Method of production of sealing composition

FIELD: manufacture of sealing materials on base of liquid thiocol for sealing-up fuel compartments and structural members of flying vehicles; aerospace engineering; automobile manufacture; shipbuilding.

SUBSTANCE: proposed method includes mixing the sealing and vulcanizing pastes containing dibutyl phthalate with vulcanization accelerating agent; prior to preparation of vulcanizing paste, carbon nano-modifying agents are additionally introduced into dibutyl phthalate and dispersion thus obtained is treated by ultrasound. Used as carbon nano-modifying agents is fulleroid multi-layer nano-modifying agent Astralene or open carbon nano-tubes in the amount of 0.037-0.069 or 0.014-0.020 parts by mass, respectively per 100 parts by mass of vulcanizing paste.

EFFECT: enhanced tensile strength; reduction of relative elongation; enhanced fuel resistance properties and fungus resistance.

3 cl, 1 tbl, 8 ex

 

The invention relates to the field of sealing materials based on liquid Thiokol, which can be used for sealing the fuel compartments and structural elements of aircraft in aerospace, automobile and shipbuilding and other industries.

A method of obtaining sealing compositions performed by mixing the sealant and curing pastes when the mass ratio of sealing and curing pastes from 1:1 to 20:1. Sealing paste contains polysulfide oligomer, filler, adhesive, diakidoy ester of phthalic acid, pigment. Vulcanizing paste contains manganese dioxide, diakidoy ester of phthalic acid, a filler and a vulcanization accelerator (RF patent No. 2205197).

The disadvantages of sealing compositions obtained in this way are not sufficiently high tensile strength and low teplostoykost.

The closest analogue adopted for the prototype, is a method for sealing compositions by mixing of sealant, including liquid Thiokol, filler and adhesive additives, and curing the paste, in which the liquid Thiokol pre-treated aqueous saturated solution of FeCl3based 0.24 to 0.34 weight. including FeCl3*6N About 100 weight. hours of Thiokol at 70° within 2 hours (ASV of the USSR №1002340).

The disadvantages of sealing compositions obtained by the method prototype, are not sufficiently high tensile strength, high residual elongation and low teplostoykost and funginertness.

The technical task of the invention is to develop a method of producing a sealing composition with increased tensile strength, low elongation and high teplostoykost and funginertness.

For the technical solution method for obtaining sealing compositions based on liquid Thiokol by mixing pre-cooked sealing paste and curing the paste, including dibutyl phthalate, vulcanization accelerator, in which during preparation of vulcanizing paste in dibutyl impose additional carbon nanomodifiers and thus obtained dispersion is treated with ultrasound. As carbon nanomodifiers use of fulleroid multilayer nano modifiers Astral in the number 0,037-0,069 parts by weight, or from - 0,037-0,069 parts by weight or open the multilayer nanotubes in an amount of 0.014 at 0.020 parts by weight per 100 parts by weight of vulcanizing paste.

Introduction carbon nanomodifiers as modifying debauchery receiving a sealing composition causes an increase in strength at break, and teplostoykost and gribomont. The modifying additive is introduced into the plasticizer is dibutyl phthalate in the preparation of vulcanizing paste. To improve the dispersive ability of the pigment modifying additives and reducing the duration of the process of obtaining sealing compositions proposed ultrasonic effect.

Wetting and spreading of the sealant composition on the substrate surface followed by surface diffusion, migration of molecules of carbon nanomodifiers to the surface. The components of the sealant composition and the substrate have a functional group capable of interaction with carbon nanomodifiers due to their high activity.

Introduction carbon nanomodifiers linking not entered into the stitching free radicals polymer, prevents the leaching of filler and other components of vulcanized material and, thereby, allows to increase teplostoykost.

The technical result of the claimed invention is achieved by the use of any carbon nanomodifiers, but it is most preferable to use a multilayer fulleroid the Astral modifier necessary for THE 31968474.1319.001-2000 and open the multilayer nanotubes on THE 31968474.1319.001-2000. In embodiments were used fulleroid multilayer nanomodified the tor Astral with a carbon content not less than 99.99%, with an average particle size of 80-150 nm and the interlayer distance of 3.42 angstroms and open multilayer nanotubes with carbon content of not less than 99,999%, with 80% of open ends and an average pore size of 2-4 nm.

Examples of implementation

Example 1.

According to the invention is prepared vulcanizing paste to get teplostojkogo sealant WAS-5, which in 5,062 parts by weight of plasticizer is dibutyl phthalate enter 0,037 parts by weight of fulleroid multi-layered nano modifiers Astralene, and the resulting dispersion is subjected to ultrasonic stimulation of installing USSN (TU 25-7401.0027-88) with a frequency of 22 kHz for 15 minutes then mix 5,099 parts by weight of the obtained dispersion of nano modifiers in dibutyl phthalate, to 6.67 parts by weight of manganese dioxide, of 0.03 parts by weight of stearic acid and 0.2 parts by weight of Aerosil.

Then prepare a sealing paste by mixing and 70.5 parts by weight of Thiokol brand UXO-2, and 4.8 parts by weight of epoxy resin e-40 and 24.7 parts by weight of carbon black, and then mix the resulting sealing and curing the paste and add 0,8 M.Ch. of a vulcanization accelerator of diphenylguanidine.

The method of preparation of the sealing compositions in examples 2,3 analogous to example 1, but in example 2, in dibutyl enter 0,049 parts by weight of Astralene, as in the example 3-0,020 parts by weight of opened carbon nanotubes.

Example 5.

According to the invention is prepared vulcanizing n the STU to get the sealant VITAP-1, working in an air environment, which in 5,866 parts by weight of dibutyl phthalate enter 0,014 parts by weight of opened multi-layered nanotubes and the resulting dispersion is treated with ultrasound, as in example 1. Then mix 5,88 parts by weight of the obtained dispersion of nano modifiers in dibutyl phthalate, is 2.88 parts by weight of epoxy resin e-40, 2,11 parts by weight of red iron oxide and of 1.13 parts by weight of aqueous solution of sodium bichromate. Then prepare a sealing paste by mixing 75,1 parts by weight of Thiokol brand UXO-2, 14,27 parts by weight of titanium dioxide, 8,84 parts by weight of chalk active and 1.79 parts by weight of phenol-formaldehyde resin, and then mix the resulting sealing and curing paste and add 0,8 M.Ch. of a vulcanization accelerator of diphenylguanidine.

The method of preparation of the sealing compositions according to examples 6, 7 is similar to example 5, and example 6 in dibutyl enter 0,017 parts by weight of opened carbon nanotubes, and in the example 7-0,069 parts by weight of fulleroid multi-layered nano modifiers Astralene.

The number of carbon nanomodifiers given in terms of 100 parts by weight of vulcanizing paste. The mass ratio of sealing and curing pastes is 100:(5-12).

Examples 4 and 8 prototype.

The properties of the vulcanizates are shown in table. As can be seen from table 2, the claimed method of obtaining a sealing composition allows to obtain a sealant with a high in the middle is m 20-40% strength at break in comparison with the prototype. No shrinkage (reduced 2-3 times the residual elongation) of vulcanizates, the persistence of high levels of physical and mechanical properties after aging in the fuel at a temperature of 100°With over 600 hours, and improved funginertness (score of 4 is "bad", grade 3 - satisfactory grade 2 - good) lets talk about better quality material.

Application of the proposed method of obtaining sealing compositions will improve the reliability of sealing coatings integral tanks and glazing aircraft.

Table
PropertiesExamples according to the invention
U-MS-5VITAP-1
12345678
The tensile strength, kg/cm230,032,028,022,031,032,032,818,0
Elongation, %160180170260200200213355
Relative residual elongation,% 2005,80005,9
Hardness shore a, usled4155554860606260
Funginertness, score32243333
Teplostoykost (after soaking in fuel TS-1 at a temperature of 100°With over 600 hours)
The tensile strength, kg/cm229,732,028,515,5----
Elongation, %160179175300----
Relative residual elongation, %20012----

1. A method of obtaining a sealing compositions based on liquid t the stake by mixing pre-cooked sealing paste and curing the paste, including dibutyl phthalate, vulcanization accelerator - diphenylguanidine, characterized in that in the preparation of vulcanizing paste in dibutyl impose additional carbon nanomodifiers and thus obtained dispersion is treated with ultrasound.

2. A method of obtaining a sealing composition according to claim 1, characterized in that the carbon nano modifiers use fulleroid multilayer nano modifiers Astral in the number 0,037-0,069 parts by weight per 100 parts by weight of vulcanizing paste.

3. A method of obtaining a sealing composition according to claim 1, characterized in that the carbon nano modifiers use open multilayer nanotubes in an amount of 0.014 at 0.020 parts by weight per 100 parts by weight of vulcanizing paste.



 

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