RU2027737C1 - Method of raw preparing for low-active technical carbon - Google Patents

Abstract

FIELD: chemical technology. SUBSTANCE: extracts of selective oil purification were subjected for extraction with furfural at the mass ratio furfural: raw = 1.2-1.5:1. Preferably, extract of selective oil purification is used in the mixture with catalytic gas oil at the mass ratio = 5-95:5-95. EFFECT: improved method of raw preparing. 2 cl, 2 tbl

Description

 The invention relates to a method for producing petroleum feedstocks for the production of carbon black used as a filler in the rubber and tire industries.

 Currently, the main focus is on obtaining high-index raw materials for the production of highly active carbon blacks.

 However, raw materials with a relatively low correlation index are necessary for the production of inactive carbon black.

 A known method of producing raw materials for low-activity carbon black by catalytic cracking of vacuum distillates on a cytolite-containing catalyst. The disadvantage of this method is the low yield (12.9 wt.%) From raw materials and high cokeability (2.49-5.3 wt.%) Of the target product with a correlation index of 90-105.

 The closest in technical essence and the expected result is a method for producing raw materials for inactive carbon black from extracts of the selective purification of oils. According to this method, the extracts of oil production in a mixture with gas oils of catalytic cracking are subjected to thermal cracking. The yield of the target product of thermogasoil is 24-32 wt. % of processed raw materials with a correlation index of 90-95 and coking ability of 0.8-1.5 wt.%.

 The disadvantage of this method is the relatively low yield of the target product, as well as the need to dispose of a significant amount of a by-product of the cracking residue having high viscosity and cokeability and not having the intended purpose without mixing with valuable low-viscosity products.

 The purpose of the proposed technical solution is to increase the yield of the target product using non-waste technology.

 This goal is achieved by the fact that the extracts of the selective purification of oils are subjected to repeated extraction with a mass ratio of solvent and raw material of 1.2-1.5: 1. Comparative analysis with the prototype shows that the new method is that the extracts of the selective purification of oils are subjected to re-extraction with a mass ratio of solvent and raw material of 1.2-1.5: 1.

 In order to increase the correlation index and yield of the target product, as well as reduce its coking ability and viscosity, extracts are subjected to selective extraction of oils in a mixture with catalytic gas oil in a ratio of 95: 5-5: 95 wt.%.

 Another difference is that the extracts are subjected to selective extraction of oils in a mixture with catalytic gas oil in a ratio of 95: 5-5: 95 wt.%.

 This technical solution is not obvious to experts in the field of obtaining raw materials for carbon black and therefore meets the criterion of "novelty."

 The essence of the method lies in the fact that the thermal and extraction processes for the processing of oil residues are fundamentally different.

 In the first case, chemical transformations of the hydrocarbons of the feedstock occur due to the thermal decomposition reaction, and, in addition to the main reactions of dealkylation of arrenes, secondary compaction reactions take place, resulting in the formation of a significant amount of by-products with high viscosity and coking ability, which adversely affect the formation of carbon black. In addition, light decomposition products are formed. Both high-boiling and low-boiling products must be removed from the reaction products, and therefore, the yield of the target fraction from the feed is relatively small. The residue from distillation (cracking residue) due to its high viscosity and coking ability cannot be a marketable product and for disposal it must either be further processed (for example, sent to produce coke or bitumen), or by introducing distillate fractions (such as diesel) coking ability to boiler fuel standards.

 In the process of extraction with selective solvents, in particular furfural, almost no chemical transformations of the feedstock occur. Selective solvent emits aromatic components, which are the raw material for carbon black without changing their structure. Non-aromatic components have a lower viscosity and coking ability than the feedstock, and can be used as a commercial product - boiler fuel, without mixing and distillate products.

 Mixing the extracts with catalytic gas oils before re-extraction improves the extraction process, since the high molecular weight alkylaromatic hydrocarbons of the extracts are dissolved by dealkylated aromatic hydrocarbons of the catalytic gas oil, which increases their solubility in furfural and increases the selectivity of the process, and as a result, the yield of the target product and its correlation index.

 The introduction of the process of extraction of dealkylated aromatic hydrocarbons also leads to a decrease in coking ability and viscosity of the target product.

 The invention is confirmed by examples.

PRI me R 1. The experiments are carried out on a laboratory extraction unit, furfural is used as a solvent, which is introduced into the upper part of the extraction column. The mid-column feed is introduced, heated to 50 ^° C and the weight ratio of furfural feedstock was 1.4: 1.

The temperature regime of extraction is as follows:
Extractor temperature, ^о С:
top 60
mid 50
bottom 40
From the resulting extract solution by distillation under vacuum at a residual pressure of 0.005 MPa in a stream of nitrogen, furfural is separated. The extract yield is 45 wt.% On raw materials. Qualitative indicators of the extract are presented in table 1 (see experiment 5).

 Subsequent experiments differ from the mass-solvent-to-raw material ratio described, which will be 1.1: 1, 1.2: 1, 1.3: 1, 1.5: 1, 1.6: 1, respectively. Yield of extract and its quality presented in table. 1 (see experiments 2,3,4,6,7).

Parallel experiments were conducted on a prototype, wherein in a laboratory extract in a mixture with a catalytic gas oil in a ratio of 50:50 wt.% Is subjected to thermal cracking at a temperature of 490 ^C and a pressure of 2.5 MPa. Distillation of the reaction products isolated target fraction (250-490 ° ^C), yield fraction was 32 wt.% Of the feedstock. Qualitative indicators of the target product are presented in table 1 (experiment 1). In addition, an experiment is carried out at a laboratory extraction plant in which a mixture of distillate extract and catalytic gas oil in a ratio of 50:50 wt.% Is used as the extraction raw material with the following extraction parameters.

Extractor temperature, ^о С:
top 60
mid 50
bottom 40
The mass ratio of solvent: raw material is 1.4: 1. The yield of extract was 51.0 wt.% From raw materials.

 Qualitative indicators of the extract are presented in table 2 (see experiment 4). Subsequent experiments differ from that described by the ratio of the extract and the catalytic gas oil in the mixture, which is 95: 5, 90:10, 80:20, 30:70, 10: 90, 5:95, 0-100 wt.%. The results of the experiments (yield of extract and its quality) are presented in table. 2 (see experiments 1,3,5-8).

 The data table. 1 and 2 indicate the following. Obtaining raw materials for inactive carbon black by the proposed method, in contrast to the prototype, allows to increase the yield of the target product with an increase in its quality (a larger correction index). The yield of the target product increases from 32 to 37-55 wt. % In addition, obtaining raw materials for carbon black extraction, compared with thermal cracking, allows you to get raffinate, the properties of which correspond to the requirements for fuel oil brand "40", that is, raffinate can be used as a commercial product without additional processing, which makes This technology is non-waste.

 In the case of thermal cracking, a significant amount of a highly viscous product is obtained, for utilization of which it is necessary to dilute it with diesel fractions or additional processing (see table 1, experiments 1-7).

 The data in Table 1 show that the optimum mass ratio of solvent to feed is 1.2: 1 - 1.5: 1. Extraction with a mass ratio of solvent: raw material of less than 1.2: 1 is not advisable, since in this case there is insufficient solvent and extraction practically does not occur (there is no phase separation in the extraction column), and the correlation index is not sufficient (see table 1 , experience 2). When the mass ratio of solvent: raw material is more than 1.5, the yield of the extract sharply decreases. The correlation index of the target product increases significantly, but at the same time, the viscosity and coking ability sharply increase, which negatively affects the process of producing carbon black (Table 1, experiment 7). Mixing the extract with a catalytic gas oil in a ratio of 95: 5 - 5: 95 wt.% Allows you to get an additional effect by increasing the yield and quality of the target product (the correlation index increases, and the viscosity and coking ability decrease) see table 2, experiments 1-7 . Beyond the boundaries of the specified interval, the effect of the additive in the feed of catalytic gas oil is below 5 wt. % is practically not felt (see experiment 5 of table 1 and experiment 1 of table 2), and when the extract content in the mixture is below 5 wt.%, the quality and yield of the extract practically do not differ from the extract obtained from pure catalytic gas oil (see experiments 7 and 8 of table 2).

 Thus, the above examples confirm the advantages of the proposed technical solution compared to the known method (the yield of the target product with higher quality increases and the process becomes waste-free).

 Implementation of the proposed technical solution is possible at practically no cost on existing installations for the selective purification of oils.

Claims (2)

 1. METHOD FOR PRODUCING RAW MATERIALS FOR LOW-ACTIVE TECHNICAL CARBON by treating extracts of selective oil purification, characterized in that the treatment is carried out by extraction with furfural in mass, respectively, furfural: raw materials 1.2 - 1.5: 1.  2. The method according to claim 1, characterized in that the extract is subjected to an extract of selective oil purification in a mixture with catalytic gas oil in a mass ratio of 5-95: 5-95.

Images