SU1500654A1 - Method of producing mouldable urethane elastomers - Google Patents

Description

The invention relates to the synthesis of urethane elastomers of the injection type and can be used in the mining industry for the manufacture of large thin-walled parts of a complex profile. The invention improves the elastic modulus of elastomers (up to 100 MPa), iznostoykost (up to 0.3 mm - ^ / m), tensile strength (up to 45 MPa), hardness (up to 82 Shore A) _prn preserving elasticity due to the fact that when synthesized as a hydroxyl-containing polyester, it is

use polytetramethylene oxide mol.m. 1000, as diisocyanate - 2,4 toluene diisocyanate, as a hardener - 3,3-dichloro-4,4 '-diaminnodiphenylmethane, and as a plasticizer - dibutyl phthalate, which is previously introduced into the hardener at a molar ratio (0.25-0.85 ): 1 respectively. The synthesis is carried out through the stage of obtaining prepolymer with the content of free isocyanate groups of 2.8-4.1 wt.%, 2 table.

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The invention relates to the synthesis of injection molded elastomers with an improved modulus of elasticity and can be used in the manufacture of large-sized thin-walled products of a complex profile in the mining and other industries.

The purpose of the invention is to increase the modulus of elasticity, wear resistance,

tensile strength, hardness of the elastomer while maintaining its elasticity.

As a source of raw materials used polytetramethylene oxide, bifunctional with a molecular weight of 1000 (PTMO); 3,3'-dichloro-4,4 '-diaminodiphenylmethane (MOKA); ethylene glycol (EG); 2,4-toluenyl isocyanate (TDI);

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dibutyl phthalate (DBP) with solubility = 9.3 cal / cm.

Synthesis of molded urethane elastomer, measures carried out in two stages.

The calculated amount of pre-melted PTMO with molecular mass 1000 is placed in a container and dried at 100 + 5 ° С and with constant stirring under vacuum until the moisture content is less than 0.05%. The estimated amount of TDI is mixed with dried PTMO at 60 ° C. Then the temperature is increased to 80 ° C and at this temperature, the EG is added to the propolymer and the synthesis is carried out for 60 minutes under vacuum to the required content of terminal isocyanate groups (2.84.7 wt.%). Then the temperature of the reaction mixture is reduced to 50 ° C and DBP with MOKA is injected into re-20 actor at the rate of 0.24-0.85 mol. DBP per mole of MOKA and mix for 3 minutes under vacuum. Then liquid polyurethane is poured into molds. Thermostatting is carried out at 120 ° C for 3 minutes.

Note 1 (counter.). G stage - getting prepolymer. ','

5000 g PTMO with a molecular weight of 30 1000 are pre-melted and loaded-. are being fed into the reactor. Drying is carried out at 100 + 5 ° C with constant stirring under vacuum to a moisture content of 0.05% or less. Then the temperature of 35 is reduced to 60 ° C and add 1662 I "

Tdi The synthesis is carried out at 80 ° C for 30 minutes under vacuum to a '50% conversion, isocyanate groups. The finished prepolymer is drained into a container and .40 creates a nitrogen blanket.

Stage 2 - getting elastomer.

To 100 g of the prepolymer obtained in the first stage, with the content of isocyanate groups of 6.0 wt.%, Add 45 18.1 g of molten MOKA. At 50 ^th pergmeshivayut C under vacuum for 3 min. Liquid polyurethane is poured into molds. Temperature control is carried out at 120 ° C for 3 hours.

The compositions in examples 1-21 are given in table. 1 (initial components of the synthesis Per 100 g of prepolymer). ^four

Example 2. (counter.) To 10.0 g of the prepolymer prepared in Example 5-1, add a mixture of 18.1 g of MOKA with 4.52 g of DBP. At 50 ° C, they are stirred for 3 minutes and poured into molds. The thermostabilization is analogous to Example 1.

Properties of polyurethane are presented in table. 2

Example 3 (control). To 100 g of the prepolymer prepared in Example 1, add 18.1 g of MOKA with 9.75 g of DBP. Further synthesis and temperature control, as in example 1.

Example 4 (counter.) To 100 g of the prepolymer obtained in example 1, add 18.1 g of MOKA with 15.7 g of DBP. Further synthesis and thermosetting as in example 1.

Example 5 (counter.) To 100 g of the prepolymer obtained in Example 1, add a mixture of 18.1 g of MOKA with 18.1 g of DBP. Further synthesis and temperature control, as in example 1.

Example 6 (counter.) To 100 g of the prepolymer obtained in example 1, add 1.59 g of EG. At 80 ^ 0, under pressure, the synthesis is carried out until the content of isocyanate groups is 2.8 wt.%. Then the reaction mass is cooled to 50 ° C and add 8.5 g of MOKA. Temperature control, as in example 1,

Example 7. To 100 g of the prepolymer obtained in example 6, add a mixture of 8.5 g of MOKA with 2.2 g of DBP, Further synthesis and temperature control, as in example 1.

Example 8. To 100 g of the prepolymer prepared according to example 6, add a mixture of 8.5 g of MOKA with 4.6 g of DBP. Further synthesis and temperature control, as in example 1.

Example 9. To 100 g of the prepolymer prepared according to example 6, add a mixture of 8.5 g of MOKA with 7.4 g of DBP. Further synthesis and temperature control, as in example 1.

Example 10. To 100 g of the prepolymer prepared according to example 6, add a mixture of 8.5 g of MOKA with 8.5 g of DBP. Further synthesis and temperature control, as in example 1.

Example 11 (counter.) 1.36 g of EG are added to 100 g of prepolymer prepared according to Example 1, synthesis is carried out at 80 ^° C under vacuum until the content of isocyanate groups is 4.1 wt.%. Then the reaction mass is cooled to 50 ° C and add 12.4 g of MOKA. Temperature control as in example 1.

Example 12. To a 100 g prepolymer prepared according to example 11, add a mixture of 12.4 g MOKA and 6.8 g DBP. Further synthesis and temperature control, as in example 1.

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Example 13. To 100 g of prepoly-? the measure obtained in example 11, add 12.4 g of MOKA and 6.7 g of DBP. Further synthesis and thermostating as in example 1.

Example 14. K100g of prepolymer prepared according to Example 11 are added with 12.4 g of MOKA and 10.8 g of DBP. Further synthesis and thermostatic control, as in example 1.

Example 15 (counter.) To 100 g of the prepolymer obtained in example 11, add 12.4 g of MOKA and 12.4 g of DBP. Further synthesis and thermostatic control, as in example 1.

Example 16 (counter.) To 100 g of the prepolymer obtained in Example 1, add 0.9 g of EG. At 80 ° C under vacuum, the synthesis is carried out until the isocyanate groups are kept at 4.7 May.2. Then the reaction mass is cooled to 50 ° C and add 14.2 g of MOKA. Thermostatting, as in example 1.

Example 17. To 100 g of the prepolymer-25mer obtained in Example 16 are added 14.2 g of MOKA and 5.0 g of DBP. Further synthesis and thermostating, as in example 1.

Example 18. To 100 g of prepolymer 30mer prepared according to example 16, 14.2 g of MOKA and 7.6 g of DBP are added. Further synthesis and temperature control, as in example 1.

Example 19. To 100 g of the prepolymer 35mer prepared according to Example 16, 14.2 g of MOKA and 12.4 g of DBP are added. Further synthesis and temperature control, as in example 1.

Example 20: To 100 g of the prepolymer obtained from Example 16, 14.2 g of MOKA and 14.2 g of DBP are added. Further. Synthesis temperature control as in Example 1.

Example 21 (prototype). To 100 g of prepolymer based on polyethylene propylene adipate, m. 2000 and 4.4 * -diphenylmethane diisocyanate (MDI) with a content of isocyanate groups of 3.8 wt.% 1.2 g of EG are added, then 1.8 g of 1,1,1-trimethylolpropane (TMP) and 7.4 g are introduced di-2-ethylhexyl phthalate.

The properties of polyurethane in examples 1-2 ^ are presented in table. 2

Claims (1)

Claim The method of obtaining molded urethane elastomers by reacting polyester with an excess of aromatic diisocyanate, followed by the introduction of ethylene glycol to a content of free ΝΟΟ-groups equal to 2.8-4.1 wt. X and a curing agent in the presence of a plasticizer, characterized in that increase the modulus of elasticity, wear resistance, tensile strength, hardness. elastomer while maintaining its elasticity, polytetramethylenediamine mol.m. 1000, as an aromatic diisocyanate - 2,4 toluenediisocyanate, as a curing agent - 3,3'-dichloro-4,4 ^G- diaminodiphenylmethane, and as a plasticizer - dibutyl phthalate, and dibutyl phthalate is pre-introduced in 3,3 * -dichloro-4 , 4 ¹ - diaminodiphenylmethane with a molar ratio of (0.25-0.85): 1, respectively. 7 1500654 eight but I I about. ABOUT "s kovtr ^ koatr ^ koitri "" vtr- | kokr4kojatr.1 konty koty * khodyoykoyatr 0.977 0 0.25 0.48 0.85 0.977 0 0.24 0.48 0.85 0.977 ten 1500654 • AO SM "a bB - leather dzhontr "1coatr] koitr. CocktailLoiter ^ I | hon vdkoyatr κοκτρΊχοητ ^. m> δ ABOUT • · About “A b. cm sh cm • SM SM - - in - -I and m "about o "s'a" A about "" h o% & a o ** o 3 N * On? Viability