Rubber mixture

FIELD: chemistry; rubber industry.

SUBSTANCE: invention pertains to rubber mixtures based on fluoroprene, used for making rubber goods, which can work in conditions affected by fuel and used in the motor-car industry. The rubber mixture consists of a vinylidene fluoride terpolymer and tetrafluoroethylene, magnesium oxide, calcium hydroxide, technical carbon T-900, di-(4hydroxyphenyl)dimethylmethane, pentaerythritol tetrastearate, dibutyl sebacate and a catalyst. The catalyst used is in the form of guanidine quaternary salts, and more specifically, guanidine bromide or chloride. The catalyst is a compound obtained from interaction of phenyl-bi-guanidine hydrochloride or hydrobromide with lower bromide or ethyl chloride, with molar ratio of 1:7 in the presence of a base. The catalyst is taken in percentage mass ratios of 0.5-0.7% at 100% mass of terpolymer.

EFFECT: increased rate of vulcanisation of rubber mixtures; wide range of catalysts for fluoroprene.

3 tbl, 2 ex


The invention relates to the development of rubber compounds based on silicone elastomer used for the manufacture of rubber products (rings, gaskets, fuel hoses), working in the conditions of influence of fuel used in the automotive industry.

Known rubber compound using for vulcanization of ftorkauchukov copolymers of hexaferrite with vinylidenefluoride, as well as other ferreirae catalysts (accelerators) of compounds such as Nitron and their salts, crown ethers (Nudelman Z.N., Lavrov L.N., Dontsov A.A. Vulcanization ftorkauchukov acid reagents. Rubber & rubber, No. 10, 1983, p.40-41).

In rubber mixtures based ftorkauchukov as catalysts can be used other compounds, namely, Quaternary ammonium, postname and archieve salt (Nudelman Z.N., Lavrov L.N., Dontsov A.A. Vulcanization ftorkauchukov acid reagents. Rubber & rubber, No. 10, 1983, p.40-41; RF Patent 2097393, 27.11.1997).

Famous recipe rubber compound 4930 - 103, intended for manufacturing of range of the fuel hose low toplivopriemniki with an inner diameter of 7,94-15,5 mm, corresponding to the standard Euro 3 (TU 2556-119-00149289-2001, THE 305-57-089-95) based on fluoro GFR-264/3 (terpolymer of vinylidenefluoride, hexaferrite and tetrafluoroethylene), according to the ARTICLE the 044-410-2003. The rubber mixture contains fluoropolymer elastomer GFR-264, binding di-(4 oksifenil)dimethylmethane (bisphenol a), a catalyst bromide octamethyltetrasiloxane, magnesium oxide MgO RA-150, calcium hydroxide Caldic 2000, dispersers Aflux-54 (tetrastearate pentaerythritol) and dibutylsebacate, carbon black T-900 (N.G. Morozova, martyusgov GG, Kochetkova, GV, Sokolov V.E., Ganina T., Konovalov TR, Pichhadze SJ "Rubber compound rubber-based GFR-264 for internal camera hoses low toplivopriemniki." (In the collection "XII international scientific-practical conference. Rubber industry. The raw materials. Materials. Technologies". M.: OOO "STC NISP". 2006. - c.129-130)).

The closest analogue is the rubber mixture on the basis of high and low molecular weight copolymers of vinylidenefluoride with HEXAFLUOROPROPYLENE containing carbon (carbon black) and mineral (barium sulfate) fillers, crosslinking agent, bisphenol a, magnesium oxide, calcium hydroxide, catalyst triphenylmethylchloride, dispersant therapeutically pentaerythritol (RF Patent 2220989 C2, 10.01.2004) prototype. This rubber compound is enough technology, however, requires increasing the rate of vulcanization.

The technical result of the invention is to increase the rate of vulcanization of the rubber mixtures based Tripoli the development of vinylidenefluoride, hexaferrite and tetrafluoroethylene and expanding Arsenal of substances having catalytic activity to perkowska in the process of vulcanization.

This technical result is achieved by creating a rubber mixtures based terpolymers of vinylidenefluoride, hexaferrite and tetrafluoroethylene, in which the catalyst used Quaternary salt biguanidine General formula:

where Hal Is Cl, Br.

EXAMPLE 1. The synthesis of the salts biguanidine.

1 pray hydrochloride phenylpyrimidine add 7 moles bromatologia ethyl, boiled for 4 hours in a water bath in the presence of a base (NaOH 30% aqueous solution), the reaction mixture cooled down to room temperature, the precipitate was separated and crystallized from benzene. Get the connection

the number of 363 g (the yield of the target product, 80%) as a grey amorphous powder with a melting point 120-123°C.

Elemental analysis data. C22H40N5Br, calculated, %: C - 58,15; N - 8,81; N - 15,41; Br - 17,62, found, %: C - 57,85; N At 8.60; N - 15,51; Br - 17,37.

An NMR spectrum1H recorded on the instrument Bruker WM-250, solvent DMSO-d6, internal standard TMS: 1,03 ppm soof 1.13 ppm, soof 1.27 ppm, sois 3.08 ppm sq 3,37 ppm USSof 3.85 ppm sq7,21-7,30 PM (3H, C6H5), 7,40-7,50 m (2N, C6H5).

Similarly receive the connection

showing similar catalytic activity.

As the catalyst of comparison we used the connection:

The kinetic characteristics of the process of vulcanization of the rubber mixture 4930 for the various catalysts are shown in table 1.

Comparison of the kinetic characteristics of cured using salt I, II and III shows increased speed of vulcanization for salt I and II in comparison with salt III (prototipo).

Table 1

The kinetic characteristics of the investigated rubber blends (Rheometer of the company "Monsanto", 175°C for 12 min, the amplitude of the oscillations of the rotor 3°)
IndexI bromide biguanidineII chloride biguanidineIII bromide actualitate-aminophosphine (prototyp)
ts2, min0,540,571,00
MmaxN·m8,49 8,538,32
T'90, min2,112,152,52
T'50, min1,261,281,39
Note: ts2min - the start time of vulcanization,

MminN·m - minimum torque,

MmaxN·m - maximum torque

t'90, min - time optimum vulcanization,

t'50, min - time 50% vulcanization.

EXAMPLE 2. Analysis of rubber compounds.

The object of research was the rubber mixture 4930 according to the recipe, parts by weight, % on 100 parts weight of rubber: SCF-264 (terpolymer of vinylidenefluoride, hexaferrite and tetrafluoroethylene) - 100%, magnesium oxide - 3%, calcium hydroxide - 6%, carbon black T-900-30%, Aflux-54 (1.5%), dibutylsebacate - 1.5%), bisphenol a is 1.5%, the catalyst is 0.5%.

The mixture is prepared in the mill according to the following mode: roll rubber GFR-264 for 1 min, then injected into the rubber sequentially magnesium oxide (5 min), calcium hydroxide (7 min), carbon black (6 min), bisphenol a (5 min), the dispersant (5 min) and the catalyst (6 min).

The mixture is prepared by passing it 3-4 times through the rollers with a gap between the rollers 0.5-0.8 mm, resulting in the preparation of a thickness of 3 mm, which is then spazout on extrusion equipment in the manufacture per the CSO layer (inner chamber) fuel hoses thickness 0,4-0,8 mm

The compositions of the samples investigated rubber blends are given in table 2 and the results of their physico-chemical tests in table 3.

As can be seen from table 3, the inventive rubber mixture has the technical characteristics correspond to the norm, and conditional tensile strength and relative elongation superior to the prototype.

Table 2

The samples investigated rubber blends
№ p/pIngredientsThe contents of the ingredients, parts by weight
the placeholder12345
1Terpolymer of vinylidenefluoride, hexaferrite, tetrafluoroethylene100100100100100100
2Magnesium oxide355426
3Calcium hydroxide668759
4Carbon T-9003030252717
5Di-(4 oksifenil)dimethylmethane1,51,51,71,60,71,1
6Tetrastearate pentaerythritol1,01,01,51,250,91,6

Table 3

Physico-mechanical properties of rubbers THAT 2556-119-00149289-2001, THE 305-57-089-95
p/pIndexNormathe placeholder12345
1Hardness according to ISO, the international unit IRHD75±5737572747675
2Conditional tensile strength of not less kgf/cm2 61676869706065
3Elongation at break, %, not less than160168180200210170167
4Relative residual deformation when compressed by 25% after 24 hours at 100°C, %, max504845,646,9445355

The rubber mixture, comprising terpolymer of vinylidenefluoride, hexaferrite and tetrafluoroethylene, a crosslinking agent di(4 oksifenil) dimethylmethane, vulcanization activators - magnesium oxide and calcium hydroxide, the filler is carbon black T-900, dispersers - tetrastearate pentaerythritol and dibutylsebacate, the catalyst is a Quaternary salt biguanidine, namely bromide, biguanidine or chloride biguanidine connection, obtained by the interaction of the hydrochloride or hydrobromide phenylpyrimidine with methyl or ethyl chloride, respectively, in a molar ratio of 1:7 in the presence of a base in the following ratio of components, rubber compounds, parts by weight:

terpolymer of vinylidenefluoride, hexafluoro Elena
and tetrafluoroethylene100
magnesium oxide3-5
calcium hydroxide6-8
carbon T-90025-30
di-(4 oksifenil)dimethylmethane1,5-1,7
tetrastearate pentaerythritol1,0-1,5
the specified catalyst0,5-0,7


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