RU2275408C1 - Process of producing bitumen binder from acid sludge - Google Patents

Abstract

FIELD: petroleum processing and disposal of waste.

SUBSTANCE: neutralized acid sludge is subjected to thermal oxidation with air oxygen in presence of additionally introduced modifying additive, in particular regenerate from coagulum obtained by autoclaving in amount 5-10% based on the weight of raw material.

EFFECT: achieved utilization of polymeric production waste.

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Description

The invention relates to the production of building materials by processing waste oil refineries formed during the purification of distillate oils with concentrated sulfuric acid or oleum. Currently, this product, the so-called acid tar (KG), of varying degrees of acidity, is discharged into storage ponds, where over time acid is washed out by atmospheric precipitation, as well as the release of SO ₂ and SO ₃ , as a result of which water and air are polluted pools. Disposal of CG solves an important task of creating waste-free production and environmental protection.

A known method of producing bitumen by mixing acidic refinery wastes with heated high boiling oil products, to obtain a reaction mass and gas-bitumen foam, with its subsequent destruction. But this method did not find application because of the complex and expensive hardware design (A.S. USSR No. 973589, class C 10 S 3/04, aut. A.D. Rudkovsky et al., 1982).

The closest in technical essence to the present invention is a method for producing a bitumen binder by treating pond acid tar with a neutralizing agent, followed by oxidation of the neutralization products and mixing them with asphalt deasphalting oil tar with propane. This method is characterized by the ability to obtain a bitumen binder that meets the requirements of GOST for road bitumen, but this method does not seem to be able to process acid tar, since deasphalting asphalts are a commodity product and have a high cost and are currently exhausted (A.S. USSR No. 910723, class С 10 С 3/04, bulletin No. 9, author A.F. Frolov, A.N. Aminov, N.M. Mayorova).

The objective of the invention is the production of bituminous binders based on KG using synthetic rubber (kaogulum) as a modifying additive.

The problem is solved by thermal oxidation of acid tar using a modifying additive - a regenerate from the waste of synthetic rubber plants (kaogulum).

Kaogulum is a polymer waste from the production of styrene-butadiene latexes formed in the process of coagulation of latex-containing wastewater and equipment cleaning.

The methodology of the process of obtaining a paste-like regenerate from kaogulum by the autoclave method.

1. A mixture of kaogulum with a swelling agent in ratios of 1: 1 or 1: 0.75. Characterization of swelling agents is presented in table 1, 2.

2. Introduction to the mixture of regeneration activator. Swelling of the mixture in swelling agents at 110 ° C. for 3 hours in a thermostat.

3. Coagulum regeneration during heating of the autoclave in an oil jacket for 6 hours, the regeneration temperature is 185 ° C.

The resulting regenerate was evaluated by chloroform extract, by the number of volatile components, and ash content was also determined.

Table 1.
The characteristic of waste oil is a swelling agent. Indicator Waste oil (OAO Avtodiesel) GOST 21046-86 Conventional viscosity at 20 ° С 58 > 40 Kinematic at 50 ° C 47 > 65 Flash point in an open crucible, ° С, not lower 134 120 The content of fractions boiling up to 340 ° C 10 10 The pour point of the fractions -10 -10 Mass fraction of mechanical impurities,%, no more 1,1 1,0 Mass fraction of water,%, no more 0.4 2.0

Table 2.
Characterization of petroleum oils - swelling agent. Name of indicator The content of the component, wt.% petroleum slams pasty liquid Water content 5.60-13.00 16.10-42.00 Organic compounds (during extraction) 28.60-38.40 22.10-40.00 Mineral residue 48.60-71.80 28.00-40.00 The composition of the mineral the remainder 7.60-14.40 8.00-16.10 Fe ₂ About ₃ 18.20-42.40 20.00-42.00 CaO 0.02-0.05 0-0.035 CuO 0.13-0.18 0-0.16 Zno not found not found Cr total the rest is up to 100% the rest is up to 100% Sand (SiO ₂ )

Table 3 shows the data of the chloroform extract of the regenerate obtained with these swelling agents. (Regeneration temperature - 185 ° С, time - 6 hours).

Table 3.
Chloroform extract (%) of a paste-like regenerate obtained by an autoclave (a / c) method using these swelling agents. No. Softener name Koagulum (SK plant) (a / c) one Used oil 1: 1 25 2 Neftemaslošllam 1: 1 21 3 Waste Oil 1: 0.75 31 four Neftemasloşllam 1: 0.75 27

EXAMPLE 1. As a feedstock, KG with an acid number of 30-70 mg KOH / g of tar is used, as a neutralizing agent we use air hydrated lime (calcium hydroxide), corresponding to GOST 9179-77, a modifying additive - 5% regenerate, (1: 0.75), a regenerate is a coagulum in oil processing, introduced at the beginning of the oxidation process. Oxidation of acid tar in bitumen is carried out with atmospheric oxygen for 1.5 hours, with constant stirring and a process temperature of 95 ° C.

EXAMPLE 2. As a feedstock, KG with an acid number of 30-70 mg KOH / g of tar is used, we use air hydrated lime (calcium hydroxide), corresponding to GOST 9179-77, a modifying additive - 5% regenerate, as a neutralizing agent, (1: 1), a regenerate is a coagulum in oil and slag introduced at the beginning of the oxidation process. Oxidation of acid tar in bitumen is carried out with atmospheric oxygen for 1.5 hours, with constant stirring and a process temperature of 95 ° C.

EXAMPLE 3. As a feedstock, KG with an acid number of 30-70 mg KOH / g of tar is used, as a neutralizing agent we use hydrated slaked lime (calcium hydroxide) corresponding to GOST 9179-77, a modifying additive - 5% regenerate (1: 0 , 75), the regenerate is the coagulum in the oil and oil sludge introduced at the beginning of the oxidation process. Oxidation of acid tar in bitumen is carried out with atmospheric oxygen for 1.5 hours, with constant stirring and a process temperature of 95 ° C.

EXAMPLE 4. As a feedstock, KG with an acid number of 30-70 mg KOH / g of tar is used, as a neutralizing agent we use hydrated slaked lime (calcium hydroxide), corresponding to GOST 9179-77, a modifying additive - 10% regenerate (1: 0 , 75), the regenerate is the coagulum in the oil and oil sludge introduced at the beginning of the oxidation process. Oxidation of acid tar in bitumen is carried out with atmospheric oxygen for 1.5 hours, with constant stirring and a process temperature of 95 ° C.

The results of the experiments are presented in table 4.

Table 4.
The results of the experiment to obtain roofing bitumen with different content of modifiers. Name of indicator Regenerate - coagulum in oil processing Regenerate - coagulum in oil and grease Roofing bitumen BNK-45/190 KG + 5% regenerate (1: 0.75) KG + 5% regenerate (1: 1) KG + 5% regenerate (1: 0.75) KG + 10% regenerate (1: 0.75) 1. The depth of penetration of the needle, mm 170 160 172 183 160-220 2. The softening temperature of the ring and ball, ° C 41 44 44 49 40-50 3. Mass. the proportion of water soluble compounds. 0.31 0.36 0.32 0.33 0.30 4. Mass fraction of water,% 0.35 0.29 0.26 0.22 Traces 5. Flash point ° C, not lower 242 245 244 247 240

Thus, the use of coagulum regenerate as a modifying additive makes it possible to obtain a bitumen binder, which in its parameters corresponds to roofing bitumen. (Roofing bitumen BNK-45/190).

Claims (1)

A method of producing a bituminous binder from acid tar by thermal oxidation of neutralized acid tar by atmospheric oxygen, characterized in that a modifying additive is additionally introduced - a coagulum regenerate obtained by the autoclave method in an amount of 5-10% per 100% of oxidizable raw material.