RU2100379C1 - Method for production of binder for road building - Google Patents

Abstract

FIELD: road building. SUBSTANCE: synthetic binder is prepared by cooligomerization of heavy resin of pyrolysis having temperature higher than 200 C with fraction C of pyrolysis, their ratio being 2-3:1. Catalytic complex of titanium tetrachloride and triisobutyl aluminium having ratio of titanium and aluminium 3-6:1 is used for copolymerization. Quantity of said catalyst is 0.35-0.55 mass %. EFFECT: improved efficiency. 1 tbl

Description

 The invention relates to a method for producing a synthetic organic binder for construction.

Known methods for producing a synthetic binder based on polyester epoxy resins [Mikhailov K.V. Paturoev V.V. Chrys R. Polymer concrete and constructions based on them. M. Stroyizdat, 1989, 304 p. Despite their high efficiency, they have significant drawbacks that limit their use: the multicomponent composition (synthetic resin, hardener, plasticizer, hardening accelerator), a narrow temperature range of application and technological viability, comprising 16-40 ^o C and 15-20 min, respectively.

 Known astringent, including petroleum resin, phenolic purification extract and waste polypropylene production. The disadvantage of this binder is the limited raw material base and the presence of the compounding stage of the components.

Closest to the proposed method is binders obtained by catalytic copolymerization of unsaturated pyrolysis fractions of hydrocarbons with a boiling point of 30-260 ^o C in the presence of 0.5-5 wt. Oligomers and polymers of α-olefins C ₈ -C ₃₀ [2]
The disadvantages of this method include
multi-stage process;
difficulties in disposal of toxic catalyst decomposition products.

 The objective of the invention is the creation of a binder with high technical and operational properties, as well as the expansion of the raw material base and the disposal of by-products of pyrolysis.

The technical result is achieved by the fact that the binder is obtained by co-oligomerization of unsaturated compounds contained in a heavy pyrolysis resin with a boiling point above 200 ^° C and a fraction of C ₅ liquid hydrocarbon pyrolysis products, boiling point up to 60 ^° C in the ratio (2-3) 1 in the presence of a tetrachlor catalytic system titanium-triisobutylaluminum in a molar ratio of (3-6) 1 in an amount of 0.35-0.55 wt. The reaction is carried out for 3-4 hours at a temperature of 30-50 ^o C. Then the catalyst is neutralized with isopropyl alcohol in the ratio of catalyst: alcohol 1: 1.2. The distillation of unreacted hydrocarbons is carried out at a temperature of 150 ^o C and 20 mm Hg. Art.

Example 1. In a reactor with a capacity of 1 l serves 700 ml of a mixture of heavy resin (TSP) and fractions C ₅ in a ratio of 2: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor at a Ti: Al ratio of 3: 1 in an amount of 0.35 wt. The reaction is carried out for 3 hours at a temperature of 40 ^o C, after which add 8 ml of isopropyl alcohol and carry out the distillation of unreacted hydrocarbons. Characteristics of the resulting product are shown in the table.

Example 2. In a reactor with a capacity of 1 l serves 700 ml of a mixture of TSP and fraction C ₅ in a ratio of 2: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor with a Ti: Al ratio of 3: 1 in an amount of 0.55 wt. The reaction is carried out for 3 hours at a temperature of 40 ^o C, after which add 13 ml of isopropyl alcohol and carry out the distillation of unreacted hydrocarbons. Characteristics of the resulting product are shown in the table.

Example 3. In a reactor with a capacity of 1 l serves 700 ml of a mixture of TSP and fraction C ₅ in a ratio of 2: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor at a Ti: Al ratio of 6: 1 in an amount of 0.35 wt. The reaction is carried out for 3 hours at a temperature of 40 ^° C., after which 6.5 ml of isopropyl alcohol are added and the unreacted hydrocarbons are distilled off. Characteristics of the resulting product are shown in the table.

Example 4. In a reactor with a capacity of 1 l serves 700 ml of a mixture of TSP and fraction C ₅ in a ratio of 2: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor with a Ti: Al ratio of 6: 1 in an amount of 0.55 wt. The reaction is carried out for 3 hours at a temperature of 40 ^° C., after which 10.4 ml of isopropyl alcohol are added and the unreacted hydrocarbons are distilled off. Characteristics of the resulting product are shown in the table.

Example 5. In a reactor with a capacity of 1 l will submit 700 ml of a mixture of TSP and fraction C ₅ in a ratio of 3: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor at a Ti: Al ratio of 3: 1 in an amount of 0.35 wt. The reaction is carried out for 3 hours at a temperature of 40 ^o C, after which add 8 ml of isopropyl alcohol and carry out the distillation of unreacted hydrocarbons. Characteristics of the resulting product are shown in the table.

Example 6. In a reactor with a capacity of 1 l serves 700 ml of a mixture of TSP and fraction C ₅ in a ratio of 3: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor with a Ti: Al ratio of 3: 1 in an amount of 0.55 wt. The reaction is carried out for 3 hours at a temperature of 40 ^o C, after which add 13 ml of isopropyl alcohol and carry out the distillation of unreacted hydrocarbons. Characteristics of the resulting product are shown in the table.

Example 7. In a reactor with a capacity of 1 l serves 700 ml of a mixture of TSP and fraction C ₅ in a ratio of 3: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor at a Ti: Al ratio of 6: 1 in an amount of 0.35 wt. The reaction is carried out for 3 hours at a temperature of 40 ^° C., after which 6.5 ml of isopropyl alcohol are added and the unreacted hydrocarbons are distilled off. Characteristics of the resulting product are shown in the table.

Example 8. In a reactor with a capacity of 1 l serves 700 ml of a mixture of TSP and fraction C ₅ in a ratio of 3: 1. When the temperature of the mixture reaches 20 ^o C, a TXT-TIBA catalytic complex is introduced into the reactor with a Ti: Al ratio of 6: 1 in an amount of 0.55 wt. The reaction is carried out for 3 hours at a temperature of 40 ^° C., after which 10.4 ml of isopropyl alcohol are added and the unreacted hydrocarbons are distilled off. Characteristics of the resulting product are shown in the table.

Example 9. 700 ml of a mixture of TSP and a C ₅ fraction in a ratio of 2.5: 1 are fed into a 1-liter reactor. Upon reaching a temperature of 20 ^° C, a TXT-TIBA catalytic complex is introduced into the reactor with a Ti: Al ratio of 4: 1 in the amount of 0.4 wt. The reaction is carried out for 3 hours at a temperature of 40 ^o C, after which add 9 ml of isopropyl alcohol and carry out the distillation of unreacted hydrocarbons. Characteristics of the resulting product are shown in the table.

Example 10 In a 1 l reactor is fed a mixture of 700 ml of a PMT (iodine value 53 g, I _2/100 g, the dienes content of 6%) and a C ₅ fraction with a plant EP-60 in a ratio equal to 3: 1. When the temperature of the mixture reaches 20 ^o C, the TXT-TIBA catalytic complex is introduced into the reactor, the reaction is carried out for 3 hours at a temperature of 40 ^o C, after which 10.4 ml of isopropyl alcohol are added and the unreacted hydrocarbons are distilled off. Characteristics of the resulting product are shown in the table.

Example 11 In a 1 l reactor is fed a mixture of 700 ml of a PMT (iodine value 55 g, I _2/100 g, the dienes content of 7%) and fraction 05 with EP-300 in a ratio equal to 3: 1. When the temperature of the mixture reaches 20 ^o C, the TXT-TIBA catalytic complex is introduced into the reactor, the reaction is carried out for 3 hours at a temperature of 40 ^o C, after which 10.4 ml of isopropyl alcohol are added and the unreacted hydrocarbons are distilled off. Characteristics of the resulting product are shown in the table.

Example 12 In a 1 l reactor is fed a mixture of 700 ml of a PMT (iodine value: 56 g, I _2/100 g, the dienes content of 7%) and C ₅ fractions (obtained by pyrolysis of kerosene-gas oil fraction in the high mode) in a ratio equal to 3: 1. When the temperature of the mixture reaches 20 ^o C, the TXT-TIBA catalytic complex is introduced into the reactor, the reaction is carried out for 3 hours at a temperature of 40 ^o C, after which 10.4 ml of isopropyl alcohol are added and the unreacted hydrocarbons are distilled off. Characteristics of the resulting product are shown in the table.

Example 13 (prototype). 700 ml of a mixture of heavy pyrolysis resin and C ₅ fraction in a ratio of 2.5: 1 are fed into a 1 L reactor. Upon reaching a temperature of the mixture of 20 ^o C with stirring for 3 min, 21 ml of the catalytic complex of aluminum trichloride with benzene containing 40 wt. AlCl ₃ . The polymerization is carried out for 4 hours at a temperature of 20 ^o C. The reaction is stopped by adding 200 ml of water. The aqueous layer was separated and the resulting mixture was washed twice with 400 ml of water, after which unreacted hydrocarbons were distilled off. Characteristics of the resulting product are shown in the table.

From the data in the table it follows that the yield of binder according to the proposed method is 1.78 times higher compared to the prototype at the lower limit and 2.13 times higher at the upper. There is a coincidence in the softening temperature, however, the strength characteristics of plastic concrete based on a binder according to the proposed method is higher in comparison with the prototype. In addition, plastic based on a binder according to the proposed method have reduced heat resistance, so the heat resistance coefficients R $\genfrac{}{}{0ex}{}{\text{-ten}}{\text{fifty}}$ , R $\genfrac{}{}{0ex}{}{\text{25}}{\text{fifty}}$ , R $\genfrac{}{}{0ex}{}{\text{-ten}}{\text{25}}$ at 3.95; 1.59 and 2.42 times less compared to the prototype.

 Thus, the proposed method provides a high yield of binder material, which allows to obtain plastic concrete with high mechanical characteristics.

Claims (1)

A method of producing an astringent for road construction by copolymerization of liquid hydrocarbon pyrolysis products in the presence of a catalyst, characterized in that a heavy pyrolysis resin with a boiling point above 200 ^° C and a C ₅ fraction in a mass ratio of 2 1 to 3 1, respectively, are used as liquid pyrolysis products and as a catalyst, a complex of titanium tetrachloride with triisobutylaluminum in a molar ratio of from 3 1 to 6 1, respectively, introduced in an amount of 0.35 0 55 wt. from the reaction medium.

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