SU1281584A1 - Method of producing shale bitumen - Google Patents

Abstract

The invention relates to methods for producing shale bitumen for road construction and can be used in the shale and coal processing industry. In order to simplify the process technology by reducing the erosion of the equipment by reducing the ash content of the original paste, heat treatment of the shale is carried out in the presence of brown coal, solvent and distillate fraction with mp. 200-340s from gasification or semi-coking of slate. The ratio of the organic mass of shale and the organic mass of coal is 1: (O, 7-1, O). The desired product is separated by distillation. The process is carried out at a temperature of 400-420 ° C, a pressure of 5-9 Mlla. The ash content of the original paste is reduced to 8.0 wt.%, The yield of the target product increases to 159.0 wt.%. 1 hp f-ly, 2 tab. i (L s

Description

tc

00

ate

00 4

bitumen for road construction and can be used in the shale and coal processing industries.

The aim of the invention is to simplify the process technology by reducing the erosion of the apparatus by reducing the ash content of the original paste,

Example I. The initial paste is prepared by mixing shale (Herogen 70) 260 g, brown coal 70 g (OMC: OMD 1: 0.9), regenerated solvent with Tcip. 200-320 ° C 350 g of fresh distillate shale solvent with a bp. 200-340 ° С 210 g (the ratio between the mixture of slate + coal and solvents is 1: 1.3).

. Kerogen-70 has the following pattern: .., wt.%: A 22.67; CO.J M ,, 5.47: C / ° 80.40; ,four; 5 2.00; N 0.25; W 1.13.

Brown coal has the following characteristics, wt.%: W 1,8; A 3.55; CJ 571.62; ,12; S 0.20; N 0.66.

Fresh distillate solvent with a bp. 200-340 ° C has a density of P 992 kg / m, elemental composition, wt.%; C 82.80; H 9.40; S 0.64; N 0.55; fractional composition; 10% boils at 255 ° С, 30% - at 282 ° С,, 50% - at, 70% - at, the phenol content is 31.0%,

Thermal dissolution of the paste is carried out under a pressure of 8 Sha, temperature. 415 C for 10 min. The resulting liquid products are distilled — initially, at atmospheric pressure, water is distilled off and benzoic acid is distilled.

tum 533.6,

Example 2. Raw materials and conditions for the process of thermal dissolution

5 are analogous to Example 1. The ratio of OMC: WMD is 1: 1.2,

Example 3. A paste is prepared by mixing shale 326 g, lignite 109 g (OMSGOM ratio 1: 0.8),

10 regenerated solvent with

bp 200-320 C 229 g and a fresh distillate solvent with a boiling point of 200-340 ° C 331 g (the ratio of a mixture of slate + coal: solvents

5: 1,3),

Slate has the following characteristics, wt.%: A 47.83} C °°; 80, 12; H 9.435 S / 0.91;

", S1c (1 l of g-., And lt

.about

, 25; 3

.five

The characteristic of fresh solvent with a boiling point of 200-340 ° C and brown coal is given in Example 1.

Thermal dissolution of the paste is carried out under a pressure of 5 MPa for 30 minutes. The processing of the liquid products of the process is carried out analogously to example 1,

Example 4. The process of thermal dissolution of shale and brown coal is carried out at a process time of 60 minutes and a pressure of 6 MPa.

Example 5 A paste is prepared by mixing a sample of shale sulphate 308 g, lignite 103 g 35 (OMC: OMD ratio 1: 0.7) p 325 g of regenerated solvent, sulphate semi-coking resin 270 g (slate + coal: solvents mixture 1: 1.45).

3G

40

Slate has the following characteristics, wt.%: W 5,87; A 44.25,

i r- 47- 73 S9 “I am 7/1. p Oh, / H,

S 5,10; 1.41.

The semi-coking resin has a 1-fraction fraction with a bp. to 00 C, and

then stripped liquid products

distilled under vacuum

with a residual pressure of 50 mm Hg. nost 1033 kg / m, elemental composition,

wt.%: C 79.785 N 8.68; S N 1.46, fractional composition: 10% boils away at,. 30% -, 50% - 310 ° С, 90% - 338 ° С.

The distillate is selected with a boiling point. 200-320 ° C in terms of atmospheric pressure, which is used as

regenerated solvent. The residue with boiling point of higher than 20 sec, containing in its composition the insoluble organic matter of shale and coal and their mineral part, is the desired product.

The process is conducted at a pressure of 9 MPa, a temperature of 395 ° C for 40 minutes.

Example 6. The method is carried out at a ratio of OMC: WMD equal to 1; 1,

The yield of marketable products per 430 g of a mixture of kerogen-70 and coal is, g: gasoline formula.

tum 533.6,

Example 2. Raw materials and conditions for the process of thermal dissolution

analogous to example 1. The ratio of OMC: OMU is 1: 1.2,

Example 3. A paste is prepared by mixing shale 326 g, lignite 109 g (OMSGOM ratio 1: 0.8),

reclaimed solvent

bp 200-320 C 229 g and a fresh distillate solvent with a boiling point of 200-340 ° C 331 g (the ratio of a mixture of slate + coal: solvents

: 1,3),

Slate has the following characteristics, wt.%: A 47.83} C °°; 80, 12; H 9.435 S / 0.91;

", S1c (1 l of g-., And lt

, 25; 3

The characteristic of fresh solvent with a boiling point of 200-340 ° C and brown coal is given in Example 1.

Thermal dissolution of the paste is carried out under a pressure of 5 MPa for 30 minutes. The processing of the liquid products of the process is carried out analogously to example 1,

Example 4. The process of thermal dissolution of shale and brown coal is carried out at a process time of 60 minutes and a pressure of 6 MPa.

Example 5 A paste is prepared by mixing a sample of shale sulphate 308 g, lignite 103 g (OMC: OMD 1: 0.7) p regenerated solvent 325 g, sulphate semi-coking resin 270 g (mixture slate + coal: solvent ratio 1 : 1.45).

Slate has the following characteristics, wt.%: W 5,87; A 44.25,

i r- 47- 73 S9 “I am 7/1. p Oh, / H,

S 5,10; 1.41.

Semi-coking resin has a density of 1033 kg / m, elemental composition,

The process is conducted at a pressure of 9 MPa, a temperature of 395 ° C for 40 minutes.

Example 6. The method is carried out at a ratio of OMC: WMD equal to 1; 1,

Example 7. The process with a sample of sulfur oil shale and brown coal is carried out at a ratio of OMC g OMD 1: 0.6 and a process time of 35 mic.

.

The results of thermal dissolution of combustible shales mixed with brown coal in an autoclave and shale mixed with fuses in an autoclave are shown in Table 1.

The data in Table 1 shows that the optimum ratio is between the organic mass of shale and the organic mass of brown coal, equal to 1: (O, 7-1.0). With a decrease in the amount of the brown coal organic mass (less than 0, 7) with respect to the organic mass of the shale, the liquefaction of the initial mixture does not deteriorate, but the ash content of the initial mixture of solid fuels remains high.

The use of a mixture in which the ratio between OMC and OMU is greater than 1: 1.0 leads to a decrease in the solubility of the organic mass of solid matter and the appearance in the liquid products of the coke-like process. The latter make it difficult to carry out the process of thermal dissolution,

To carry out the process of thermal dissolution of a mixture of shale and coal in a shorter time than 10 minutes, it is technically difficult to increase the time of dissolution (60 minutes) technically and economically impractical.

The properties of the samples of bitumen obtained under the conditions of examples 1, 3 and 5, are presented in Table 2. From Table 2, it can be seen that bitumens based on the products of thermal dissolution are mixed.

This kerogen-70 and lignite (example), shale and lignite (example 3) and a sample of slate and lignite (example 5) satisfy the requirements of GOST for oil bitumen used as road construction,

 О Thus, the proposed method allows to simplify the process technology, as well as to increase the yield of the target product.

15 f

about rmu l and

the invention

Claims (1)

1, A method for producing shale bitumen by heat treatment of shale at elevated temperature and pressure in the presence of a solvent: and a distillate fraction with m, kip, 200-340 ° C of gasification or semi-coking processes of shale, followed by distillation of the desired product by that, with the aim of simplifying the process technology, heat treatment of shale is carried out in the presence of brown coal with a ratio of organic mass of shale to organic mass of coal equal to 1: (0.7-1.0), 2, the method according to claim 1, about t l and h and -. This process is carried out at a temperature of 400-420 ° C, a pressure of 5-9 MPa, t - with l to and 1 Ash content (L + CO), slate n brown coal mixtures tUJCVW becoming pasta, Mac.Zl xrogei-70, in g, h OMC of wedges, incl. OMS 18.5 8.0 60.5 42.8 14.7 6.4 15.5 31.9 In {Sorich) 1lL o6pa jetl ci. pimcToro. schist, and so on OMS 47.2 20.5 39.7 16.2 17.6 8.0 57.4 41.0 43.4 17.7 "0.61 26.3 74.9 29.5 100.0 39.39 74.9 33.4 78.5 35.1 Characteristic one 1281584 Indicators for example 5 Continuation of that T T I T J 2 ILi (mz Pure coal, incl. WMD 39.5 38.1 fresh distal solvent pro Gasification process 48, 8 reclaimed distillate solvent 81.2 fraction of semi-coke-sulfur slate ratio OMC: OMU, 9 sieve shale + coal: solvent, 3 Process conditions 54.5 52.6 56.0 74.0 25.125.1 24.224.2 76.1 79.1 53.9 50.8 23.1 24.2 79.3 65.7 1: 0.8 1: 0.8 1: 0.7 1: 1.3 1:, 3 1: 1.45 Needle penetration depth at 25 ° C (100 g, 5 s), mch Needle penetration depth at (200 g, 60 s),  mm Continued table. I i (on the third) .. 42.6 41.0 50.0 21.5 20.3 . 48.8 79.3 65.7 1: 0.7 1: 1.45 80.0 81,581.2 63,515.0 (fuses) 1: 1 1: 0.6 1: 1.3 1: 1,, E 138 232 94 68 128 37 Temperature is ramping, ° С Change of softening temperature after warming up, s Clutch Testing Extendability, cm at 25 ° C at 42 37 50 1.7 2.00.8 Endures 68 8762 10.8 24.55.1