SU721432A1 - Method of combined preparation of acyclic and cyclic amines - Google Patents

Description

3

an amine with 1-6 mol of ammonia under pressure of hydrogen from 1OO-4OO atm at 2OO26O C in the presence of a hydrogenation catalyst.

This forms a mixture of etipenediamine diethylenetriamine, piperazine (P), N - (p-amino-ethyl) -piperazine (AEP), aminoethylethanolamine and higher amines. The ratio of the target products strongly depends on the molar ratio of the starting products, but the conversion of the starting ethanolamine does not exceed 80% 4.

The disadvantages of the known method 5W-l gots are the relative deficiency of ethanolamine, the use of a catalyst and the relatively low conversion of ethanolamine.

The aim of the invention is a simplified process. associated with the absence of a catalyst and using more access to the first precursor dichloroethane.

This goal is achieved by the method of joint production of acyclic and cyclic amines, which consists in the fact that dichloroethane is reacted with 73-77% aqueous solution of pthiac with a starting material ratio of 1: 6.5-7.5 by weight under a pressure of 75-8 p ATM and at 11О130 С.

After carrying out the process in the synthesis reactor, the excess ammonia is stripped in high and low pressure evaporators, the amine chlorohydrates are neutralized with 33-42% alkali. Aqueous amines are evaporated at 12 ° –140 ° C, after which they are transferred to a distillation column in which water is distilled off at 99–1O1 ° C, the vat residue is dried azeotropically (81.5% EDA and 18.5% water at 4-6 aTivi) , then allocate marketable EDA with a yield of 75-80% (the content of the target product is at least 95%).

The cube of the column contains less than 1% water, about 2% EDA, 6O-65% EDTA, 3-5% P. 13-15% AED, the rest is higher amines. EDTA (with a purity not lower than 96%) and Pi AEP (with a purity not lower than 80%) are distilled from the bottom liquid by distillation.

In the following examples, the quantitative composition of the reaction mixtures is determined on an LHM-72 chromatograph with a thermal conductivity detector, a fluoroplast-4 sorbent treated with a silicone elastomer, a helium gas carrier, speed of 5 O ml / min.

4324

column temperature (EDA); 15O С (EDTA, AED), evaporator temperature (EDA); 250 ° C (EDTA, AEP).

Example 1. In the synthesis reactor serves dichloroethane in the amount of 10OO kg / h and ammonia 76% in the amount of 7296 kg / h. The ratio of components is maintained equal. 1: 7.3. The synthesis is carried out at 115130 C and a pressure of 8 O atm. Excess ammonia is stripped in high and low pressure vaporizers, after which the amino-hydrochlorides are neutralized with 3342% scab. The aqueous amines are evaporated at 12 ° -40 ° C, after which they are fed to a distillation column, where water is distilled off at 99-10. The contents of the cube (O 6 O 6% amines) are sent to the next distillation column to dehydrate the azeotropic EC.A, which forms an azeotrope of 81.5% EDA and 18.5% water, under a pressure of 4-6 kg / cNf. After that, at the third distillation column at atmospheric pressure (the temperature of the top of column C), commercial ethylenediamine was isolated in an amount of 465 kg / h, 77.5% yield in one line with 2 strands, content 97.5% (chromatographic analysis) . The cube of the column after the release of ED in the amount of 135 kg / h in a single line of the composition,%: water 0.4, EDA 2.2 piperizin 4.1 DETA 63.2 P) -amino ethyl piperazine 14.2, higher amines - 16.0, sent for separation by fraction.

Thus, the yield of α-amino ethyl piperazine is 19.2 kg / h, the yield is 3.2%.

Example 2: Under conditions of Example 1, 10OO kg / h of dichloroethane and 74% of ammonia were 6552 kg / h. The ratio of source1.1X components is maintained at 1: 6.5. The synthesis is carried out at 11513 ° C at a pressure of 75 atm. The rest of the operations and the nth sequence are the same as in the first example.

EDA was selected 455 kg / h, yield 75.8%, content 96.6% during chromatographic analysis.

Polyethylenepolyamines obtained 145 kg / h composition,% water 0.5 EDA

2.0, piper-ezin 4.0, DETA 63, 1 p -amino ethyl nitperazin 14.8, higher 15.6. The amount of α-aminoethylpiperazine is 21.4 kg / h, the yield is 3.6%.

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Formula H3o6peTefiHfl

The method of joint production of acyclic and cyclic; amines based on ethylene and ammonia derivatives at elevated pressure and temperature, about the fact that, in order to simplify the process, dichloroethane is used as an ethylene derivative, which is reacted with 73-77% aqueous ammonia solution with a ratio of initial products 1 : 6.57, 5 by weight under pressure of 75-8 O atm and at 110-130 2.

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Sources of information taken into account in the examination

1. The patent of Italy 6173-48, CP. C O7 C 4, publ. 1961.

2. Patent-Italy No. 631882, cl. C 07 C 4, pub. 1962.

3. The temporary technological regulation of production is ethylenediamine. L.,

1966.

4. US patent number 3151115,

cl. 26О-268, rggubl. 1964, (prototype).

Claims (1)

SUMMARY OF THE INVENTION A method for the joint production of acyclic and cyclic amines based on a derivative of ethylene and ammonia at elevated pressure and temperature, about 5-5 liters, and that, in order to simplify the process, dichloroethane is used as an ethylene derivative, which subjected to interaction with a 73-77% aqueous solution of ammonia with a ratio of starting products 1: 6,5- 7.5 by weight under a pressure of 75-80 atm and at 110-130¾.