Barbarastrasse oligoadenylate as heat monomeric basis cured compositions and anaerobic composition based on them


(57) Abstract:

Use: for sealing and fixing the threaded and smooth cylindrical joints, seal flanged connections subject to prolonged exposure to elevated temperatures. The inventive anaerobic composition comprising barbarastrasse of oligoadenylate General formula

where 100 hours hydropeaking initiator, and 0.2 to 5.0 hours, the polymerization accelerator is 0.2 to 5.0 hours, the stabilizer of 0.002 to 0.2 h 2 S. p. F.-ly, 3 tables.

The invention relates to the chemistry of polymers, namely, the cured compositions, such as heat-resistant anaerobic compositions, which are used for sealing and fixing the threaded and smooth cylindrical joints, seal flanged connections subject to prolonged exposure to elevated temperatures (400oC for at least 50 h, and the strength of the connection shall be not less than 5 N. m), as well as to new chemical compounds-carborundorum oligoadenylates General formula

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used as heat-resistant Monomeric basis cured compositions.

Known connections (application YAP 3;4

used as a Monomeric basis anaerobic compositions and compositions for coatings, cured by heating under the action of UV radiation.

Anaerobic composition based on the specified connection, after curing in a narrow metal gap (bolt, nut) for 24 h at room temperature has time unscrewing 30,0 34,0 N. m, and after exposure to 180oC for 6 h and tested at the specified temperature 26,0 32,0 N. m

Coatings on steel obtained by curing a monomer basis at a temperature of 150oC for 0.5 h or under the action of UV-irradiation, have a pencil hardness H-2H.

Data on thermal stability of the compositions at 400oC in the patent are not given.

Closest to the present invention is an anaerobic composition containing acrylate oligomer triethyleneglycoldinitrate, hydrophilicity initiator, a polymerization accelerator, a stabilizer (patent Germany N 2802360, CL 09 To 3/10, published. 1978).

This composition has a viscosity of 28 180 SDR and the time of unscrewing after curing it into the narrow metal gap (pain nut) for 24 hours at room temperature 125 350 CT cm (12,5 35,0 Nm).


The set task is solved by synthesis carborundorum of oligopyrroles General formula

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and the fact that the anaerobic composition comprising barbarastrasse oligopyrroles, hydrophilicity initiator, a polymerization accelerator and a stabilizer, in contrast to the known, contains barbarastrasse oligopyrroles General formula

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in the following ratio, wt. h

Specified barbarastrasse oligopyrroles 100

Hydrophilicity initiator 0,2-5,0

The polymerization accelerator 0,2-5,0

The stabilizer 0,002 0,2

Barbarastrasse oligoadenylate General formula (I) are not described in literature. They are synthesized in the Institute of polymers and are used as heat-resistant Monomeric basis cured compositions for the first time.

These compounds are produced by interaction of the acid chloride of 2-tarakanovas acid 1,7-bis(oxymethyl)-meta-carboran or 1,2-bis(oxymethyl)-ortho-carboran in the medium of organic solvent in the presence of an acceptor of hydrogen chloride triethylamine (Et3N). The synthesized compounds are high-boiling substances, soluble in diethyl ether, the Mr spectra.

Example 1. Synthesis of bis-(2-forcricket)-meteorburn (product 1).

Charged to the reactor 81,72 g (0.4 mol) of 1,7-bis (oxymethyl)-meta-carboran (ICD), 300 ml of diethyl ether, 95,48 g (0.88 mol) of acid chloride of 2-tarakanovas acid (HAPAC) and at 0-5oC, and stirring was added dropwise 96,96 g (0,48 mol. ) Et3N within one hour. The precipitation is filtered off, the reaction mass is washed with 5% aqueous solution of hydrochloric acid and then with water until neutral. After distillation in vacuum, diethyl ether get 131,16 g (94 from theory.) light yellow product 1 with the value of kinematic viscosity 6010-6m/s, n2D0= 1,5160, which is at +5oC during the day crystallizes (tPL32-35oC). Found (%): 31,28; F 10,67; 34,32. Calculated for C10H18B10O4F2(%): 31,03; F 10,91; 34,48.

Range PMR 10% R-RA in CCL4, .m.D. was 4.42 (4H, och2), 5,44 D. D. (2HACH*2,2IHAHB3,4 Hz3IHAF 12.9 Hz), 5,73 D. D. (2HBCH2,2IHAHB3,4 Hz3IHBF 42,8 Hz).

IR spectrum (cm-1):B-H2600,C=01760,C=C1670.

Example 2. Synthesis of bis-(2-thoracicoabdominal)-orthocarbonate (p the ether, 47,7 g (0.44 mol) HATAK and under stirring at 0-5oC was added dropwise 48,48 g (0.48 mol) Et3N within one hour. Subsequent selection operation carried out analogously to example 1. Get 66,27 g (95 from theory.) the crystalline product 2. Tpl.36-38oC. Found (%): 31,14; F 10,78; C 34,16. Calculated for C10H18B10O4F2(%): 31,03, F 10,91; C 34,48.

Range of the MRP . M. D. 4,84 (4H, och2), 5,47 D. D. (2HACH*214,2IHAHB3,6 GS3IHAF 12.9 Hz), 5,76 D. D. (2HBCH2,3IHAHB3,6 Hz3IHBF 42,6 Hz).

The IR spectrum similar to the spectrum of the product 1.

The synthesized compounds are used as Monomeric fundamentals of anaerobic compositions (AK).

As the polymerization accelerator in AK using N, N-dimethyl-para-toluidine (DMPT), di(hydroxyethyl)-para-toluidine (DGAT), o-benzosulfimide (OBSI), dibenzosuberone (DBSI). Note: W spin system AWH

As hydroperoxide initiator use the hydroperoxide has been studied (CCP), tertiary butyl (GATB). In the stabilizer is used 2,2,6,6-tetramethyl-4-oxopiperidin-1-oxyl (TMOP), malachite green (MOH), oxalic acid (SC).

From table. 2 shows that the proposed anaerobic composition has the following values of M1/MpNm (in parentheses on the prototype):

after curing of the composition on the samples of the bolt-nut at room temperature for 24 h 28,5 40,0/39,5 60,0 (39,5/55,0);

after heating the samples at 400oC for 50 and 100 hours, and tested them at 400oC 17,5-28, and testing them at room temperature 40,5 51,0/29,0 and 45,5 45,0 55,0/27,0 42,0 respectively (27,0/a 0.5, 31.0/0).

Thus, the use of new synthesized carborundorum of oligopyrroles General formula (I) as a monomer basis anaerobic compositions can improve the strength of the hardened anaerobic compositions after prolonged exposure 400oC.

The increase in the number hydropeaking polymerization initiator and polymerization accelerator more than 5 wt. hours at 100 wt.h. monomer leads to premature polymerization of the composition during storage.

The use of these components is less than 0.2 wt. hours at 100 wt.h. monomer dramatically reduces the ability of the AK dried at room temperature in a threaded connection. Increasing the amount of stabilizer is more than 0.2 wt. am also leads to a decrease in the rate of curing and reducing its content of less than 0.002 wt. PM affects the stability of AK during storage.

Below is shown the possibility of using synthesized carborundorum of oligopyrroles as heat Monomeric bases compositions for coatings, cured by heating under the action of UV-irradiation and see their properties.

Example 9. 2. The composition is prepared by mixing (wt. PM): 100 product 1 and 1.0 peroxide be the Les which they receive a coating thickness of 60 Myron.

Example 10. The composition prepared according to example 9, only use instead of 100 wt. including product 1 the same amount of product 2. After curing of the composition at 150oC for 1 h on aluminium receive a coating thickness of 70 μm.

Example 11. The composition is prepared by mixing (wt. PM): 100 product 1 and 3.0 benzylacetone as photoinitiator. The composition applied to the glass surface and subjected to UV irradiation (lamp CES-400, the distance from the radiation source to the surface 15 cm). After 15 to get a solid coating thickness of 100 microns.

Example 12. The composition is prepared by mixing (wt. PM): 66,7 product 1, 33.3 product 2 and 3.0 benzylacetone. Composition utverjdayut analogously to example 11. After 15 to get a solid coating thickness of 110 microns.

For comparison, we have tested the properties of the coatings obtained by curing known carborundorum of oligopyrroles formula (III), in particular bis(acryloyloxy)-meteorburn (BAMC), when heated under the action of UV radiation.

Example 13 (for comparison). The composition is prepared by mixing (wt. PM): 100 BANK and 1.0 benzoyl peroxide. The coating thickness of 70 μm was prepared as in example 9.

Example 14 (comparison). Whom will gorhaut UV irradiation in example 121. After 15 second exposure, the composition remains liquid. After 60 seconds, the result is a floor with an upper liquid layer. The thickness of the coating after removal of the liquid layer by treatment with acetone 50 microns.

The resulting coatings determine the adhesion method of lattice cuts (GOST 15140-78), as well as the loss of mass when heated in air in a dynamic mode (5oC/min) from 20 to 900oC derivatograph Q-1500D system Paulik-Paulik and Erdei (Hungary). The weight of the portion 50 mg.

The results of the tests are presented in table. 3.

From table. 3 shows (examples 9, 10 and 13 for comparison; examples 11, 12 and 14 for comparison) that the coatings obtained on the basis of the synthesized compounds of formula (I) have a higher adhesion and heat stability as compared with the coatings on the basis of known compounds of the formula (III).

Thus, the synthesized barbarastrasse oligoadenylate can be used as heat-resistant Monomeric basis cured compositions.

1. Barbarastrasse oligoadenylate General formula

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where R-CB10H10C-,

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as heat Monomeric basis cured compositions.

2. Anaerobic comp, trichomania the fact that as acrylate oligomer contains barbarastrasse oligopyrroles General formula

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where R-CB10H10C-,

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in the following ratio, wt.h.

Barbarastrasse oligopyrroles 100

Hydrophilicity initiator 0,2 5,0

The polymerization accelerator 0,2 5,0

The stabilizer 0,002 0,2


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