SU1456413A1 - Salts of n-sulfobenzylidene malonic esters as stabilizers of reverse emulsions - Google Patents

Abstract

The invention relates to organo-organic compounds, in the particular and salts of p-sulfobenzylidene malonic esters of the formula -MSO 3-e H CHjCOOR J, where R is octyl and M is sodium or R is dodecyl and M is potassium, or R is cetyl and M is ammonium, which can be used as stabilizers of inverse emulsions. The goal is to create more effective stabilizers. Synthesis of the target compounds is carried out by the reaction of dioctylmalonate or malonic acid dododendselnogo ester, or malonic acid dimethyl ester with benzaldehyde in the presence of piperidine and benzoic acid in benzene at boiling (16 hours) followed by treatment of the obtained product with dioxane-SOj complex in dichloroethane and a solution of sodium chloride, potassium or ammonium. Yield 22-30%. New stabilizers make it possible to increase the stability of the inverse emulsion from 6.5 to 7.5-8.5 hours. Table 2.

Description

I

This invention relates to the novel sol. M p-sulfobenzylidene malonic esters of the formula

3-011 CCCHgCOOR)

Kso,

where R is octyl and M is sodium or R is dodecyl and M is potassium, or R is cetyl and M is ammonium, which have the ability to stabilize hydrocarbon emulsions and can be used as stabilizers for reverse emulsions.

The aim of the invention is the improvement of new derivatives of sulfo-carboxylic acids, stabilized inverse emulsions and having a higher water-in-oil stability as compared to their counterparts - derivatives of diallylammonium (DAA-12),

Example 1. Sodium salt of p-sulfobenzylidene octyl mapping ether.

A solution of 122 g (0.37 M) of dioctyl smalll ester, 40 g (0.38 M) of benzaldehyde, 7 mp of piperidine and 1 g of benzoic acid in 200 mp of benzene is boiled for 16 h at 130–40 ° C with distillation of benzene with water. 200 mp of benzene are added, washed twice with water, 1N. HCl solution and saturated NaHC03 solution. The aqueous extracts were extracted with benzene, the benzene was dried with CaCl „. The benzene is distilled off, the ether ne09

about

distilled at 1 mm Hg. The product is placed in dry dichloroethane, 1 equimolar amount of dioxane-SOj in dichloroethane is added, and left for a day. The mixture is poured into saturated NaCl solution. The upper layer is collected, dried, washed with mist, heptane, and dried. Obtain 60 g (30% of theory) of the target product.

that

The analysis data are given. In. Table-1 Example 2. Kaliev salt of p-sulfobenzylidendodecyl small

the ether.

The compound was prepared as in example 1. Take 163 g (0.37 M) of maloniconic acid dodecyl ester. Get 53 g (22% of theory) of the target product.

Example 3. The ammonium salt of p -sulfobenzylideneacetyl ether.

The compound was prepared as in example 1. Take 206 g (0.37 M) of malonic acid diethyl ester. Obtain 64 g (23% of theory) of the target product.

that

The stability of the emulsion is determined after stirring for 10 minutes a mixture of 10 ml of water and 1% emulsifier in xylene. Examine the limit of destruction in a centrifugal field of 5000 rpm in comparison with the known DAA-12.

Data analysis of compounds are given in table. 2

Comparison of data table. 1 and 2 show that the new compounds form more stable water-in-oil emulsions, which makes it possible to recommend them for use in industry.

Salts of p-sulfobenzylidenmalonovye esters of the formula

MS (SN COOR)

where R is octyl and M is sodium

or R is dodecyl and M is potassium,

or R is cetyl and M is ammonium,

as reverse stabilizers

emulsions.

IT a b l and c a 1.

Claims (1)

Claim Salts of p-sulfobenzylidene malonic 2o esters of the formula MS CH = C (CH ₂ COOR) ₂ where R is octyl and Μ is sodium 25 or R is dodecyl and M is potassium, or R is cetyl and M is ammonium, as stabilizers of inverse emulsions. - - L-r ^ n- -ι 1T a b l and c a 1. 1 & imer X .. " CM PIR, Hz " Found % Calculated,% ^ c = c j '’SgO. Leng) from I ^st Ll. C ___ L * 1 1720 1630 1230 95.0 58.8 7.9 6.0 60.3 7.55 6.19 2 1718 1630 1220 94.2 62.0 8.8 4.75 63,2 ^8.5 5,0 3 1721 1630 1220 94.6 67.3 11.4 4.2 68.5 10,2 4.35 table 2 Connection example Decrease in; Time is full surface tension at the water / air interface, erg / cm ² the first destruction of the emulsion, h 1 28 8.0 (fifteen)* 2 32 8.5 3 thirty 7.5 DAA-12 39 6.5 (12.5) * * Destruction time at 3000 rpm.