The method of obtaining sodium caprolactamate

 

(57) Abstract:

Usage: caprolactamate sodium catalysts for anionic polymerization of lactams. The inventive caprolactamate sodium is obtained by metallation of the hydride of sodium caprolactam in the environment aprotic solvent at 20-80 °C and stirring for 2-5 h, using a mixed hydride of aluminium and sodium, selected from the group NaHAlH3, NaH(AlH3)2: (NaH)3AlH3. The product is separated, evaporated, and dried in vacuum. table 2.

The invention relates to methods for caprolactamate sodium, used as catalyst for the anionic polymerization of lactams, for receiving polycaproamide and its copolymers.

The known method (1) obtain caprolactamate sodium interaction of metallic sodium with caprolactamate at 100-120aboutWITH

Na+CLN __ NaK+0,5 H2where KL=H=0 . This method in its apparent simplicity has several disadvantages. In addition to the fire hazard of released hydrogen is partially restores the lactam to cyclohexylamine, cyclohexanol and other compounds, which generally reduce the catalytic activity caprolactamate sodium. The consequence of this is nanoproizvodstvu essence and the achieved result to the invention is a method of obtaining a (2) caprolactamate sodium interaction hydride sodium caprolactam from the reaction in organic solvents

NaH+H=0 __ NA=0+H

However, this method is not without disadvantages.

Sodium hydride obtained in the USSR, the purity does not exceed 90%. A significant portion of the impurities are alkyl derivatives of sodium, which are the initiators of the occurrence of adverse reactions, with the formation of different products recovery and condensation, which reduces the catalytic activity caprolactamate sodium.

The aim of the invention is a method for caprolactamate sodium.

This objective is achieved in that for obtaining caprolactamate sodium use mixed sodium hydride and aluminum selected from the group NaHAlH3, NaH (AlH3)2or (NaH)3AlH3and as the solvent used diethyl ether.

Source hydrides NaHAlH3, NaH (AlH3or (NaH)3AlH3get a known method (3).

Chemical analysis of the obtained mixed hydrides are presented below.

Found,%: Na 42,3; Al 49,5; H 7,25.

NaH AlH3< / BR>
Calculated,%: Na 42,5; Al 50; H 7,4.

Found,%: Na 27,5; Al To 70.9; H 7,3.

NaH (AlH3)2< / BR>
Calculated,%: Na 27,3; Al 71,4; H 7,2.

Found,%: Na 70,72; Al 25,9; H 5,85.

(NaH)3AlH3< / BR>
isout to get caprolactamate sodium.

Their interaction with the caprolactam is carried out in an environment of diethyl ether at room temperature and stirring for reaction at a ratio of reagents:

NAHAlH3+=0=1:1

NAH(AlH3)2+=0=1:1

(NAH)3AlH3+N=0=1:3 for 2-5 h, clarified water is separated from the precipitate evaporated at T-200aboutWith/HAC.

The process is reflected by the equations

NAHAlH3+O __ NAO+AlH3+H2(1)

NAH(AlH3)2+O __ NAO+2AlH3+H2(2)

(NAH)3AlH3+O __ NAN-(CH2)5-CO+AlH3+3H2(3)

For example, in the synthesis according to equation (1)

to a suspension of 2 g (0,0037 mol) NaH AlH3in Et2O dispense 100 ml Et2O containing 4,2 g (0,037 mol-caprolactam).

The reaction mixture is filtered off from NaHAlH3and evaporated in vacuum at 20aboutC. Received 49 g (98%) caprolactamate sodium representing a white crystalline substance, deliquescent in the open air, therefore synthesized caprolactamate sodium is stored in closed vials in an argon atmosphere.

Found,%: From 52.5; H 7,3; N 10,2; Na 16,5.

NAO

Calculated,%: From 52.9; H 7,4; N 10,3; Na 16,9.

In table. 1 and 2 shows the results of synthesis caprolactamate sodium and it is,5%. The process is simple in execution and to use the available synthesis of source materials, to improve the quality caprolactamate sodium, i.e., its catalytic activity.

One of the major advantages of the proposed method is to obtain as a by-product of aluminum hydride, which neutralizes the negative effect of H2to get caprolactamate sodium, expressed in recovery caprolactamate sodium, which leads to a decrease in its catalytic activity. In addition, the aluminum hydride is used as a reagent to obtain the source of hydrogen compounds of aluminum and sodium.

Another advantage of this technique compared with the prototype and the analogue is that the production caprolactamate sodium on the proposed method makes it possible to ensure the following requirements are met:

to get the most pure and highly efficient catalyst for polymerization lactamases;

to increase the level of waste products due to the minimum defective parties polycaproamide, as a result of increased purity caprolactamate sodium, used as a catalyst for the anionic polymerization in its production - 80oWith mixing in the environment aprotic solvent for 2-5 hours, separating the clarified solution with subsequent evaporation and drying in vacuum, characterized in that the metal hydride used mixed sodium hydride and aluminum selected from the group NaH AlH3, NaH (AlH3or (NaH)3AlH3and as the solvent used diethyl ether.

 

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