SU1047907A1 - Method of producing phosphate surfactants - Google Patents

Abstract

Odys of production of surface-active phosphoric acid esters by phosphorylation of higher hydroxyl-containing compounds with phosphoric anhydride; , or a lower carboxylic acid, taken in the amount of 1 wt. h. 1.7-20.5 ma.ch. higher aliphatic alcohol.

Description

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This invention relates to organophosphorus compounds; It is important for the method of obtaining the surface-active phosphoric acid esters, which find their use as dispersing agents, polymer modifiers, additives for various purposes in composites.

A known method for producing alkyl phosphorus surfactants phosphorus is the reaction of ethoxylated higher alcohols with phosphoric anhydride in the presence of water additives (1-10 -3% by weight of the starting alcohols) at 12G-13Q ° C Cl.

There is also known a method for producing alkylphosphoric surfactants by phosphorylation of higher ethoxylated alcohols with polyphosphoric acid in the presence of amino alcohols in SO-XO C 2.

The closest technical essence and achievements / results to the proposed is a method of obtaining surface-active phosphoric acid esters by phosphorylation of higher aliphatic alcohol with phosphoric anhydride in the presence of

additives containing O from 2 to b hydroxyl groups with a molar ratio of 1: 2: 4 / p, where n is the number of hydroxyl groups of the alkyl polyol at 0-120s 3 3.

However, the products obtained by this method exhibit insufficient surface activity, have a high pour point, are poorly soluble in water, and are noticeably colored

The aim of the invention is to improve the quality of the target products.

The goal is achieved according to the method of obtaining surface-active phosphoric acid esters by phosphorylation of higher hydroxyl-containing compounds with phosphoric anhydride at 30-90 0 followed by treatment of the resulting product with lower aliphatic alcohol or C.-C5 alkylphenol or lower carboxylic acid, taken in an amount of 1.mas., h. at 1,720,5 mache.h. higher aliphatic alcohol. I

Example 1 {prototype). 1048.5 g of primary fatty alcohols of C -, (, - Ci8 6-09-4147-76) fraction, 362.1 g of 1,2-butanediol (TU 6-09-28278), 6 g are loaded into a 2 liter reactor. phosphoric acid and 567.9 phosphoric anhydride (MRTU 6-09-71776), the phosphorylation is carried out with stirring for 3 hours at 60 ° C. Get 1826.2 g of the product, the quality indicators and physicochemical properties of which are presented in table 1. and 2.,

Example2. K800g primary fatty alcohols of the C-, (C 38-10730-72) fraction are added. With stirring, 348 g of phosphoric anhydride, stirred for 0.5 h. Per hour and 147.0 g of iopropanol (TU 6-0.9402-75) are added. The weight ratio of high molecular weight: low molecular weight alcohol is 5.44: 1. 1245.8 g of final product are obtained. Analysis results

0 and the physico-chemical properties of the product are presented in table 1 and 2.

For example, to 1022.8 g of acidic alkyl phosphates based on secondary fatty alcohols of the fraction (TU 38-40848-80) under the conditions of Example 2 was added 50.2 g of methanol (GOST 6995-77). The ratio of 20.5: 1. Get 1119,0 gzelnogo product, characteristics and properties of which 0 are shown in table 1 and 2.

Note 4. to 800 g of primary fatty alcohols fraction. (according to example 2) 348 g of phosphoric anhydride are added with stirring at 80 ° C. After 1 h after the start of phosphorylation, 480.7 g of isooctylphenol (r. 270.3

k.ch. 0.5, 1%). The ratio is 1.67: 1. Get 1531 g of the target product, characteristics and properties of which are presented in table 1 and 2.

Example K800g of decyl alcohol, ethoxylated with 3 moles of ethylene oxide, was added 244.8 g of phosphoric anhydride with stirring at 70 s. After about 0. 5 hours, 127.6 g of tert-butanol (TU 6-09-406975) was added, the ratio was 6.3: 1. Get 1145,3 g of the target product, the characteristics and properties of which are presented in table 1 and 2.

Example To 800 g of the primary fatty alcohol fraction (according to example 2), 34.8 g of phosphoric anhydride are added with stirring at 90 ° C. After 0.5 h, 40 g of isobutyric acid (TU 609-72448) are added. The ratio is 20: 1. Get 1176.1 g of the product, the characteristics and properties of which are presented in table 1 and 2.

P: R and measure 7. To 1000 g of dodecylphenol, ethoxylated at 4 moles

/ 11/1 kgTHERON ethylene oxide (r.u. 124-,

.. 0.2

H <0> 0.5% by weight, 188.3 g of phosphoric anhydride are added with stirring at 40 ° C. After 0.5 h, 79.5 g of isopropanol are added (as in Example 2). The ratio of 12.6: 1. 1170.1 g of product are obtained. characteristics and properties of which are presented in Tables 1 and 2. Example. To 1000 g of dodecylphenol, oxethylated on 4 mol of ethylene oxide HjO 0.5 wt.%), K.H. 0.2 was added with stirring 188.3 phosphoric anhydride at 30 ° C. After 0.5 h, 98.1 g of tert-butanol is added. The ratio is 10.1: 1. 1261.9 g of product are obtained, the characteristics and properties of which are presented in Tables 1 and 2.. Sample To 1022.8 g of acidic alkyl phosphates based on secondary fatty alcohols of the C g-Czoi fraction obtained in accordance with the example, 94.1 g of isopropanol are added with stirring at 70 ° C.

Table 1152.4 g of the product, the characteristics and properties of which are presented in Tables 1 and 2. As can be seen from the data of Table 2, the surface-active esters of phosphoric acids, obtained by the proposed method, are of higher quality than the known Cz2 compounds. Thus, the proposed method makes it possible to lower the pour point by 5-20 ° C, increase the solubility in water by 10-20 times, lower the surface tension by 1.2-1.5 times, and produce less colored products. All these factors are important because they make it possible to use the surfactants obtained in the form of aqueous solutions at lower temperatures, especially in winter, while many surfactants lose their effectiveness under these conditions.

Table 2

) the index at the value e means the value of concentration (May.

Claims (1)

METHOD FOR SURFACE-ACTIVE phosphoric acid esters of higher phosphorylation of hydroxyl compounds with phosphoric anhydride: _s 30-90®S characterized 'in that, to improve the quality of the target products, the product phosphorylation higher aliphatic alcohol phosphoric anhydride is treated with lower aliphatic alcohol or C ^ -Cg-alkylphenol, or lower carboxylic acid, taken in an amount of 1 wt.h. 1.7-20.5 parts by weight higher aliphatic alcohol. SU, 1047907