The polymerized composite material

 

(57) Abstract:

The polymerized composite material for application mainly protective coatings contains methyl methacrylate, polybutylmethacrylate, polyisocyanate, perchlorovinyl resin, a polymerization initiator, a polymerization catalyst, amine and modifying additive. To obtain a homogeneous quality corrosion resistant coatings on large products and engineering mainly operated in conditions of tropical climate, it contains the modifying additive in the form of aliphatic polyhydric alcohols, or esters of such alcohols and phosphoric acid, or mixtures of these alcohols and the above-mentioned phosphates of these alcohols, and the ingredients are taken in the following ratio, wt.h.: the methyl methacrylate 100, polybutylmethacrylate 3 - 65, the polyisocyanate 1 - 75, perchlorovinyl resin of 0.1 to 50, the polymerization initiator is 0.1 to 15, the polymerization catalyst is 0.05 - 5, Amin 0.01 to 5, modifying agent, 0.1 to 15. 2 C.p. f-crystals, 2 tab.

The invention relates to the qualitative and quantitative composition of the polymerized compositions on the basis of methyl methacrylate, which are:

for the application of predominantly acid - the BR>
- tanks for storage of acids and alkalis,

- internal and external surfaces of pipelines for transporting and

- road and rail tanks and the vessel's tanks for the transport of solutions of acids and alkalis;

as the fundamentals of corrosion and antiobrastayuschim coatings bottoms and propellers of ships (preferably sea and particularly preferably - type "river-sea");

as the basis of a corrosion-resistant electrically insulating protective coating electroplating bath, etc.;

as an adhesive or sealant mainly for the connection of metal products with each other or with concrete and for sealing (in particular, waterproofing) joints of metal, concrete and reinforced concrete structures.

Coverage of (or based on) the proposed material can be applied as in the final stages of manufacture or construction of the protected products or facilities, and during their repair (including underwater).

Moreover, the material can be used directly as a lacquer, or in combination with suitable mainly fine fillers.

As can be seen from the description, respectively, these materials shall meet the complex systematically tightening hardly compatible requirements.

Indeed, it is desirable that these materials:

first, it provided as much as possible protective effect in particular conditions of use;

secondly, could be made from commercially available ingredients;

thirdly, almost did not require the expenditure of energy on curing the applied wet coating.

Separate fulfill these requirements does not pose significant difficulties.

Indeed, the well-known ability of oligoesters or mixtures of acrylic mono - and polymers are widely used as the basis of the polymerized composite materials, dried at room temperature and often at much lower temperatures (see, for example: US patent 2452669, 1949; Bagdasarian H. S. Theory of radical polymerization. - M.: Publishing House. AN SSSR, 1959).

Well known for their high chemical resistance to most inorganic and organic acids and bases (see, for example: Polyakov, K. A. chemical-resistant Nonmetallic materials. - M.: Goskomizdat, 1950).

However, to improve the weather-, water - and and the eating and/or reactive additives, which can hardly be called otherwise than exotic.

For example, to increase the corrosion resistance of the finished coating oligoamine curable composition is injected from 10 to 100 mass parts (hereinafter wt. h) glass flakes, the average thickness of which can be selected in the range of 0.5 to 5.0 μm, and the average diameter is in the range 100-400 μm, or a mixture of 10-70 wt.h. these glass flakes with 10-150 wt.h. scaly metal pigment (see US patent 4363889).

The receipt of such fillers is very time consuming.

A few more available on the market chemically resistant fillers type mica like micaceous iron pigments (E. Carter Micaceous iron oxide pigment in high performance coating//POLVMER PAINT COLOUR JOURNAL, 1986, v.176, N 4164, p.226, 228, 230, 232, 234).

However, their use significantly increases the cost protected from corrosion products or engineering structures and, hence, it is appropriate only in those cases where the possible loss from the output of such products or structures of the system outweigh the cost of protection.

So basically the attention of the producers of materials for anticorrosive coatings aimed at the development of such curable materials that fully meet the torus following proposed new invention, provided for use as filler basalt scale and complex polymerized complexes (see, in particular, the patents of the USSR 1825510, 1825511, 1825514, 1831870 and 1831871 and the patent of Russia 2028347).

Among the polymerized composite materials of this type to offer the closest reactive composition consisting of polymers, monomers, polymerization initiators, and other active ingredients known from the description of the invention, "Water - and crack-resistant polymer composition" (patent of the USSR 1831870).

This curable composition contains, by weight. including:

The methyl methacrylate - 100

Polybutylmethacrylate - 5-100

The polyisocyanate - 10-70

Perchlorovinyl resin and 0.1 - 50

The polymerization initiator is 0.1 to 10

The polymerization catalyst is 0.05-2

The divinylbenzene and 0.5-15

Diethanolamine - 0,01-1,5

Amin - 0,1-5

This composition is very effective in the manufacture of coating materials of high heat resistance by using as filler from 5 to 400 wt. including activated basalt scales. This increase in resistance was achieved by the use of integrated modifying additives containing divinizes the time, as a means of partial blocking chemical activity MDI.

However, even if taken in the form of varnish, without filler, known composition has less vitality than above ambient temperature and the more actively used filler. So, at a temperature of about 18-25oC its viability does not exceed 30 minutes

Further, as divinylbenzene capable of intense radical polymerization even at low (less than 0oC) temperatures, and diethanolamine hardly compatible with the basic ingredients of the curable composition and therefore may not significantly weaken the chemical activity of MDI, insofar processes matching circuits formed of polymethyl methacrylate-divinylbenzene and education polyurethane occur substantially independently from one another.

Ultimately hampered the formation of a homogeneous quality coatings on large area (about 10 square meters) products or structures.

In connection with the stated basis of the invention is by improving the quality of the composition and changes in the ratio of ingredients to create such polimerizuet what s more uniform in quality corrosion resistant coatings on large products and engineering mainly operated in conditions of tropical climate.

The problem is solved by the fact that the polymerized composite material for application mainly protective coatings containing methyl methacrylate, polybutylmethacrylate, polyisocyanate, perchlorovinyl resin, a polymerization initiator, a polymerization catalyst, amine and modifying additive according to the invention contains the modifying additive in the form of aliphatic polyhydric alcohols, or esters of such alcohols and phosphoric acid, or mixtures of these alcohols and the above-mentioned phosphates of these alcohols, and the ingredients are taken in the following ratio, wt. including:

The methyl methacrylate (MMA) - 100

Polybutylmethacrylate (PBMA) - 3-65

The polyisocyanate (PI) - 1-75

Perchlorovinyl resin (PHS) is 0.1-50

The polymerization initiator (PI), and 0.1 - 15

Catalyst polymerization (KP) is 0.05-5

Amin is 0.01-5

Modifying additive (MD) - 0,1-15

(in brackets are the abbreviations used in the future in the same clear from the above text values).

These polyhydric alcohols, or phosphates, or mixtures of such alcohols and their phosphates are well compatible with the rest in the above ratio gives an opportunity not only to weaken the chemical activity of polyisocyanates and thereby significantly increase the viability of the total composition, but to get through the regulation of the speed of hardening the three-dimensional structure of the transverse cross-linked polyurethane and linear macromolecules of polymethylmethacrylate, which are randomly distributed in the volume of polyurethane and are "valves". Of course, that the proposed curable composite material suitable for the production of homogeneous quality coatings on large area products or facilities and that such coatings can be made in the form of lacquer films, and using an arbitrary solid dispersed fillers.

The first additional difference is that the polymerized composite material according to the invention as an amine contains 2,4,6-triamino-1,3,5-triazine (melamine).

This amine is the most effective means of controlling the speed of curing (and therefore viability) proposed the polymerized composite material containing the modifying additive according to the invention (especially in the case where the composition contains phosphates polyhydric alcohols). In addition, the use of the amine improves heat and weather resistance of protective coatings.

Versajette amine comprises a mixture of melamine and bis-(4-amino-3-chlorophenyl)-methane (diameter-X).

This mixture of amines in relation to the proposed curable composite material is the most effective finisher MDI, almost completely blocking isocyanate groups and, thereby, precluding the emergence of gas inclusions inside surfaces and the interaction of the coating with oxygen and moisture of the air.

Further, the invention is illustrated:

specific examples of the proposed composition of the polymerized material (see tab. 1),

description of the method of manufacturing,

examples of the coating and the results of comparative tests.

As can be seen from the table. 1, examples 1 and 8 are compositions in which the ratio of ingredients is outside the claimed range; examples 2 and 7 to compositions in which the ratio of ingredients corresponds to the boundaries of the claimed range; other examples set the ratio within the boundaries of the claimed range, and example 9 relates to the best variant embodiment of the inventive concept according to the patent of the USSR 1831870 and are shown here for comparison.

Obviously, listed in table. 1 specific ingredients in no way limit the ability to implement the s along with these can be used butanediol, terity type L - or D-erythritol and entity type L - or D-arabitol and their alkyl substituted derivatives, exity, polyvinyl alcohol, etc.;

as the ethers of polyhydric aliphatic alcohols and phosphoric acid along with these can be used phosphates listed in the previous paragraph alcohols;

as initiators of polymerization along with these can be used and other organic peroxides and gidroperekisi, diazoamino-, azo - and isothiazolinone, tetrazene etc.;

as polymerization catalysts along with these can be used methylaniline, organic salts of divalent iron and so on;

as amines along with these can be used commercially available tribunil and dimethylbenzylamine.

The choice of specific ingredients of the specified type in accordance with the inventive concept may exercise specialist with knowledge in the chemistry and technology of polymers and common experience in paint manufacturing.

A method of manufacturing the proposed curable composite material in General involves three basic steps:

in the first stage, prepare a mixture of metalmaterial, Amin and modifying additives.

- rated amount of powdered polybutylmethacrylate and perchlorovinyl resin mix,

- the resulting mixture was dissolved in a total volume of methyl methacrylate (usually under stirring and, if necessary, to accelerate the dissolution, when it increased to 40-45oC temperature) and

- in the resulting viscous solution of the polymer make a calculated quantity of the selected polymerization catalyst, amine and modifying additives;

at the second stage in the previously obtained mixture make estimated number of MDI and preparation of the reaction mixture is again thoroughly mixed and

the final third stage, make the polymerization initiator and again thoroughly stirred the reaction mixture in order to avoid local overheating.

The obtained curable composite material can then be known to specialists used:

or as a varnish for a protective coating,

or as water-, acid - and alkali-resistant adhesive or sealant (including for repairs under water),

or as a binder for corrosion and/or wear-resistant paints containing artificial pigments prikovannyj, for example, fibrous materials, plastics for the manufacture of shell structures or for repair mainly sheet metal products (in particular, deck the decks and bulkheads of marine and river vessels).

The mixture of ingredients obtained in the first stage, can be stored long-term (not less than six months in a tropical climate) as part of the 1st composite material has been changed, and the polyisocyanate and the chosen polymerization initiator in the required doses can be stored separately, respectively, as the 2nd and 3rd part of this same material. Such parts can be mixed immediately prior to use. The specific formulations of these parts for any of these applications in accordance with the inventive concept can be picked up by the chemist with experience.

Naturally, in cases involving the imposition of any of dispersed fillers, their settlement amounts can be made either at the first stage of preparation of the polymerized composite material (ingredient 1 part), or ex tempora.

In the cases of the fillers of the type filaments, bundles of continuous fibers or filaments, technical the ed laying (or laying) on the protected surface (or form), using fully prepared curable composite material.

In accordance with the formulations 1-8 and formula 9 according to table 1 were manufactured unfilled samples suggested the polymerized composite material and, accordingly, the samples filled with basalt scales of the polymerized composite material of the prototype, namely:

to test for viability - in the form of freshly prepared in chemical glasses with a capacity of 150 ml of the polymerized compositions weighing 100 g each;

to determine the specific toughness in the form of solidified within 10 days at room temperature bars with dimensions of 100 x 10 x 5 mm, respectively, the length, width and thickness;

to determine the adhesion to the metal substrate in the form of adhesive layers utverzhdenii within 10 days of the polymer mass thickness of about 80-100 microns between glued on the lower ends of the steel parts, which had the form of a stepped cylinder with a total length of 25 mm, 35 mm in diameter and 5 mm thick in parts, to be used later for clamping in a tensile testing machine, and a diameter of 25 mm in the remaining part;

to determine the corrosion rate of 3% aqueous solution of chloride by matricardi plate of low carbon steel length 100, a width of 60 and a thickness of 3 mm;

to determine thermal stability on derivatograph PAULIK-PAULIK-ER - DY (Hungary) - in the form of micro-doses (initial mass to 0.5 g each) filled in the standard crucible and solidified within 10 days of the trial.

These samples were used for testing according to the following methods:

viability was determined by well-known through time, which has elapsed from the moment of adoption of the proposed composition of the initiator of polymerization before gelation;

specific impact strength was determined on a standard pendulum impact-testing machine (in particular according to GOST 4647-80 "Plastic");

adhesion to the metal substrate was determined on discontinuous machines (in particular according to GOST 14760-69 "Method for the determination of strength at the margin");

the rate of corrosion in 3% aqueous solution of sodium chloride was determined in a laboratory setup, ensuring the removal of the electrochemical potentiodynamic curves with subsequent calculation of the corrosion rate by well-known specialists formula (see, for example, Damascene B. B., Petri O. A. Russ. - M.: Vysshaya SHKOLA, 1987);

the resistance on the specified derivatograph was determined by continuous monitoring of the mass of the samples is as smooth POI known composite materials, representing the average for the standard series of samples are presented in table. 2.

Industrial applicability the proposed curable composite material mainly in the tropical environment is evident from the data given in table. 2.

As can be seen from it, the viability of the proposed curable composite material at 40oC in one of the examples is 45 minutes, and in the worst examples is not less than 25 minutes, whereas the known composition in the same environment becomes unsuitable for coating the gel for 5 minutes. Thereby creates the prerequisites for obtaining a substantially more uniform physical and mechanical properties of coatings.

Then, with a slight advantage in comparison with known composition on the adhesion strength and heat resistance of the proposed composite material is significantly more impact-resistant and resistant to corrosive environment.

1. The polymerized composite material for application mainly protective coatings containing methyl methacrylate, polybutylmethacrylate, polyisocyanate, perchlorovinyl resin is h contains the modifying additive in the form of aliphatic polyhydric alcohols, or esters of such alcohols and phosphoric acid, or mixtures of these alcohols and the above-mentioned phosphates of these alcohols, and the ingredients are taken in the following ratio, wt. including:

The methyl methacrylate (MMA) - 100

Polybutylmethacrylate (PBMA) - 3 - 65

The polyisocyanate (PI) - 1 - 75

Perchlorovinyl resin (PHS) is 0.1 - 50

The polymerization initiator (PI), and 0.1 - 15

Catalyst polymerization (KP) is 0.05 - 5

Amin is 0.01 - 5

Modifying additive (MD) - 0,1 - 15

2. The material under item 1, characterized in that it contains amine 2,4,6-triamino-1,3,5-triazine (melamine).

3. The material on p. 2, characterized in that the amine as it contains a mixture of melamine and bis-(4-amino-3-chlorophenyl)-methane.

 

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