SU1384598A1 - Method of producing bitumen - Google Patents

Abstract

The invention relates to petrochemistry, in particular to the preparation of bitumen (BM). The goal is to improve the quality of the EM and reduce the consumption of catalyst (CT). The preparation of BMs is carried out by oxidation of oil tar with oxygen to zhudu in the presence of QD. The latter has a composition of wt.%: Manganese dioxide 3,32-13,0; ferrous sulphate and manganese sulphate 0.01-1.0; oligoquinones else, taken in an amount of 0.0001-0.1 wt.%. As QD, it is preferable to use the waste production of hydroquinone from aniline from the stage of distillation and reduction of quinone, reducing the content of polyvalent metal compounds from 1-10 to 0.000013- 0.000032 wt.% In BM leads to increased resistance of BM to oxidative aging. 1 hp f-ly, 1 tab. with co (L

Description

00 CX)

four

ate CO 00

The invention relates to the production of oxidized petroleum bitumen and can be used in the petrochemical and refining industries.

The purpose of the invention is to improve the quality of bitumen and reduce catalyst consumption.

PRI m 1 p. In a glass reactor with a capacity of 2 liters, equipped with an external electric heater, at 100-150 ° C, 1 kg of oil tar is charged, and 0.00005% by mass of catalyst 1 — waste from the production of hydroquinone from aniline is introduced.

The catalyst is a slurry in the form of a powdered product of the recovery stage of the quanine and has the following composition, wt%: manganese dioxide 3.32, ferrous and manganese sulfates 1, oligoquinones the rest. distillation stages and rest

The formation of quinone is obtained in the production of hydroquinone from aniline in an amount up to 40% by weight.

The slurry from these stages has the same qualitative composition.

The temperature is brought to 250 ° C and the air supply through the bubbler is switched on at a flow rate of I l / min and oxidation is carried out for a predetermined time. Tar is used for oxidation; having the following indicators:

Density, g / cm 0.98

Viscosity relative

at 80 ° C, cSt20

The temperature of the flask, C, in an open crucible 191

Temperature zastaoo nor

ten

The results obtained in this experiment are shown in the table, where the results of the experiments in examples 2-10 are also given.

Catalyst

The amount of catalyst, wt.%

0.50, G 0.001 0.1 0.2 0.001 0.0001

Time of experience, h

5 3

Example

12

Needle penetration depth

at 25 ° С 100 g, 5s, mm

Softening temperature

ring and ball with

Extensibility at 25 C, cm Adhesion to marble

Brand of bitumen in accordance with GOST

22245-76margan

0.15. 0.32 0.323 0.646

0.3

0.4

235 8 522.5

3456 78 9

ten

170 21 15 105 97 12855

39 70 85 92100 39 4353

66 8 - 3.5O - 6051

Hor. Hor. Hor. Hor.Hor.Ud

4- BI-5

- BNYA BND 90/130 60/90

0.15

-four

0.4542

In examples 2-7, the same catalyst 1 is used, in examples 8-9 catalyst 2 is used, and in example 10 -. 3

Catalyst 2 - this sludge from the quinone stripping column - containing, wt%: manganese dioxide 5,17; iron and manganese sulfates 0.05, the oligoquinones rest, and the catalyst 3 sludge from the quinone distillation stage, containing, in wt%: manganese dioxide .12.84, iron and manganese sulfates 0.01, oligoquinones the rest.

Example 11. As a catalyst using a model system containing, in wt.%:

Manganese dioxide13

Manganese (II) sulfate 0.5 Iron (II) sulfate 0.5 QuinhydronEmost

represent quinhydrone molecular complex p-benzoquinone and hydroquinone, is an oligomer from alternating molecules of the oxidized and reduced form.

Using a catalyst of this composition under the conditions of Example 5, bitumen is obtained having. The following indicators:

Depth of needle penetration at 25 ° С (100 g, 5 s), mm

The softening temperature around the ring and the ball

Extensibility at 25 C, cm4

Adhesion to marble Good Example 12. The test was carried out analogously to example 4, but oxidation was carried out in the presence of pure manganese dioxide in an amount equal to the content of this substance in the catalyst introduced into the reaction mixture in example 4 (0.000032% by weight of the raw material) Bitumen having the following characteristics is obtained:

Needle penetration depth

at (100 g, 5 s), mm 10

The softening temperature is about.

80

on the ring and the ball, C Adhesion with marble GOST 22245-76

40

Good Does not match

Comparison of the properties of bitumen obtained in examples 4 and 12 implies

that pure manganese dioxide has a significantly lower catalytic efficiency compared with the waste, in which it is included in the amount of 3.23 wt.%. The same results are obtained when using other catalyst samples.

Example 13 The experiment was carried out similarly to Example 6, but oxidation was carried out without the introduction of a catalyst. Bitumen is obtained having the following characteristics:

Needle penetration depth at 25 ° С (100 g, 5s),

mm 0 260

The softening temperature of the ring and the ball, C 31 Extensibility cm, with

 25 ° С43

Adhesion to marble Good GOST 22245-76Not match

Carrying out the process of oxidizing crude oil to produce bitumen that meets the requirements of GOST 22245-76 requires a much longer time (up to 12 hours) without a catalyst. When a catalyst is added less than 0.000 wt.%, The desired quality of bitumen is not observed at the optimum time of 2-3 hours, and an increase in the amount of catalyst of more than 0.1 wt.% Results in products with high viscosity during the same time.

Thus, the proposed method makes it possible to drastically reduce the number of polyvalent metal compounds introduced into bitumen to reduce the time of its production. As examples 3,9,10 use of the catalyst in an amount of 0.001-0.001% wt. , 5–3 h, the main brands of road bitumens of NDB grades with the content of polyvalent metal compounds in the finished bitumen are 0.000013-0.000032 wt.%. A decrease in the content of compounds of polyvalent metals (from 1–10 wt.% To 0.000013–0.000032 wt.%) In bitumen leads to a higher resistance of bitumen to oxidative aging.

55

Claims (2)

1. A method for producing bitumen by oxidizing petroleum tar acid 5 13845986 the genus of air in the presence of manganese dioxide was 3.32–13.0 yoytora, soda, stainless steel manganese – iron sulphate and tsa, about tl and h and with that, manganese sulphate 0.01–1.0 which, in order to increase the quality of bit Oligoquinones, the remainder and reduction of catalyst consumption, taken in an amount of 0.0001-0.1 wt.%, use a catalyst, additional 2. The method of claim 1, which contains iron sulphates and mar-shi, and with the fact that, as a catanthus and OLIGOCHINONS, 10 is used for the use of a solubilizer in the production of components containing hydrochlorinone from aniline from stage May %: distillation and reduction of quinone.