SU859356A1 - Alkanolamine salts of alkylsulfates as surface-active substances - Google Patents

Description

(54) ALKANOLAMINE SALTS OF ALKYLSULPHATES AS SURFACE-ACTIVE SUBSTANCES

one

The invention relates to new compounds - alkanolamine salts al -. Kilsulfates Formula

R о SO ,, NH () y, I where R is the residue of the alcohol fraction

g ... g

 - (to iopropyl and or

R is the residue of the alcohol fraction

 10 in

 butyl to,

or

R is decyl;

 isopropyl and

or

R-pentadecyl;

R is isopropyl and

which exhibit surface-active properties and therefore can be used in formulations of synthetic liquid and paste-like detergents, cleaning and polishing agents, in the textile, cosmetic and pharmaceutical industries, in compositions of household chemicals and other areas of national economy, using surface active agents (surfactants).

The closest to the proposed are various ethanolamic salts of alkyl sulfates, for example, triethanolamine salts of secondary alkyl sulfates or triethanolamine alkyl sulfates, which have the surface-active properties Cljl

and r2.

However, the known surfactants have not enough high foaming ability of their aqueous solutions.

The purpose of the invention is to expand the ar10 of the surfactant surfactant, which, along with good surface activity, would have a higher foaming capacity and foam stability.

Yale delivered

15 new alkanolamine salts of alkyl sulfates of formula I, which can be used as surfactants and have a high foaming surface and foam stability.

20

The novel compounds of formula I are obtained by sulphating the corresponding alcohols with an gas-air mixture containing 6 to 9% by volume of sulfuric anhydride at 45-50 ° C, followed by treating the obtained sulfas with an aqueous solution of the corresponding alkanolamine at 30-55 °.

Example 1. Diisopropanolamine salt apkylsulfate "1 anodine-30 alcohols

The preparation of this salt is carried out in two stages. In the first of these, the sulfation of alcohols is carried out according to a known method on an operating industrial saw installation. For sulfating, a fraction of alcohols is used, the composition of the second group includes alcohols in an amount up to 75%, Sb-Cd up to 10% and, j5 up to 15%.

Characterization of alcohols: Hydroxyl 250-290 mgKOH / g

number (average

193-224 cu.) Pier, weight Acid

Not more than 0.2 mgKOH / g number of Essential

Not more than 2.5 mgKOH / g number

Hydrocarbon content not more than 2.5 wt.% Dov

Content Not more than 0.3% by weight of moisture Iodine Not more than 13 MrJ, j / 100 number Carbonyl Not more than 2.0 mgKOH / g No colorless or slightly Appearance yellowish mobile liquid

The first stage — the preparation of sulfomass — is carried out by sulphating synthetic primary fatty alcohols with a gas mixture containing 6–9% sulfuric anhydride. The sulphating gas mixture is obtained by burning sulfur at the air point, followed by catalytic oxidation of sulfur dioxide to sulfuric oxide on vanadium oxide catalysts at 450-550 ° C Sulfation is carried out in continuous mode. The process is carried out in E 5 sulfurizing reactors. Alcohols are injected into the first anos sulfonator and are transferred sequentially to all the other sulforators through the streams, and the sulphating gas mixture is fed into all the sulphurisers in parallel.

Process conditions: Alcohol consumption 1040 kg / h. Sulfur consumption 130 kg / h. Air consumption 1200 MV Temperature

sulphation 45-50 ° C. Second stage. Load 70 g of diisopropanolamine and 300 g of water into a two-neck flask equipped with a thermometer, a stirrer, and a cooling water bath. The mixture is stirred and 70 g of the sulfomass obtained in the first stage are added at such a rate that the temperature of the reaction mass does not exceed 50 ° C. As a result, 440 g of product are obtained, which are analyzed in the aforementioned mesodic: surface tension and critical concentration according to the Rebinder method / foaming ability, appearance, water solubility, pH (pH of 1% solution), content of non-sulphated substances, water, inorganic salts and alkanolamine sulfate, as well as optics eska product density on triethanolamine salts of alkyl sulfates,

Examples: 2,3 and 4. Triisopropanolamine, monoisopropanolamine and monobutanol salts of alkyl sulfates in the alcohol fraction.

Salts are transmitted by identical steps to obtain the diisopropanolamine salt of alkyl sulfates (Example 1), only in the second stage of the process, instead of 70 g of diisopropanolamine, the corresponding amine is taken in the amount shown in Table. 2

Characteristics of the products obtained are given in table.1.

Example 5. Under the conditions of Example 1, decyl alcohol was subjected to sulphation with a gas mixture, and then 70 g (0.295 M) of the resulting sulfomass were added under continuous conditions of stirring and water cooling to 396 g of a 15% aqueous solution of triisopropanolamine for 5 minutes (0.302 M). The result is a 28% aqueous solution of the triisopropanoamine salt of decyl sulfate with a non-sulfated product content of 1.0%. The resulting product is an easily mobile fluid that lowers the surface tension of water at a concentration of 0.3% by active substance from 72 to 32 dyn / cm. 5. The triisopropanolamine salt of decyl sulfate is isolated by known methods.

Example 6. Pentadecyl alcohol under the conditions of example 1 is subjected to sulfation, and then 154 g (0.5 M) of the resulting sulfomass under the conditions of example 5 is added to 250 g of a 35% aqueous solution of triisopropanolamine (0.5 M), B As a result, 406 g of paste are obtained with a content of the triisopropanolamine salt of pentadecyl sulfate 58.0% and non-sulfated substances 0.8%. Paste is well soluble in hard water, at a concentration of 0.25% (on the basic substance) has a good foaming ability. The triisopropanolamine salt of pentadecyl sulfate is isolated by extraction with a solvent by distillation.

Example 7.119 g (M) of the sulfomass prepared according to Example 5 is added to 224 g of 30% aqueous

60 solution of diisopropanolamine. 400 g of 46.0% diisopropanolamine salt of decyl sulfate are obtained. The latter is isolated by known methods. 0.25% solution

65 decylsulfate dinzopropanolamium salt lowers the surface tension of water by a factor of 2.3 and gives foam with a factor of 0.93,

In tab. 2 shows the conditions for the preparation of alkanolamine salts. ,

The new compounds have surfactant properties and can be used as surfactants.

The tests were carried out according to generally accepted methods: the foam-forming ability according to the Ross-Miles method. Rehbinder surface tension, critical micelle concentration (CMC found graphically).

The test results are shown in table 3.

The data shown in Table 3 shows that alkanolamine salts of alkyl sulfates, obtained both on individual alcohols and on the fraction of alcohols f, are surface-active substances. At a concentration of 0.25%, they reduce the surface tension of water by more than 2 times. These compounds have a high foaming ability and are distinguished by the mild effect of their aqueous solutions (up to 40%) on the skin of the hands.

Table 4 gives the characteristic of the surface-active properties of the known triethanolamine salts of alkyl sulfates.

As can be seen from the data presented in Table. 3 and 4, new surfactants — alkanolamine salts of alkyl sulfates are not inferior in terms of the surface activity of the known triethanolamine salts of alkyl sulfates (surface tension of solutions 32–34 dyn / cm), but at the same time the new substances have a higher

: foaming ability and .stability foam foam.

five

In addition, the advantage of new alkanolamine salts of alkyl sulfates is the technological safety of the production of the raw material. Oxide

0 Propylene is practically non-hazardous and non-toxic compared to ethylene oxide, which is an intermediate in the production of triethanolamine. High foaming ability of new alkanolamine

5 cpe lyl sulphates are of great value for the preparation of fire extinguishing agents.

Surface tension, dyne / cm Critical concentration, micelle formation,% Foaming. capacity, mm Appearance Solubility in water Hydrogen index (pH) of 1% solution Content of non-sulfated substances,% Water content,% Content of inorganic salts Optical density

Tab. egg 1 7.2 1.3 69.1 0.2 mobile liquids Full 7.0 7.8 1; 11.7 0/0 69.5 no 0,20,2

70.0

122.0 300.0 35

100.0

122.0 400.0 35 40.0

125.0 250.0 35

50.0

162.0 250.0 35

Diisopropanolamine salt of alkyl sulfates on the fraction of alcohols

R-G -10

Triisopropanol 1min salt of alkyl sulfates on the fraction of spit (in

Monoisopropanolamine salt of gishyl sulfates on the fraction of alcohols

Monobutanolamine salt of hyskylsulphates in the alcohol fraction

(at

Triisopropanolamine salt of desyl sulfate

Triisopropanol salt1 salt of penthenescylsulfate

Diisopropanolamine salt of decyl sulfate

table 2

492 38.0

5,622 35.0

415 39.0

62 45.5

210 32.3 0.063 0.96

215 33.9 0.059 0.93

200 29.6. 0.059 0.93

215 34.6 0.065 0.95

210- 33.9 0.053 0.96

220 32.6 0.052 0.96

0.93 Triethanolamine salt of lauryl sulfate Triethanolamine alkylsulfates synthetic, primary Triethanolamine salts gshkilsulfaTofi on the fraction of alcohols,, Triethanolgimine salts of secondary EShK sulfate

formula I of the invention Alkanols1 New salts of alkyl sulfates of the formula I

R Oh,) p,. where R is the residue of the alcohol fraction

V3

corrugated and or the residue fraction of alcohols

,at ,

butyl and, or

decyl;

Table 4

R. - isopropyl and, or R - pentadecyl; isopropyl and, as a surfactant.

Sources of information taken into account in the examination

1. USSR author's certificate 740754, cl. C 07 C 141/02, 06/27/78.

2. USSR author's certificate 1 5231Eb, cl. CUD 1/14, 69.09.74.

Claims (1)

Formula of the invention Alkanolamine salts of alkyl sulfates of the formula I 8o C O NH ₄ _ _{5 minutes,} {R ^ OH) _n, where K - residue fraction ^alcohols 40 ^{-? (1β} ' K ^ is isopropyl and n = 1-3 or K is the remainder of the alcohol fraction ^C / H> “ ^C 4B ^; butyl and n = 1, or K is decyl; isopropyl and n = 2-3, or K - pentadecyl; K ^ - isopropyl and n = 3, as surface-active 35 substances.