SU632303A3 - Method of processing resin of pyrolysis hydrocarbon raw - Google Patents

Description

its air at 18О.300 С for О, 5-1О h with obtaining the fraction of aromatic condensed hydrocarbons and the residual fraction. Distinctive features: the method of heating the raw material and oxidation under the conditions described above. According to the invention, the feedstock is preheated, and air is fed to the oxidation reactor continuously or intermittently, depending on the type of reactor used. Air is brought into theoretical contact with the feedstock, for example, by passing it through the feedstock to accelerate the oxidation solutions. The fraction of aromatic condensed hydrocarbons is separated from the residual fraction by steam distillation. The residual fraction consists of a resin, initially contained in the feedstock, and polymer products, which are formed during the oxidation process, and is a mass from red-cinnamon to dark brown color, well soluble in aromatic hydrocarbons. Physical and chemical properties of the residual fraction depend t mainly depends on the duration and temperature of the oxide, as well as on the amount of air. With a continuous process, the duration of the oxidation, the temperature and the amount of air can be controlled by the rate at which the feedstock arrives. A change in the physicochemical /, properties is especially often traced by a change in the softening temperature. The parameters of the process parameters are shown at the temperature of the residual fvdia (by TSC) shown in Table. 1 The main indicators of the residual fraction are as follows: softening temperature (Tissue) 90 ° С, density, 1Д779, molecules, weight (average) 45О; viscosity at 94 ° C 1.710 spz, elemental composition,%: C 93.8; H 6.2; S O; 00 .. Fraction of aromatic condensed hydrocarbons is a fraction of oxidized aromatic hydrocarbons OB, which can be used to produce aromatic hydrocarbons not containing sulfur, to obtain aromatic compounds (aromatic oils with different boiling points) and in the production of ,, The yield of the fraction of aromatic hydrocarbons (by weight of the initial material), depending on the properties of the raw materials of the process conditions. Its composition is very insignificant at a certain baseline yield. Fraction components are aromatic hydrocarbons with no side chains or with very co saturated saturated side chains. their content in the fraction can be up to 90-1OO%. The content of compounds with an unsaturated side chain is much lower, since they are not stable to the effects of temperature and oxidation, during oxidative processing they are converted into compounds with a higher molecular weight and pass into the residual fraction. The ratio between the fraction containing aromatic compounds and the residual fraction can be varied by changing the time and temperature of oxidation, as well as the air flow. When the oxidation temperature increases by 5 ° -70%, the oxidation time and air consumption increase 6-7 times, the yield of the aromatic hydrocarbon fraction rises by 35-45%, and the residual resin decreases by 25-35%. The ratio between the aromatic and residual fractions With continuous process, you can also change it at the expense of the feed rate of the raw material. When the speed increases 3-3.5 times, the yield of the aromatic hydrocarbon fraction increases by 6 ° -7%, and the output fraction decreases by 15% -25%. This ratio can be adjusted by simultaneously changing the oxidation temperature, air amount and feed rate. Thus, with an increase in oxidation temperature by SO-50, C, a 3-fold increase in air consumption (taken by weight of the raw material) and an increase in the feed rate of the raw material by 1 / 5-1 / 4, the yield of the aromatic fraction will increase by 2-ZO% 8 a the residual heavy fracdine is reduced by 10-15%. The properties of the residual fraction also vary from time to time when the oxidation temperature and temperature and air flow change. The feedstock gasoline pyrolysis resin iiNieeT has the following characteristics: density d 1.0523; 1%, boils at 183 ° С | 5O vol.% - at 281 ° С | end of boiling point 306 ° C | composition of components, weight%: products boiling at a temperature below the boiling point of naphthalene 16j naphthalene 10 | 2-methylnaphthalene 5; 1 "-methyl l naphthalene 4 aime-1: silt aftinin 4 and proiopodnye 3; (iyoi eH ii production 6; phenanthrene and derivatives 7; anthracene 1; other coefficients 44. PRIMER 1. Raw materials heated to 21O C are fed at a rate of 81 O kg / into an oxidative reactor of the autoclave type with a reaction volume of 2.5 m The air feed rate is 55 im / h. During the reactions, the temperature of the reaction mass increases to C. A product is obtained containing 4O% (by weight of the raw material) fractions of aromatic hydrocarbons and 58% of the residual fraction. PRI me R 2. Raw materials preheated up to 200 ° C, continuously at a rate of 6OO kg / h are introduced into the reactor in an autoclave with a reaction volume of 2.5 The air is fed at a rate of 77 nm / h. During the reaction, the temperature rises to 27 ° C. The product obtained contains 43% by weight (based on the weight of the raw material, fractions of aromatic hydrocarbons and 56% by weight of a heavy pyrolysis resin. Example 3. The experimental conditions are the same as in example 2. After 10O hours of operation, the exhaust of the raw materials is stopped. The air supply rate is increased to 85 mph, and at this speed another 3 hours are used. 47% by weight (by weight of the raw material) of the residual fraction is obtained. Example 4. The raw material is preheated to 195 ° C and then continuously introduced into the autoclave with a reaction volume of 2.5 liters. The temperature in the reactor is maintained at 245 C. The feed rate (O, 58 kg / h) increases to 2.14 kg / h and at the same time the amount of supplied air is increased from 59 to 67 i «i / 4. The yield (based on raw materials) of the aromatic fraction increases from 23 to 38 weight. and the residual fraction is reduced from 77 to 62 wt.%. Example 5. In a reactor with a capacity of 2.5 l, 1.04 kg / h of raw material preheated to 198 C is continuously fed. The air supply rate is 67 nl / h-kg / raw material. The temperature in the reactor is increased from 245 to 26 ° C. The yield of the aromatic fraction (based on raw materials) increases from 33 to 4O, 5 wt.%, And the residual fraction decreases from 67 to 59.5 wt.%. The fractions of aromatic hydrocarbons obtained in examples 1-5, have the following composition; wt.%: hydrocarbons boiling at a lower temperature than naphthalene 22; naphthalene 16; 2-methylna4-talin 11; 1-1-methylnaphthalene 6; dnmethylnaphthalene 4; phenyl and its derivatives 5; acenaphthene and its derivatives 3 fluorene and its derivatives 9; phenanthrene and its derivatives 1O; anthracene 2; other 12.1 Vkod such fraction (in terms of raw materials) 49%, and the residual fraction (in the calculation of raw materials) 51 weight. The high correlation coefficient of the fraction of aromatic hydrocarbons (more than 10O) allows it to be used to produce carbon black. In addition, individual aromatic hydrocarbons, such as naphthalene, monomethylnaphthalenes, anthracide, etc., or aromatic oils with different boiling points can be distinguished from it. PRI me R 6. A batch reactor with a working volume of 0.5 l is charged with 0.5 kg of raw material. By changing the process parameters, the yield (in terms of raw materials) of the target products is changed. These experiments are given in table. 2. Properties of the residual fraction obtained in examples 1-3, are given in table. 3. The residual fraction is used in the preparation of rubber, paints and varnishes, the formation of masses, in the woodworking and construction industries as raw materials for fillers and auxiliary substances. In addition, coke with a low content of sulfur and ash, used to make electrodes, can be obtained from the residual fraction with an increased softening temperature. Table 1.

2O

180 51 20O

44

150

45 63

63

250

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