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Auxiliary, preparation method of adjuvant and recrystallization method of laurolactam

A technology of cinnamic lactam and recrystallization, which is applied in the separation/purification of lactam, chemical instruments and methods, organic chemistry, etc., can solve the problems of cumbersome operation and achieve the effects of simple process, lower interface energy and low cost

Active Publication Date: 2021-02-02
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Invention patent CN1252404A and patent CN101885705A both mentioned the preparation method of lactam substances, but there is no clear description of the phenomenon of avoiding coalescence and agglomeration in the refining and recrystallization process; Invention patent CN109867616A described a kind of laurolactam The production method uses one solvent for auxiliary extraction and liquid separation, and another solvent for crystallization, but the full dissolution of laurolactam in the first solvent requires a certain temperature and a large excess of solvent, and the reaction solution needs to be maintained at 80 Above ℃, the operation is cumbersome, and the invention patent has no clear statement on the phenomenon of ion agglomeration that is prone to occur during the crystallization process

Method used

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  • Auxiliary, preparation method of adjuvant and recrystallization method of laurolactam
  • Auxiliary, preparation method of adjuvant and recrystallization method of laurolactam
  • Auxiliary, preparation method of adjuvant and recrystallization method of laurolactam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Auxiliary agent a is synthesized (structure is as formula (I), and R 1 =-CH 2 CH 3 ):

[0044] Weigh 35g of 1,3-diiminoisoindoline into a 250mL three-necked reaction bottle, which is connected with a thermometer and a condenser respectively, add 10g of silicon tetrachloride into the system, put it into a magnet, and put it in an oil bath Heat up to 210°C for reflux reaction, use a silica gel plate to monitor the reaction, and reflux for 1 hour;

[0045] Cool to 50°C, add 3g of ethylamine to the system, stir for 10min, then add 20mL of dichloromethane, 2mL of triethylamine (the molar ratio of 1,3-diiminoisoindoline to triethylamine is about 0.05) and 9g cyclohexanoyl chloride, continue to stir and react for 30min, separate and obtain auxiliary agent a 39g, yield 95%;

[0046] Elemental analysis of additive a: C, 70.36; H, 4.72; N, 18.46; O, 2.34; Si, 4.11;

[0047] 1 H NMR (400MHz, DMSO-d 6 ):δ1.22(-CH 3 ),1.56~1.81(-CH 2 -,), 2.38(-CH), 3.24(-CH 2 -), 5.56(2H)...

Embodiment 2

[0052] The difference with Example 1 is that in the recrystallization process, the auxiliary agent used is replaced by auxiliary agent b (the difference with auxiliary agent a is that R in formula I 1 =CH 3 ), other feeding intake and experimental conditions in the recrystallization process are all consistent with embodiment 1, no particle coalescence occurs in the recrystallization process, and the yield of the recrystallization process is 93.3% after analysis, and the purity is 99.4wt%. Electron microscope pictures are attached figure 1 As shown in Figure B;

[0053] The synthesis process of auxiliary agent b is basically the same as that of auxiliary agent a in Example 1, the only difference is that ethylamine is replaced by methylamine; the structural detection information of auxiliary agent b is as follows:

[0054] Elemental analysis of the obtained additive b: C, 70.36; H, 4.72; N, 18.46; O, 2.34; Si, 4.11.

[0055] 1 H NMR (400MHz, DMSO-d 6 ): δ1.53~1.73(-CH 2 -)...

Embodiment 3

[0057] The difference from Example 1 is that during the recrystallization process, 10 g of auxiliary agent a was used, and no particle coalescence occurred during the recrystallization process. The yield of the recrystallization process was analyzed to be 87.9%, and the purity was 99.0 wt%.

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Abstract

The invention provides an auxiliary agent, a preparation method of the auxiliary agent and a recrystallization method of laurolactam. By applying the auxiliary agent of the present invention to the recrystallization process of laurolactam, the surface tension of the interface can be reduced, and the laurel lactam can be effectively reduced. Particle coalescence and agglomeration of lactam occurred during recrystallization. The auxiliary agent provided by the present invention has the following structural formula (I): wherein, R 1 is methyl, ethyl, isopropyl or n-butyl.

Description

technical field [0001] The invention relates to an auxiliary agent and a synthesis method thereof, and also relates to the application of the auxiliary agent in recrystallization, in particular to the recrystallization process of laurolactam compounds. Background technique [0002] Lauryl lactam (Lauryl lactam, pelletized), referred to as LA. LA is polymerized to obtain nylon 12. As a special nylon product, compared with general nylon (such as nylon 6), nylon 12 has the advantages of low water absorption, high toughness, wear resistance, and swelling resistance. Globally, Nylon 12 (and Nylon 11) have replaced metal materials as indispensable and hard-to-replace non-metallic materials such as automotive fuel pipes and air brake hoses. In addition, in the fields of submarine cables, solar energy, medical treatment, 3D printing, etc., nylon 12 has demonstrated superior performance advantages. In the next five years, the demand for nylon 12 will grow at a rate of 8%. From a t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22C07D225/02C07D201/16
CPCC07D201/16C07D225/02C07D487/22
Inventor 冯民昌边新建李俊平黎源
Owner WANHUA CHEM GRP CO LTD
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