Procedure for extraction of amine

FIELD: machine building.

SUBSTANCE: electrochemical treatment of amine-chlorine-hydrate is performed in four-chamber electrolyser with ion-changing membranes at density of current 100-500 A/m. For this purpose the chamber of electrolyser next to a cathode chamber is filled with solution of amine-chlorine-hydrate for extraction of amine from it. Also, cathode and anode chambers are separated with cation exchanging membranes; while an anion exchanging membrane is set between the second and the third chambers of electrolyser. Amine is concentrated in the cathode chamber, and hydrochloric acid is concentrated in the chamber of electrolyser next to the anode one.

EFFECT: raised ecological safety of procedure, reduced power expenditure at extraction of amine.

2 cl, 1 dwg, 2 tbl, 2 ex

 

The present invention relates to the selection of amines from clorhidrato generated in the process of their reception.

A method of obtaining amines (in particular, Ethylenediamine) the interaction of 1,2-dichloroethane with ammonia. In the reaction is an aqueous solution of amanohashidate. To highlight the amine, the reaction mass is treated with a solution of sodium hydroxide, and the resulting mixture containing water, ammonia, sodium chloride and amine, is subjected to evaporation, and then rectification (Lebedev N.N. Chemistry and technology of basic organic and petrochemical synthesis. Ed. 2nd Per. - M.: Chemistry, 1975. - 736 S., pp. 336-339).

The disadvantage of this method is that the VAT residue after evaporation, representing an aqueous solution of sodium chloride mixed with amines, generates large amounts of wastewater.

A method of obtaining amines (in particular, piperazine) from the halo-genorosity organic substances, in which is formed an aqueous solution of aminoguanidine containing excess acid. To highlight amines this solution is treated with alkali, is evaporated and sent to distillation (U.S. Pat. 3095417 USA, NRI 260-268. Process for production of piperazine / Poppelsdorf, Richard Smierci (USA) - No. 44005; claimed 20.07.60).

The disadvantage of this method is the formation of large quantities of wastewater, pre the excitation VAT residue after evaporation and containing salt mixed with amines (1-2%).

Closest to the claimed, i.e. the prototype is the allocation method of piperazine aqueous solution of its hydrochloride, whereby a solution of the hydrochloride before treatment with alkali electrolyzed in a three-chamber electrolyzer containing cation-exchange and anion-exchange membranes (A.S. 1155597 the USSR, MKI 07D 295/00; SV 3/00. The allocation method piperazine / Anegasaki, VII, Vasil.ev, Udinov, VMedia (USSR). No. 3453497/23-04; claimed 21.06.82 published 15.05.85, bull. No. 18). A solution of piperazine hydrochloride was placed in the cathode chamber of the electrolytic cell, separated by anion-exchange membrane in the middle chamber of the electrolyzer, limited on the one side of the cation exchange membrane, and on the other hand anion-exchange membrane, pour a weak solution of hydrochloric acid in the anode chamber is poured a solution of sulfuric acid. This streamlined process allows you to remove hydrochloric acid from a solution of amanohashidate and to concentrate it in the middle chamber of the electrolyzer. However, this does not exclude the processing solution amanohashidate alkali, since complete removal of hydrochloric acid from amanohashidate is associated with significant energy consumption.

The main disadvantage of the prototype is the impossibility of complete removal of hydrochloric acid from halogenerator piperazine. Uncovered hydrochloric acid is eutrality alkali, resulting in the formation of waste water containing salt mixed with amines.

The present invention solves the technical problem is to simplify the process of separating the amine from the aqueous solution of amanohashidate formed during the interaction of 1,2-dichloroethane with ammonia and reduce the amount of wastewater by excluding from the operation of the processing solution amanohashidate alkali.

This object is achieved in that in the method of selection amine by treatment of an aqueous solution of its amanohashidate in membrane electrolyzer according to the invention the electrochemical processing amanohashidate carried out in the four-chamber electrolysis cell with ion exchange membranes, for which the solution of amanohashidate to extract from him amine and hydrochloric acid are placed in neighboring cathode chamber of the electrolytic cell, while the cathode and anode chambers separated by cation exchange membranes, and between the second and third chambers of the electrolyzer is placed anion-exchange membrane, Amin concentrated in the cathode chamber, and hydrochloric acid in a cell of the cell adjacent to the anode.

The drawing shows a General view of the cell.

The allocation method Ethylenediamine as follows. In the cathode chamber (camera 1) cell is placed distilled water or a weak solution of (p is imushestvenno 1%) Ethylenediamine. The latter is used to create in a cathode chamber of the initial conductivity. In the camera of the cell adjacent to the cathode (camera 2), was placed a solution of amanohashidate. In the camera of the cell adjacent to the anode (camera 3), placed in a weak solution of (mostly 0.1 N.) hydrochloric acid. In the anode chamber (camera 4) cell placed a weak solution of (mostly 0.1 N.) of sulfuric acid. The cathode and anode chambers separated by cation exchange membranes (C), and between 2 and 3 cameras cell is placed anion-exchange membrane (A). In the electric field generated in the electrolytic cell when a voltage is applied to the electrodes is transferred amine ions from the chamber 2 through the cation exchange membrane into the cathode chamber of the electrolytic cell, and chloride ions through the anion exchange membrane into the chamber 3 of the electrolytic cell. Further movement of chloride ions to the anode prevents cation-exchange membrane separating the chamber 3 and the anode chamber of the electrolyzer. On the electrodes of the decomposition of water. At the cathode, this process proceeds with the release of gaseous hydrogen and the formation of ions of HE-

2H2O+2E→H2+2HE-,

and at the anode, water is decomposed to gaseous oxygen and the formation of ions H+

2H2O-2E→O2+4H+.

Ion hydrogen migrates to the 3 chamber of the electrolyzer is via cation exchange membrane and locked therein anion exchange membrane. Thus, from the camera 2 are retrieved and amine and hydrochloric acid. Amin is concentrated in the cathode chamber, and hydrochloric acid in 3 chamber pot.

Electrochemical treatment is carried out at current density of 100 to 500 a/m2.

Example 1

Investigated the extraction of Ethylenediamine and hydrochloric acid from an aqueous solution of amanohashidate Ethylenediamine in the cell, shown in the drawing, which is a cation-exchange membrane brand MK-40, A - anion-exchange membrane brand MA-40 with a working area of each 14,1 cm2.

An aqueous solution of amanohashidate Ethylenediamine used in all experiments consisted of 58.6 g/l Ethylenediamine and 70.4 g/l of hydrochloric acid. Before the beginning of the experiment in the cathode chamber of the electrolytic cell was filled with distilled water, and the anode of 0.1 n sulfuric acid solution. In the middle of the chamber was filled with a 13% solution of amanohashidate of ethylene diamine and 0.1 n hydrochloric acid (see drawing). The volume of solution, pour into each chamber was 60 ml

The amount of electricity passing through the apparatus, in all the experiments was equal to 1 And·including the Process of electrolysis was carried out at currents in the cell, varying from 100 mA to 700 mA, which corresponded to the membrane current density 71 a/m2÷ 496 a/m2. To experience hydrochloric acid was present only in 2 and 3 cameras, e is ctrainer. Moreover, in the chamber 2 was 4,284 g, and in-camera 3 - 0,219 g of hydrochloric acid. The Ethylenediamine was only in the 2nd chamber of the apparatus in the amount of 3,516,

The distribution of Ethylenediamine and hydrochloric acid to cells of the cell after passing through the 1 a·h of electricity are presented in table 1.

Table 1
The distribution of Ethylenediamine and hydrochloric acid to cells of the cell
Raft-
of
current
A/m2
Weight ED in cameras, gMass of Hcl in cameras, gThe current output, %
1223the Ethylenediaminehydrochloric acid
710,8922,2482,9161,40979,7of 87.3
1420,8882,2122,959 1,43179,389,0
2130,9362,2322,9081,39983,686,6

Continuation of table 1
The current density, a/m2Weight ED in cameras, gMass of Hcl in cameras, gThe current output, %
1223the Ethylenediaminehydrochloric acid
2840,9162,1962,929at 1,38481,885,5
3530,9442,2562,9731,41684,387,9
426 0,8942,2232,908at 1,38479,985,5
4960,8912,1982,9221,38379,685,5

In the electrolysis process is the extraction of Ethylenediamine solution amanohashidate placed in the 2nd chamber, and its concentration in the cathode chamber of the apparatus. The presence of ethylene diamine in 3 and 4 chambers of the electrolyzer was not detected. While hydrochloric acid contained in amanohashidate, concentrated in 3 of the camera. Presence of hydrochloric acid in the 1 and 4 chambers of the apparatus is not detected. This indicates that the penetration of ions Ethylenediamine through the membrane MA-40 and chloride ions through the membrane MK-40 does not occur. The material balance for Ethylenediamine (about 10%) compared with less accuracy than for hydrochloric acid (about 5%). According to the results of a series of experiments was calculated current output for hydrochloric acid and Ethylenediamine. The magnitude of the current output to Ethylenediamine (about 82%) is slightly lower than for hydrochloric acid (about 87%). A clear dependence of the current output from the membrane current density is not detected. The following is the duty to regulate to note, what if you increase the current load of the cell more than 500 a/m2, there is a strong heating of the fluids in the chambers of the device.

Example 2

To determine the maximum concentration of ethylene diamine and hydrochloric acid solutions formed in the cathode and the 3 chambers of the electrolyzer, delivered a series of experiments in which 2 camera cell circulated solution amanohashidate, and in the anode chamber was circulated solution of sulfuric acid. The solutions of ethylene diamine and hydrochloric acid formed in the cathode and the 3 chambers of the electrolyzer, the accumulation flowed by gravity from the respective chambers of the apparatus. The volumes of solutions amanohashidate and sulfuric acid circulating through 2 and the anode chamber of the electrolytic cell was 500 ml each. The working surface of each membrane was equal to 30 cm2. The concentration of the solutions used in the experiment were the same as in example 1.

The maximum content of ethylene diamine and hydrochloric acid in the solutions generated in the cathode and the 3 chambers of the apparatus, shown in table 2.

Table 2
The maximum content of ethylene diamine and hydrochloric acid in the cells concentration unit
The current density, a/m2200300400500
The concentration of Ethylenediamine, g/l192213231245
The concentration of hydrochloric acid, g/l7386,295,1101,2

The presence of hydrochloric acid Ethylenediamine produced in the cathode chamber, and Ethylenediamine in hydrochloric acid obtained in 3 chamber of the cell was not detected.

The absence in the solution of Ethylenediamine hydrochloric acid without the necessity of handling lye. The content of ethylene diamine in solution, concentrate in the cathode chamber of the electrolytic cell, almost 4 times as much of its content in the solution amanohashidate that will significantly reduce energy consumption for the evaporation process Amin.

Formed in 3 the chamber of the electrolyzer hydrochloric acid does not contain in its composition amines and can be used both in production processes and for the neutralization of alkaline wastewater.

The use of the proposed allocation method amines from clorhidrato, abrazos is, for example by transferring them in their production process, compared to the existing has the following advantages:

a) is excluded from the process of obtaining the amine process amanohashidate alkali, which greatly reduces the amount of wastewater production;

b) increasing the concentration of amine in the electrochemical processing solution amanohashidate almost 4 times compared to the concentration of amine in the solution of amanohashidate will significantly reduce the energy consumption of the process residue amine;

in) formed during the electrochemical processing solution amanohashidate hydrochloric acid can be used both in production processes and for the neutralization of alkaline wastewater.

1. The allocation method Amina, including the treatment of an aqueous solution of its amanohashidate in membrane electrolysis cell, wherein the electrochemical processing amanohashidate carried out in the four-chamber electrolytic cell, and the solution amanohashidate to extract from him amine and hydrochloric acid are placed in neighboring cathode chamber of the electrolytic cell, while the cathode and anode chambers separated by cation exchange membranes, and between the second and third chambers of the electrolyzer is placed anion-exchange membrane, Amin concentrated in the cathode chamber, and hydrochloric acid in a cell of the cell adjacent to anon the th.

2. The method of selection amine according to claim 1, characterized in that the electrochemical processing amanohashidate is carried out at a current density of 100 to 500 a/m2.



 

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