SU415889A3 - - Google Patents

Description

one

The present invention relates to a process for the preparation of surfactants, in particular a dispersing agent.

It is known to obtain surfactants by sulfonating monocyclic or bicyclic alkyl aromatic hydrocarbons, followed by neutralization with an aqueous solution of alkali.

However, the resulting dispersing agent causes, with stirring during the dispersing process, significant foaming, or, entraining air in the dispersible liquid, leads to the formation of a thin foam (foci of foaming).

In order to eliminate the formation of foaming and increase the dispersing ability of the proposed method, it is recommended to sulfate the product of high-temperature heat treatment (700-2000 ° C) of petroleum or coal raw materials. The dispersant obtained by this method can be used in various industries.

The petroleum or coal ore hydrocarbon feedstock used in the proposed method is a resin and a pitch obtained from cuts of crude oil, gas oil, kerosene, naphtha, heavy oil, asphalt, and from coal.

This raw material is heated at a temperature of 700-2000 ° C, preferably 900-1500 ° C for 0.0001-0.5 seconds, or preferably 0.005-0.1 seconds, and then the heated product

cooled in any way. When working with coal raw materials, heat treatment can be carried out at a temperature that the crude oil, but for a longer time.

High temperature heat treatment leads to significant chemical changes. The mechanism of these transformations is complicated, but the main reactions are the pyrolysis of hydrocarbons at high temperature and the polycondensation of pyrolysis products.

Liquid resinous vein

(tar) or hard pitch turns out to be very

rich aromatics.

The obtained resinous substance is a mixture of various substances, for example, a mixture of various condensed polycyclic aromatic compounds with different molecular weights, in which not only there are no aliphatic organic hydrocarbon molecules, even aliphatic side chains contain small quantities. A mixture of highly aromatic hydrocarbons is used as NLP directly as a raw material, or in the form of fractions obtained by various methods, for example, by distillation, extraction with solvents, etc., or it is subjected to further relaxation by frying at 350-600 ° C and then the resulting product. Subsequently, the highly aromatic hydrocarbons are sulfonated. The sulfonation reaction is carried out by any known method. Thus, the sulfonation can be carried out with concentrated sulfuric acid, the smoke with sulfuric acid, chlorosulfonic acid, sulfuric anhydride, etc. The degree of sulfonation depends on the conditions of sulfonation. The sulfonation reaction product is neutralized with an inorganic or organic base, for example, ammonium hydroxide, caustic soda, potassium hydroxide, calcium hydroxide, sodium phosphate, triethanolamine, morpholine, etc. The neutralization sulfonates (sulfonic acid salts) of condensed polycyclic aromatic hydrocarbons obtained can be used in a mixture other salts, obtained as by-products of the neutralization reaction, or they can be separated depending on the need. In addition, they can be used in combination with other salts and surfactants. Thus obtained sulfonates of condensed nolycyclic aromatic hydrocarbons are used as dispersing agents in various industries. For example, in the manufacture of refractories, in the preparation of pastes or suspensions, clay, cores, and the product is more compact with increased mechanical strength. The same results are obtained when forming carbon (coal) products with clay used as a drilling mud that is in contact with suction when drilling oil wells, etc. When using this dispersant in the production of cement mixtures, air does not get into the product, so that The test results for cement mixtures containing the patentable dispersant retain the necessary mechanical strength. Since this dispersant gives little foam, and in some cases, it is necessary to introduce air into the cement mixture to increase processability and to increase resistance to cold and melting, air introduction means is added from time to time. When using a dispersant in conjunction with a similar air firing agent, both additives act on the mixture, and the dissonator becomes useless as a means of air firing. Example 1. The desired naphtha is subjected to heat treatment at 1100 ° C for 0.04 seconds in an internal heating reactor and a gaseous substance containing acetylene and ethylene together with a resinous substance is obtained. The resinous substance is distilled at a temperature of up to 250 ° C under vacuum (residual pressure of 5 mm of mercury) and a pitch residue is obtained. Data from various analyzes show that this substance is a mixture of hydrocarbons with various condensed polycyclic aromatic structures. 30 g of pitch are treated with 40 g of concentrated sulfuric acid at a temperature of 80 ° C for 3 hours, then neutralized by the addition of calcium hydroxide and the precipitate is filtered. The filtered substance is evaporated, dried and 80 g of dark brown powder are obtained. Table 1 Quantity, Ingredient kg Cement (brands “Asano company, Nippon cement K °) Gravel (10 mm and larger)“ (10 mm and smaller) Sand (0.6 mm and larger) ”(0.6 mm and smaller) Water table 2 different quantities

 Weight,% in terms of cement.

b Level water content in the cement mixture without dispersant additives, taking the water content as 100.

 The amount of air involved, sediment and compressive strength are determined by Japanese J1SA standards -1128--1960 and JISA -1108-1963.

The resulting powdered material is added to the cement mixture shown in Table. 1 recipe.

The test results of cement mixtures containing different amounts of dispersant are presented in table. 2, from which it follows that with increasing dispersant content, the water content is significantly reduced, which leads to an increase in the mechanical strength of the cured cement.

Example 2. 30 g of sulfonated pitch of the same quality as in example 1, neutralized with caustic soda, receive 76 g of a dark brown sulfonate powder.

The dispersant obtained is added in varying amounts to the cement mix of the formulation given in table. 3. Test results of cement mixes with various

I Non-ionic surfactant manufactured under the brand name “Hi-Toam. Additives dispersant and vozhovov.evyekogo funds are given in weight. % of the total weight of the cement.

Example 3. Crude oil from Kuwait, heated to 300 ° C, is fed in a pulverized form at a rate of 1 kg / h, and superheated steam to 2000 ° C in a regenerative furnace using steam, using zirconium pebbles as a means of storing heat supplied at a rate of 5 kg / hour

Crude oil is in contact with superheated steam at 1100-1200 ° C for 0.06 seconds. Then it is cooled and 700 g / h of gaseous substance and 450 g / h of resinous substance are obtained.

The resinous substance is distilled at a residual pressure of 5 mm RT. Art. at temperatures up to 200 ° C and get pitch residue in the amount of 230 g / hour. This pitch residue, in accordance with the same analyzes as in Example 1, contains a mixture of hydrocarbons of various condensed aromatic polycyclic structures.

The pitch is sulfurized as described in example 1, and then neutralized with caustic soda. The sulfated pitch sodium salt thus obtained is applied to alumina forms. From the table. 5 results it follows that the dispersing agent obtained by the proposed method contributes to reducing the amount of water necessary to form a paste, as well as

Table 3

Amount,

Ingredient kg

15.0

firms

Cement (portland cement,

, Onoda cement K °)

44.1 Gravel (10 m.m. p. Larger) 14.7

, (10 mm and smaller) 22.3 Sand (0.6 mm and larger) 15.0

(0.6 mm and smaller) Water 8.3

Test results of cement mixtures,

contain, their various amounts of a disnergator, are provided to tab. 4, of which note the high ability of involvement

air and reducing the amount of water.

reduce the porosity of the mold casting and increases the mechanical strength.

Table 5

40

45

50

Note:

1) Ingredients:

alumina cement -10 wt. % of the weight of the unit aggregate - chamotte sand.

2) Curing is performed at room temperature for 24 hours.

3) Drying for 10 hours at 105 °.

4) Roasting at 1400.

Example 4. Obtained in example 3, the sodium salt of sulfonated pitch is used in the production of graphite briquettes with 65 clay as a binder. T a b. 4 and c. 4 amounts of dispersant. When adding the proposed dispersant, the amount of water needed to prepare the paste is reduced, while retaining it. Table 6 Water quantity,% Porosity,% Shrinkage during the drying process. 6 Compressive strength, after drying, kg / cm plasticity and the ability to process and roasted product has good mechanical strength, as is evident from the data given in table. 6. The subject of the invention. A method for producing a dispersing agent by sulphonating a hydrocarbon feedstock followed by neutralizing the sulphatic mass, characterized in that, in order to increase the dispersing capacity and decrease the foaming effect, the product is subjected to high-temperature heat treatment at 700-2000 ° C oil or coal raw materials.