SU1502598A1 - Method of producing binder - Google Patents

Abstract

BACKGROUND OF THE INVENTION The invention relates to bituminous substances, in particular, to the production of residents for road construction, and can be used in the oil and coal processing industry. The goal is to increase the productivity of the process and expand the raw material base. The process is carried out by mixing a heavy resin of high-speed pyrolysis of brown coal with a boiling point above 350 ° C with a solvent - dephenolated fraction of 180-300 ° C of the high-speed pyrolysis resin of brown coal, heat treating the mixture with a continuous flow at a volumetric rate of 3-6 h ^-1 (mass ratio resin and solvent - 1: (4-5)), temperature 280-320 ° C and pressure 2.5-3.5 MPa, evaporating by vacuum distillation of the regenerated solvent and the target product with recirculation of the regenerated solvent for mixing with the pyrolysis resin. The method makes it possible to increase the productivity of the process by 3 times and reduce the relative losses of the raw material by 1.5 times. 1 dw., 12 tab.

Description

The present invention relates to a method for producing a tandem solid fuel from the pyrolysis products and can be used in the coal, coking and slate chemical industries.

The aim of the invention is to increase the productivity of the process and expand the raw material base.

The drawing is a flow chart explaining the essence of the method.

Ground high speed pyrolysis resin (VSP) sized

particles less than 0.2 mm in department 1 of the preparation of the raw material are mixed with a solvent - a fraction of 180 - 300 C high-speed pyrolysis (VSP KLU). in a mass ratio of 1-4: 5 at 80 ° C and continuous stirring, and the resulting feed mixture is then pumped at high pressure 2 with a volume velocity of 3-6 to the apparatus (reactor) -3 of continuous operation, equipped with a mechanical stirrer to eliminate stagnant zones in the reaction volume, where at 280 BZO C and a pressure of 2.5-3.5 MPa

d. thermal dissolution of .noii resin. The reaction products formed in apparatus 3 are cooled in a refrigerator 4 to 100 ° C and then passed through choke 5, where the pelvic part is separated from the liquid. Liquid reaction products are then sent to a vacuum distillation column 6, where, at a residual pressure of 45 torr, they are distilled to release a recoverable solvent (then sent again to the raw material preparation compartment 1), gasoline fraction (m.p. less than 180) and a traveling one .

Example 1. 16.7 mas. crushed VSP heavy resin with particle sizes less than 0.2 mm (Table 1) is shifted from 83.3 May, h. aromatic solvent - dephenolated middle fraction of VSP resin with m.p. 180-300 ° C (Table 2) with continuous stirring at 80-100 ° C. Then, the resulting raw mixture is subjected to heat treatment with a continuous laboratory apparatus with a reactor volume of 1 dm, equipped with a mechanical stirrer, at 300 ° C, and a pressure of 4.0 MPa and volumetric feed rate 4. The reaction products obtained at the outlet of the reactor are cooled to 100 ° C, the gas phase is separated from the liquid one, and the liquid reaction products are distilled at a residual pressure of 45 Torr, separating the gasoline fraction with m.p. 180 ° С, recoverable solvent (tc, kip. 180-300 С) and a road bushing (m kip. 300 s). This gives 73.7 mash, an aromatic solvent and 24.1 masoh. road bitumen.

Examples 2-16 ° According to the procedure described in example 1, mixtures of a heavy VSP resin with a dephenolized middle fraction of a VSP resin with a different ratio of components are prepared and subjected to heat treatment under various conditions.

The conditions of the experiments are given in table. 3

In example 12, as an aromatic solvent, a non-dephenololized fraction of a secondary VSP resin with a bale of 180-300 ° C is used.

The results of the experiments are presented in table. four; properties in the ghost - in tab. five.

5984

i iipii not valuable in the table. 4 cif; yev data, 4: 1.1 maltenes when thermally dissolving heavy resin iUJii L NIGIGE of the largest values at 2, Y-320 C, pressure 2.5-3.5 MPa, volume feed rates of the raw mixture 3-6 and solvent by weight ratio: 4 to 1 g resin;

In these conditions, the ratios of maltenes / asphaltenes in the products of thermal dissolution exceed 2, which leads to a significant improvement in the plastic properties of the resulting products (Table 5).

Example 17: According to the procedure described in the gtrimer 1, a mixture of 16.7 mash is prepared. heavy (m. bale, 350 C) VSP resin (its characteristic is about 7 ede0 per B, table 6) with 83.3 wt.h. Vepfenoline fraction of VSP resin with an interval of To kip. 180-300 ° C. The characteristics of this fraction are given in table. 7 and 8

5 The mixture is subjected to heat treatment in example 1. Receive 72.8 ma.h. aromatic solvent (fraction 180-300 С), 25.1 May, h. road bitumen (fraction Qi with m. bale 300 C) and /; 1 May. h petrol fraction (fraction with m. Kip. - 1 BUT s).

The characteristics of the received-on-road-to-live are given in ta) l. 9.

When used as a solvent for the endefaction of the light fraction of a VSP resin, boiling up to, or dephenolized, the total light and medium VSP resin boiling up to

Q 300 ° С, the quality of the received road recipient does not meet the requirements of GOST 22245-76 (Table 10).

Physico-chemical characteristics of non-dephenolized and non-dephenolated VSP resin fraction with an interval t „bale. 80 300 ° C are given in table. 11, they differ only in the content of phenols, which have a negative effect on the production of a gum.

0

Thus, from the table. 11 data shows that the quality of those received in the living complies with the requirement of GOST 22245-76 for road bitumens of the type ID 40-60.

In tab. 12 shows the comparative data of the known and proposed methods.

five

five

Thus, the proposed method makes it possible to increase the productivity of the process by more than 3 times, to reduce the relative loss of raw materials in the form of volatile components by 1.5 times, making it possible to carry out the process at lower temperatures and pressures than the known one.

Claims (1)

Invention Formula The method of producing a binder by mixing solid carbonaceous material with a solvent — an aromatic fraction, followed by heat treatment of the mixture at 280–320 ° C, a pressure of 2.5–3.5 MPa, and isolation of the desired product in vacuo. smart distillation, characterized in that, in order to improve the process performance and expand the raw material base, a solid high-speed pyrolysis resin of brown coal with a boiling point above 350 ° C is used as a solid carbon-containing material, and a decafenolized fraction 180-300 ° resin is used as a solvent high-speed pyrolysis of brown coal, heat treatment is carried out in continuous mode with a volumetric feed rate of 3–6, with a resin: solvent mass ratio of 1: 4-5, and obtained with vacuum second solvent distillation is recycled for mixing with the original resin .Table 1 , Component composition, Temp- Elemental composition, m p.1as 15 ratura-yyy size d- NNF S, Mal-Ac-Unexceni (by size-falgpipo Kish, bones) shadowed bit 6980.26 6.01 1.14 12.5910.21 72.27 17.52 Table 2, C To 180 I 180-220 220-250 250-270 270-300 d, us. 3.82A321525.2 I Table 3 At- Volume- Tempe-Davle-Mass ratu-kie attitude speed, ° SMP solubility, tel: 4 4 4 4 4 3 2 6 4 4 4 4 4 4 10 4 3.0 2.5 3.5 5.0 1.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 l) but S h y fl) n 0.862.7 69.05 5.09 1.4A 0.5 23.91 Resin characteristics Density, g / cm Initial boiling point, ° С Elemental composition, wt.%: WITH H S 0 + N (by differences Content, wt.%: ash water toluene insoluble substances phenols Table 6 9.9 71.0 19.1 Table 7 Fraction of VSP 180-300 С resin Obesfenolenna 0.9714 0.9651 162 166 84.39 9.54 0.96 5.11 Missing 0, A2 0.23 absent 0.78 missing Fractions, С Up to 180 180-220 220-250 250-270 270-300 Yield, wt.% 5.65 32.90 30.40 10.60 20.45 Table 9 41 52 -14.5 66.5 66.3 26.4 7.3 Needle penetration depth (d 0.1 mm) at 25 ° C, mm Kish softening temperature, s Table 10 eleven 28 42 63 59 52.5 Condition about