SU1302651A1 - Method of producing ammonium salts of aliphatic acids - Google Patents

Abstract

The invention relates to aliphatic acid derivatives, in terms of the ammonia salts of C-Su-aliphatic acids (1), which I can. to be used in chemical and petrochemical production of various substances, as well as preservatives of feed in agriculture. Simplification of the process of obtaining 1 is achieved by using a solvent and corresponding further processing. Synthesis is carried out from the corresponding acid and NHj at a temperature of 20 and pressure of 1-10 atm in the medium of the hydrocarbon Su-C, followed by purification of the salt from the solvent in a stream of NHj at 40 -. The method provides obtaining of 1 high degree of purity with a high-quality yield with low corrosion of the apparatus g and can be carried out both in periodic and continuous mode. me (Luo Sp

Description

The invention relates to petrochemical and chemical production, specifically to methods for producing ammonium salts of organic acids.

The purpose of the invention is to simplify the process of obtaining dry ammonium salts of aliphatic acids used as preservatives in feed.

PRI me R 1. 100 g of a 40% formic acid solution in hexane is loaded into the apparatus with mixing and 19.2 g of gaseous or liquid ammonia are fed under pressure (molar ratio acid: ammonia is 1: 1.3 ). At a temperature and pressure of 1 atm, the mixture is stirred for 10 min. Unload the suspension. After filtration, the salt is dried at 75 ° C in a stream of ammonia gas. Hexane is tested for formic acid. Lastly absent. 54.8 g are obtained (100.0% of ammonium formate stoichiometry with mp. 116-117 C. Content of hexane; 0.0005 wt.%. The balance of the experiment is shown in Table 1.

T a b l and c a

40 (33.6)

19.2 (16.1) 4.4 (3.7) 60 (50.3) 60.0 (50.3)

- (-) 54.8 (46.0)

.119.2 (100.0) 119.2 (100.0) 45

35

40

Example 2. 100 g of a 30% propionic acid solution in the penta-hexane fraction are loaded into the apparatus with stirring, 10 g of ammonia are added and the mixture is kept at a temperature of 70 s and 5 atm for 5 minutes. The molar ratio of acid: ammonia is 1: 1.5. After cooling, the ammonium propionate suspension is discharged into the pentane-hexane fraction. The resulting salt is separated by filtration. solvent, the salt is dried at 70 ° C in a stream of ammonia gas. Obtain 36.9 g (100% of stoichiometry) ammonium propionate with so pl. 107 s. The balance of the experiment is given in table. 2

Table 2

Propionic acid

Ammonia

thirty

ten

(27.3) (9.1)

3.1

(-) (2.8)

thirty

Total

110

(100) 110 (100)

Example 3: The process conditions are as in Example 2, but the solution of isobutyric acid is loaded into

pentane. The molar ratio of acid: 1: 1.7. The reaction proceeds in 3 minutes at a pressure of 10 atm. After filtration and drying, in a flow of gaseous ammonia, 35.8 g (100.0% of stoichiometry) of ammonium isobutyrate with m.p. .

The balance of the experiment is given in table. 3. Table 3

313n26S14

Continuation of the table. 3 stoichiometry | 1mi) formpatl lmmopp g

m.p. 116-f17 C. Content gtksana 0.0005 wt.%.

The balance of the experience is given. Table. five.

EXAMPLE 1: The conditions of the process are as in Example 1, but a load of 200 g of a 20% strength solution of isovaleric-5 ananoic acid and 6.7 g of ammonia (molar ratio acid: ammonia t: 1). 46.5 g (99.7% of stoichiometry) of ammonium isovaperianate with m.p. . 20 formate

The balance of the experiment is given in table. 4. ammonium

Table A

Isovaleric acid .40

Hexane

Ammonia

Izovalerianate

Dichlorum

160

(19.4) 0.1 (0.05) (77.4) 160 (77.44)

thirty

The continuous method allows to simplify the apparatus and the process technology and to obtain pure salts with a quantitative yield. The lack of dissociation of the acid or salt under the conditions of the process creates a low

6.6 (3.2) 0.02 (0.01) 35 The corrosiveness of the reaction

medium, which allows the process in the apparatus of low alloy steels. The process can be pea-, lizovan both in periodic, and

(-)

46.5 (22.5)

It.o about 206.6 (100) 206.6 (100)

At measure5. 100 g of a 40% solution of formic acid in hexa and 44.3 g of ammonia (molar ratio of acid: ammonia, 1: 3, O) are loaded into the apparatus with stirring. At a temperature and pressure of 5 atm, the mixture is stirred for 5 min. Unload the suspension. After filtration, the salt is dried with ammonia gas in a stream. 54.8 g (100% of

40

in continuous modes.

Claims (1)

Invention Formula 45 The method of producing ammonium salts of aliphatic acids by reacting acid and ammonia at 20-70 ° C, characterized in that, in order to simplify the process, it is carried out in the presence of a solvent, which uses hydrocarbons and at a pressure of 1-10 atm. subsequent purification of the salt obtained from the solvent in a stream of ammonia at 40-75 ° C. VN1ShPI Order 2782 Circulation 352 Subscription Proizv-polyr. pr-tie, Uzhgorod, st. Project, 4 (27.7) - (-) (30.7) 29.5 (20.4) (41.6) 60.0 (4t, 6) 54.8 (38.0) thirty medium, which allows the process in the apparatus of low alloy steels. The process can be pea-, lizovan both in periodic, and in continuous modes. Invention Formula The method of producing ammonium salts of aliphatic acids by reacting acid and ammonia at 20-70 ° C, characterized in that, in order to simplify the process, it is carried out in the presence of a solvent, which uses hydrocarbons and at a pressure of 1-10 atm, followed by cleaning the resulting salt from the solvent in a stream of ammonia at 40-75 ° C.