: epoxy resin 100; Modified polyethylene polyamine 12-20 ; Oligoamide of T-19 grade 4-60 ; Carbonyl iron 350-450 .
Distinctive features, qualitative and quantitative composition of the composition ensured the production of non-toxic, process-oriented in processing and applying glue with guaranteed required technical and operational properties: heat resistance not lower than 300 o C and adhesion-enhanced adhesion (glued shear strength).
The modification of polyethylene polyamine by the addition of 1,2-di- (hydroxymethyl) -orto-carborane in an amount of 16 parts by weight. Per 100 parts by weight . Polyethylene polyamine provides high adhesion and heat resistance, since the new additive contains the most active of all carboranes functional groups.
The content in the adhesive composition of 1,2-di- (hydroxymethyl) -ortho-carborane and polyethylene polyamine in a ratio of less than 16 to 100 reduces the adhesion and heat resistance of the material, and their ratio is greater than 16/100 , does not lead to improved performance , But leads to a cost overrun of expensive carborane. The lower limit of the content in the carbonyl iron composition is 350 wt. H is determined by a given level of heat resistance during cyclic loading of the glue joint.
At a carbonyl iron content in an amount exceeding 450 parts by weight. , The strength of the cured composition decreases, with the preparation of which additional mixing problems arise due to the increasing viscosity.
Introduction of polyethylene polyamine- 1,2-di- (hydroxymethyl) -orto-carborane in the composition in an amount of less than 12 parts by weight . Leads to a decrease in the heat resistance of the adhesive joint.
The content in the composition of polyethylene polyamine- 1,2-di- (hydroxymethyl) -orto-carborane is greater than 20 parts by weight. Does not increase heat resistance, but increases the consumer cost of the material, while there is a reduction in the strength of the connection.
The content of the T-19 oligomide composition in an amount in excess of 60 wt. H., Not technologically due to the increase in the curing time of the glue over 24 hours.
When the T-19 oligomide is introduced into the composition, less than 4 parts by weight are used. Sharply reduces the strength of the adhesive bond to a level that is provided by glue-analogs.
The new polyethylene polyamine modifier, the proposed qualitative composition and the quantitative content of the composition ingredients have been experimentally worked out and optimized in a confidence range of values, any combination of which provides the specified characteristics and properties of the adhesive.
The proposed mixture is prepared from two structural components.
The first component - a binder - is prepared by mixing epoxydian resin, GOST 10587-84 with carbonyl iron, GOST 13610-79 in the ratio of parts by weight. 25/75 .
The second component , the hardener, is prepared by mixing the previously prepared polyethylene polyamine- 1,2-di- (hydroxymethyl) -ortho-carborane with the oligoamide T-19, GOST 2224- 249-09201208-93 with the addition of carbonyl iron in a volume of 75 parts by weight .
The modification of polyethylene polyamine is carried out by synthesis, chemical reaction when it is mixed with 1,2-di- (hydroxymethyl) -ortho-carborane , in the ratio 100 \ 16 :
Example
The technology of preparation of the proposed adhesive provides for the preliminary drying of carbonyl iron in a drying cabinet at 100-120 ° C for 4-6 hours .
5 kg of ED-22 resin are placed in the mixer, then 15 kg of carbonyl iron are added portionwise and mixed for 2-3 hours at 45-55 ° C.
In the second mixer, 0.2 kg of T-19 oligoamide , 0.8 kg of polyethylene polyamine- 1,2-di- (hydroxymethyl) -ortho-carborane and 3 kg of carbonyl iron are mixed in the same sequence and modes.
Further, both components are mixed together and the glue is ready for use for 40 minutes .
After curing ( 24 h ) the glue practically does not shrink, it is mechanically processed.
The glue in the laboratory was prepared and tested over the entire range of the contents of each component.
Table 1 shows the characteristic compositions of the proposed adhesive, and in Table 2 - inherent in these compositions, physical and mechanical characteristics.
From the tables it follows that the epoxy adhesive of the proposed composition in the optimal ratio of the constituent components provides a temperature resistance of 340-380 ° C (at 300 ° C maximally for the known cold-setting adhesives, analogous compositions) and the adhesion properties are 1.5-2.5 times higher.
The proposed epoxy adhesive is intended for use as filling, sealing compounds, putty, structural adhesive joint, protective films and coatings of parts and products.
CLAIM
An adhesive comprising an epoxy-resin resin, a hardener is a mixture of a modified polyethylene polyamine and an oligoamide of the T-19 polycondensation product of dimerized fatty acid methyl esters of tall oil and triethylenetetraamine and a filler carbonyl iron, characterized in that as a curing agent, the adhesive comprises a mixture of a modified polyethylene polyamine representing The reaction product is 16 parts by weight. 1,2-di- (hydroxymethyl) -ortho-carborane with 100 parts by weight of Polyethylene polyamine, and T-19 oligomamide, with the following ratio of the components of the adhesive, :
- Epoxy resin - 100
- Modified polyethylene polyamine - 12 - 20
- Oligoamide brand T-19 - 4 - 60
- Carbonyl iron - 350 - 450p
print version
Date of publication 31.10.2006гг
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