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INVENTION
Patent of the Russian Federation RU2287550
METHOD OF OBTAINING BITUM
The name of the inventor: Zorin Arkady Danilovich (RU); Zanozina Valentina Fedorovna (RU); Karataev Evgeniy Nikolaevich (RU); Sidorov Yuri Vladimirovich (RU); Kolmakov Georgiy Alexandrovich (RU)
The name of the patent holder: Limited Liability Company "EcoBit" (RU)
Address for correspondence: 603950, Nizhny Novgorod, Gagarin Avenue, 23, building 5, Research Institute of Chemistry, V.F. Zanozina
Date of commencement of the patent: 2005.10.03
The present invention relates to the processing of wastes from the oil refining and petrochemical industry, in particular acid tar, and can be used to produce bitumen used in road construction, in the production of roofing and insulation and other materials. Essence: acidic tar, preferably with a sulfuric acid content not exceeding 7% of tar mass, is heated in a flow reactor at cracking temperatures below the coking temperature. The non-volatile hydrocarbon fraction is withdrawn from the reactor. From the vapor hydrocarbon fraction, components with a boiling point above 200 ° C are isolated and mixed with a non-volatile hydrocarbon fraction.
DESCRIPTION OF THE INVENTION
The present invention relates to the processing of wastes from the oil refining and petrochemical industries, in particular acid tar, and can be used to produce bitumen used in road construction, in the production of roofing and insulating materials, and the like.
Acid tar is one of the main types of solid-phase wastes of industrial enterprises that are formed during the purification of petroleum products with sulfuric acid and, as a rule, are dumped in storage ponds. The invention relates to a method for processing acid tar from storage ponds, so-called pond acidic tar.
There are known methods of processing acid tar in bitumen. Common to all known methods of processing acid tar in bitumen is pre-treatment of acid tar (dehydration, washing away from sulfuric acid or neutralization with calcium compounds) and heating in the presence of additives added to acidic tar.
In accordance with the method known from AC 1176589 C1, 23.10.1984 , acidic tar containing sulfuric acid is used to produce the bitumen, into which a heated hydrocarbon fraction is introduced, which is used as the tar from direct race, asphalt deasphalting, etc. This method of processing acidic Tar to obtain bitumen is accompanied by the formation of foam, which has a negative impact on the quality of bitumen. To eliminate the influence of the foam, it is extinguished.
The disadvantage of this method of obtaining bitumen is associated with the need to use additional raw materials (hydrocarbon fractions) and a foam extinguishing operation, which requires material and time costs and leads to a complication of the method.
There are known methods for producing bitumen from acid tar, including pretreatment - neutralization of calcium carbonate, hydroxide or calcium oxide contained in tars of sulfuric acid, then hydroxides are oxidized by air oxygen.
According to the method known to RU 2215772 C1, 10.11.2003 , in order to reduce the time required for carrying out the oxidation operation, it is carried out in the presence of an iron-containing catalyst at a temperature of not more than 150 ° C, while the powder used in the purification of water and Isolated in the air purification devices of melting plants.
The main disadvantage of the method is the duration of the process of processing acid tar in bitumen, which is several hours, and a considerable time is spent on carrying out the oxidation operation. Another disadvantage of this method is the use of a catalyst, which is a waste of metallurgical production and production of which is carried out in other production areas than the production of bitumen. The production of this catalyst and its transportation increase the cost of producing bitumen. In addition, when acid tars are neutralized, calcium sulphate is formed, which loosens tars, reducing their viscosity. A consequence of this is the low water resistance of the resulting bitumen. As a result of decreasing water resistance, gradual washing out of calcium sulphate from bitumen under the influence of atmospheric precipitation occurs, which negatively affects the quality of those infrastructure facilities for the construction of which bitumen is used.
As a prototype, a method for obtaining bitumen from acid tars with relatively low time spent on heating tar is chosen. The method involves washing acid sludges from sulfuric acid, dehydrating, heating and oxidizing it with air oxygen. A feature of the method is that the heating is carried out by an electrochemical method (RU 2227802 C1, 27.04.2004) .
The main disadvantages of this method, as well as the above, are connected with the use of the oxidation operation, which requires a long time (~ several hours), and the production of tar of low quality.
The present invention is directed to the development of a simple method for producing high quality bitumen with the least time and material costs.
The method for producing bitumen from acid sludge including dehydration of acid sludges and heating in accordance with the invention is characterized in that heating is carried out in a flow reactor at cracking temperatures below the coking temperature to produce non-volatile and steam hydrocarbon fractions, from the steam hydrocarbon fraction, components with boiling point Above 200 ° C and mix them with the non-volatile hydrocarbon fraction withdrawn from the reactor.
It is advisable to use acid tars with sulfuric acid content not exceeding 7% of the tar weight.
The invention is based on experimental studies of hydrocarbon fractions obtained by cracking acid tars. The experiments were aimed at developing a method for utilization of acidic tar containing sulfuric acid, without the use of any additives, reagents, oxidants and other components. In the course of the experiments, it was found that when cracking at temperatures below the coke formation temperature, asphaltenes contained in acid tar are split to form a vapor phase containing components that, when introduced into the non-volatile hydrocarbon fraction formed after cracking, yield a high quality bitumen satisfying GOST 22245-90 . To isolate these components from the vapor phase, it is necessary to isolate hydrocarbons with a boiling point above 200 ° C. The oily fraction forming thereby contains methanonaphthenes, alkylbenzenes, polycyclic aromatic hydrocarbons and is characterized by the absence of paraffinic hydrocarbons. The non-volatile hydrocarbon fraction withdrawn from the reactor contains resins, asphaltenes, carbenes and carboides. The optimum temperature regime for cracking and the use of an oil fraction with a specific boiling point depend on the composition of the acid sludge characteristic of a particular storage pond. At the same time, conducted studies with acid tars taken from 11 different storage ponds lead to the conclusion that oil-like hydrocarbon fractions can be used to produce bitumen, the boiling point of which does not exceed 360 ° C.
The best properties are the bitumen obtained with the use of acid tar containing no more than 7% sulfuric acid. In the process of obtaining bitumen, sulfuric acid acts as an oxidizer and vulcanizer, giving the bitumen elasticity, viscosity and other useful performance properties. In the case when the content of sulfuric acid exceeds 7%, acid tar is to be washed by any known method. A higher content of sulfuric acid (> 7%) leads to a decrease in the quality of bitumen due to increased brittleness.
By varying the temperature conditions and the content of sulfuric acid, it is possible to change the characteristics of bitumen in accordance with the requirements imposed by the conditions of its operation.
The figure shows a schematic installation for the production of bitumen.
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The installation comprises a flow type reactor 1, a differential condenser 2, a gas purification system 3, a mixer 4 and a receiving tank 5 for finished bitumen. The reactor 1 is connected by means of a pump 6 with a discharge tank 7 into which an acidic tar is charged. The steam hydrocarbon fraction formed in the reactor 1 is discharged to a differential condenser 2 where it is separated into condensable hydrocarbons, volatile hydrocarbons and acid gases with SO 2 , which are discharged to the purification system 3. Hydrocarbons with a boiling point above 200 ° C are used to produce bitumen, and hydrocarbons with a boiling point below 200 ° C and volatile hydrocarbons are used to produce other products, particularly fuels. The non-volatile hydrocarbon fraction withdrawn from the reactor 1 in the mixer 4 is mixed with the liquefied hydrocarbon fraction with a boiling point above 200 ° C entering the mixer 4 from the differential condenser 2. The finished bitumen is collected in the receiving vessel 5. |
Below are examples of specific implementations of the method.
Example 1
Anhydrous acidic tar with a sulfuric acid content of 5.0% is introduced into the flow reactor 1 heated to a temperature of 380 ° C and a non-volatile fraction is discharged into the mixer 4. Simultaneously, an oil-like hydrocarbon fraction with a boiling point of 250 ° C enters the mixer 4 from the differential condenser 2 . The fractions are mixed and discharged into the vessel 5, the yield of the finished product is 93% of the mass of the acid tar. The process of obtaining bitumen takes 10 minutes per 100 kg of acid sludge. Properties of the obtained bitumen: penetration depth of the needle at a temperature of 25 ° C - 73 mm, at 0 ° C - 27 mm; The softening point along the ring and the ball is 47 ° C; The extensibility at 0 ° C is 3.5 cm, at 25 ° C - 55-60 cm; Flash point is 230 ° C.
Example 2
Anhydrous acidic tar with a sulfuric acid content of 0.3% is introduced into the reactor 1 heated to a temperature of 400 ° C and a non-volatile fraction is discharged into the mixer 4. Simultaneously, an oil-like hydrocarbon fraction with a boiling point of 280 ° C enters the mixer 4 from the differential condenser 2. The fractions are mixed and discharged into a vessel 5; The output of finished products is 95% of the mass of acid tar. The process of obtaining bitumen takes 10 minutes per 100 kg of acid sludge. Properties of the obtained bitumen: penetration depth of the needle at a temperature of 25 ° C - 90 mm, at 0 ° C - 25 mm; Softening point on the ring and ball - 48 ° C; Stretch at 0 ° C - 3.7 cm, at 25 ° C - 63 cm; The flash point is 235 ° C.
The simplicity of the implementation of the method makes it possible to use it in mobile plants for the processing of tar in the pond storage areas.
CLAIM
1. A process for the production of bitumen from acid tar including dehydration of acid tar and heating, characterized in that heating is carried out in a flow reactor at cracking temperatures below the coking temperature to produce a non-volatile and vapor hydrocarbon fraction; from the steam hydrocarbon fraction, components with a boiling point greater than 200 ° C and mix them with the non-volatile hydrocarbon fraction withdrawn from the reactor.
2. A method according to claim 1, characterized in that acidic tar with a sulfuric acid content not exceeding 7% of the tar weight is used.
print version
Date of publication 15.12.2006гг
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