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INVENTION
Patent of the Russian Federation RU2288933

HERNE-SEALING AND WATER-INSULATING COMPOSITION

The name of the inventor: Vaniyev Marat Abdurahmanovich (RU); Nistratov Andrian Viktorovich (RU); Novakov Ivan Aleksandrovich (RU); Lukyanichev Vadim Vadimovich (RU); Novopoltseva Oksana Mihailovna (RU); Lukasik Vladislav Antonovich (RU); Korchagina Tatiana Konstantinovna
The name of the patent holder: State Educational Institution of Higher Professional Education Volgograd State Technical University (Volgograd State Technical University)
Address for correspondence: 400131, Volgograd, Lenin Avenue, 28, VolgTU, Head of the Intellectual Property Department
Date of commencement of the patent: 2005.08.10

The invention relates to polymeric building materials and can be used for the manufacture of sealing and waterproofing compositions processed by pouring. The task is to develop the composition of the composition, which has increased physical and mechanical properties, and high waterproofing properties. The object is achieved in that the composition comprises a polysulfide oligomer-liquid thiokols with a number average molecular weight of 1700-5500 and a viscosity at 25 ° C of 7.5-50 Pa * s, a hydrophobized chalk, a plasticizer, manganese dioxide and an accelerator-No-hydroxyphenyl- M-phenoxyphenylmethanimine or N-p-methylphenylphenylmethanimine and additionally a solvent that is a mixture of toluene and acetone in a ratio of 60:40 wt%

DESCRIPTION OF THE INVENTION

The invention relates to polymeric building materials and can be used for the manufacture of sealing and waterproofing compositions processed by pouring.

A composition for sealing and gluing is known, which includes liquid thiokol, sodium bicarboxylic acid, water, filler, epoxy resin, diphenylguanidine [Averko-Antonovich LA Polysulfide oligomers and sealants based on them. L .: Chemistry, 1983, p.75-78].

The disadvantages of the composition are high water absorption, and a low cure rate at room temperature and high viscosity.

A composition for sealing and gluing is known, which includes liquid thiokol, sodium bicarboxylic acid, water, a filler, a four-functional epoxy resin and a solvent which is also a curing catalyst [Patent of the Russian Federation No. 2058363, Cl. From 09 to 3/10, publ. 1996].

The disadvantage of the composition is the multistage nature of the production technology, low viability and high water absorption.

A sealing composition comprising a polysulfide oligomer, a filler, manganese dioxide, an aerosil, diphenylguanidine, an epoxy diane resin, a vulcanization retardant, a plasticizer is known [AS of the USSR No. 1054397, Kl. From 09 to 3/10, publ. 1983].

The disadvantages of the composition are low: hydrolytic stability, physico-mechanical properties and thixotropy.

The closest to the proposed technical essence and achieved result is a sealing composition comprising a polysulphide oligomer, titanium dioxide, hydrophobized chalk, aerosil, polyethylene glycol adipate, manganese dioxide, stearic acid, diphenylguanidine and a plasticizer with the following component ratio, mass parts:

[Patent of the Russian Federation No. 2064955, Cl. 6 С 09 К 3/10, publ. 1996].

The disadvantage of this composition is insufficient tensile strength and elongation, high water absorption, and the need for a stepwise vulcanization regime (2 stages).

The use of such hydrophilic substances as aerosil, titanium dioxide, polyester, mixtures of dioxane alcohols and their high-boiling ethers significantly reduces the waterproofing properties of coatings in the prototype and analogues of the invention. The hydrophilicity of the polymer matrix inherent in the thiocolol vulcanizates and the presence of the aforementioned components in the composition result in a high water absorption of the coating. In addition, the complex of properties of materials based on polysulfide oligomers essentially depends on the topological structure of the vulcanization grid, determined by the type and content of the oxidant and accelerator.

The object of the present invention is to develop a composition of a composition having improved physical and mechanical properties, as well as high waterproofing properties.

The technical result is an increase in the physical and mechanical properties and waterproofing characteristics of the coating, as well as the expansion of the application areas of the claimed composition.

The technical result is achieved by using a composition comprising a polysulfide oligomer, a hydrophobized chalk, a plasticizer, manganese dioxide, and an accelerator, wherein, as a polysulfide oligomer, it contains liquid thiokoles with a number average molecular weight of 1700-5500 and a viscosity at 25 ° C of 7.5-50 Pa * C, as an accelerator, it contains No-hydroxyphenyl-m-phenoxyphenylmethanimine or N-p-methylphenylphenylmethanimine and additionally a solvent that is a mixture of toluene and acetone in a ratio of 60:40 wt.% With the following component ratio:

The essence of the invention consists in using an accelerator containing an azomethine group. The activating effect of the azomethine group on the hydrogen atom of the terminal sulfhydryl groups of the polysulfide oligomer facilitates the process of its vulcanization. The use of azomethine compounds as accelerators ensures regularity of the structure of the vulcanization grid due to deeper oxidation of thiol groups under the action of manganese dioxide. The regularity of the structure, high packing density and narrow molecular weight distribution of interstitial chains of vulcanizates make it possible to obtain materials with high physico-mechanical and waterproofing properties.

In carrying out the claimed invention, the coating, when exposed to water for a long time, under normal conditions, has a lower water absorption level, high physical and mechanical properties, high waterproofing reliability and adhesion to the substrate. As can be seen from Tables 1 and 2, when the content of No-hydroxyphenyl-m-phenoxyphenylmethanimine or N-p-methylphenylphenylmethanimine is less than 0.2 parts by weight. Deterioration of the physical and mechanical properties of the coating and the hydrostability of the coating. An increase in the concentration of the accelerator above 0.6 leads to a decrease in the viability of the formulations. When using manganese dioxide in an amount of less than 9 parts by weight. Decreases the density of the cross-linking of vulcanizate, physico-mechanical and waterproofing properties. The use of more curing agent reduces the viability of the composition. An increase in chalk content above 150 parts by weight. Leads to a decrease in strength indicators and increases the sorption capacity of the coating.

Use of plasticizer in an amount of less than 30 parts by weight It reduces the uniformity of the distribution of the components of the composition and makes it difficult to process the mixtures because of the high viscosity. The increase in the plasticizer content is higher than 60 parts by weight. Reduces strength and waterproofing properties.

The concentration of the solvent is less than 1 part by weight. Deteriorates dispersion of the accelerator into the mixture. Increasing the solvent content by more than 6 parts by weight. Leads to the formation of capillary pores in the coating.

As a polysulfide oligomer, liquid thiokols with a number average molecular weight of 1700-5500 (GOST 12812-80) are used. The viscosity of thiokols at 25 ° C is 7.5-50 Pa * s. Vulcanizing agent - manganese dioxide (GOST 4470-79). The vulcanization accelerator is No-hydroxyphenyl-m-phenoxyphenylmethanimine or N-p-methylphenylphenylmethanimine. No-hydroxyphenyl-m-phenoxyphenylmethanimine is prepared by reacting phenoxybenzaldehyde and 2-hydroxyaniline. It is an orange powder soluble in toluene and acetone. The melting point is 105 ° C. Molecular weight is 276 cu. Elemental composition,% calculated / found: C: 82.61 / 82.59, O: 11.59 / 11.57; H: 0.72 / 0.70; N: 5.07 / 5.04. Structural formula:

It is known to use it as an antioxidant and as an anti-thinner for vulcanized rubbers [Patent RF 2,171,000, MKI C 07 C 251124, C 08 K 5/29, publ. 1998].

N-p-methylphenylphenylmethanimine is prepared by reacting 4-methylaniline and benzaldehyde. It is a light yellow crystal, soluble in toluene and acetone. The melting point is 40 ° C. Molecular weight is 186 cu. Elemental composition,% calculated / found: C: 90.32 / 90.29; H: 2.15 / 2.14; N: 7.52 / 7.50. Structural formula:

[Tankov D.Yu. Diss. Cand. Tech. Sciences, 2003]. The filler is hydrophobized chalk (TU 21-143-84). As a plasticizer, compounds compatible with thiocolol oligomers, for example, flotation-agent-oxal (TU 38 103429-88) and chloroparaffin HP-470 (TU 6-01-16-90) are used as a plasticizer. As a solvent, a mixture of toluene (GOST 14710-78) and acetone (GOST 2768-84) in a ratio of 60:40% by weight is used. This amount of toluene and acetone, due to a favorable ratio of the rates of evaporation of the solvent and the formation of the spatial structure, ensures the solidity of the cured coating.

To produce the composition, a mixing equipment is used to ensure a homogeneous suspension of the components of the mixture. The mixture is applied evenly on the substrate and is kept until completely cured at 15-25 ° C for 7-10 days.

Tests of cured samples are carried out according to known methods: conditional strength and elongation at the time of rupture in accordance with GOST 270-75, hardness in accordance with GOST 263-75, water absorption and adhesion strength with concrete according to GOST 26578-85, viability time according to GOST 12812-80. The rheological properties of the compositions were determined on a RPE-1m rotary viscometer at a shear rate of 1 s ^-1 using a "cylinder-cylinder" measuring cell at 23 ± 2 ° C. The density of effective and chemical cross-links was determined by the Cluff-Glading method in modulus of compression of swollen and non-swelled samples [Gluff FS, Gladding MK, Parisor RA new method for measuring the degree of crosslinking in elastomers. - J. Polim. Sci. 1960. V.45. №e. - P.341-345].

The composition and properties of the sealing and waterproofing composition are shown in Tables 1 and 2.

Example 1. 100 g of a polysulphide oligomer, 30 g of a plasticizer (in this example chloroparaffin HP-470), 90 g of hydrophobized chalk and 0.2 g of No-hydroxyphenyl-m-phenoxyphenylmethanimine, previously dissolved in 1 G of solvent. The mill is turned on and dispersed for 3-5 hours. The resulting mass is discharged into a beaker, 9 g of manganese dioxide is added, mixed by hand for 5 minutes, then poured into a mold. The composition is kept until completely cured for 7-10 days at 25 ° C.

In a similar manner to Example 1, the compositions of Examples 2-8 are prepared, the composition of which is indicated in Table 1 and the properties in Table 2.

As can be seen from Table 2, compositions of the composition of Examples 1-4 have the best results.

An example of a prototype. 100 parts by weight Polysulfide oligomer is mixed with 79 parts by weight. Titanium dioxide, with 16 parts by weight. Hydrophobized chalk, with 4.3 parts by weight. Aerosil, with 0.7 parts by weight. Polyethylene glycol adipate, with 8.8 parts by weight. Manganese dioxide, with 0.9 parts by weight. Stearic acid, with 2.7 parts of Diphenylguanidine and 9.5 parts by weight. Dioxane alcohols and their high-boiling esters at room temperature until a uniform mass is formed. Vulcanization is carried out in two stages: at 20 ° C 24 hours and 70 ° C for 24 hours.

Thus, the present composition provides an elastomeric material with increased waterproofing and physico-mechanical properties. The composition can be used to create sealing, waterproofing and roofing coatings. Sufficient thixotropy of the composition and the properties of the coating make it possible to use the composition to seal the vertical junctions of concrete bases.

Table 2.
Index	Example								Prototype
	1	2	3	4	5	6th	7th	8	9
Viscosity (23 ± 2 ° С), Pa * s	196	194	192	194	190	180	200	197	215
Pot life, min	120	115	110	110	130	105	110	100	110
Shore A hardness, conventional units.	56	60	58	60	54	60	56	60	54
Conditional tensile strength, MPa	2.44	2.46	2.43	2.50	2.06	2.47	2.26	2.35	1.14
Relative extension, %	320	330	330	320	340	320	310	310	310
Relative residual elongation after rupture,%	4	4	4	4	6th	4	4	5	6th
Conditional tear strength, kN / m	1.331	1.349	1,341	1,340	1,201	1,345	1.331	1,335	1,210
Strength of adhesion to concrete, MPa	0.64	0.64	0.64	0.65	0.62	0.64	0.63	0.64	0.61
Water absorption, mass%
At 23 + 2 ° C
After 1 day	1.4	1.3	1.4	1.5	2.3	1.3	1.5	1.7	2.6
After 120 days	17.1	16.8	17.1	17.3	18	17.0	17.4	17.5	25.2
The density of effective chains * 10 4 , mol / cm 3	2.3	2.5	2.4	2.2	2.0	1.9	2.2	2.1	1.80

CLAIM

A sealing and waterproofing composition comprising a polysulphide oligomer, a hydrophobized chalk, a plasticizer, manganese dioxide and an accelerator, characterized in that as a polysulfide oligomer, it contains liquid thiokols with a number average molecular weight of 1700-5500 and a viscosity at 25 ° C of 7.5-50 Pa · C, as an accelerator, it contains No-hydroxyphenyl-m-phenoxyphenylmethanimine or N-p-methylphenylphenylmethanimine and, additionally, a solvent that is a mixture of toluene and acetone in a ratio of 60:40% by weight, with the following component ratio, mass parts:

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Publication date 17.01.2007gg

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