Combinational preparation method of nano zinc oxide and toluene dicarbamate

A technology of methyl toluene dicarbamate and nano zinc oxide is applied in the preparation of organic compounds, chemical instruments and methods, cyanide reaction preparation, etc. The cost of the catalyst is high, the preparation process is complicated, etc., to avoid adverse effects, reduce the subsequent separation process, and simplify the operation process.

Active Publication Date: 2007-08-08
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1488623A provides the technological process of preparing toluene-2,4-dicarbamic acid methyl ester with 2,4-diaminotoluene and dimethyl carbonate reaction, provides the regeneration method of catalyzer, makes catalyzer can recycle, but catalyzer The cost of regeneration is high
In existing literatures using zinc acetate as a zinc-containing compound to prepare nano-zinc oxide, not only only a single product of nano-zinc oxide is produced, but the preparation process is complicated and the cost is high.
[0005] In summary, there is no report on the preparation method of methyl toluene dicarbamate with simple preparation process, low production cost, no environmental pollution, and simultaneous preparation of nano-zinc oxide. Introduction of other methods for two products of nano-zinc oxide and methyl toluene dicarbamate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of methyl toluene dicarbamate

[0025] Add 0.0409mol 2,6-diaminotoluene, 1.146mol dimethyl carbonate, and 0.00436mol zinc acetate to the reaction kettle in sequence, then seal the reaction kettle, and heat it to a temperature of 150°C under stirring conditions to react for 6 hours , the reaction is completed and the material is discharged, the feed liquid is filtered at 70°C, and the resulting filtrate is then heated at 30°C, 5kp a Distilled under reduced pressure under the conditions, 0.0389 mol of solid product methyl toluene-2,6-dicarbamate was obtained, and the product yield was 95.1%.

[0026] (2) Combined preparation of nano-zinc oxide

[0027] The filter cake obtained by filtering in the step (1) was washed four times with dimethyl carbonate, then washed with distilled water, filtered, and the filter cake was dried in an oven at 120° C. for 3 hours to obtain 0.00393 mol of product nano-zinc oxide. Zinc oxide was characterized by a Japanese Rigak...

Embodiment 2

[0029] (1) Preparation of methyl toluene dicarbamate

[0030] Add 0.0409mol 2,4-diaminotoluene, 1.227mol dimethyl carbonate, and 0.0286mol zinc acetate to the reaction kettle in sequence, then seal the reaction kettle, and heat it to 200°C for 1 hour under stirring conditions. , the reaction is completed and the material is discharged, the feed liquid is filtered at 60°C, and the resulting filtrate is then heated at 70°C and 30kp a Distilled under reduced pressure under the conditions, 0.0258 mol of solid product methyl toluene-2,4-dicarbamate was obtained, and the product yield was 63.1%.

[0031] (2) Combined preparation of nano-zinc oxide

[0032] The filter cake obtained by filtering in step (1) is washed four times with N,N-dimethylformamide, then washed with distilled water, filtered, and the filter cake is placed in an oven at 100°C and a vacuum of 80kp a Under the condition of vacuum drying for 3 hours, 0.00261mol of product nano-zinc oxide was obtained. Zinc oxide ...

Embodiment 3

[0034] (1) Preparation of methyl toluene dicarbamate

[0035] Add 0.0491mol 2,4-diaminotoluene, 1.424mol dimethyl carbonate, and 0.0196mol zinc acetate to the reaction kettle in sequence, then seal the reaction kettle, and heat it to a temperature of 170°C under stirring conditions to react for 4 hours , the reaction is completed and the material is discharged, the feed liquid is filtered at 75°C, and then the resulting filtrate is filtered at 45°C, 10kp a Distilled under reduced pressure under the conditions, 0.0469 mol of solid product methyl toluene-2,4-dicarbamate was obtained, and the product yield was 95.5%.

[0036] (2) Combined preparation of nano-zinc oxide

[0037] Wash the filter cake obtained by filtering in step (1) four times with methanol, then wash with distilled water, filter, and filter the cake in an oven at 60°C and a vacuum of 100kp a Under the condition of vacuum drying for 3 hours, 0.0182 mol of zinc oxide was obtained. Zinc oxide is characterized by th...

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Abstract

The invention discloses a making method of toluenediamine methyl formate of nanometer zinc oxide, which comprises the following steps: adding diaminotoluene, zinc acetate and dimethyl ester carbonate in the autoclave with molar rate at 1:0.01-0.7:15-30; sealing the autoclave; stirring; reacting under 100-200 deg.c for 1-10h; filtering; decompressing to rectify under 30-70 deg.c at 5-30Kpa; obtaining the solid product (toluenediamine methyl formate); washing filter pie; drying in the vacuum; obtaining the nanometer zinc oxide.

Description

technical field [0001] The invention belongs to the method for preparing phenylcarbamate by catalyzed reaction of dimethyl carbonate, specifically the method for preparing methyl toluene dicarbamate by catalyzed reaction of dimethyl carbonate. Background technique [0002] Methyl toluene dicarbamate is an important organic compound. It can not only be used as insecticide, bactericide, antipyretic and analgesic drugs, but also as an intermediate for the synthesis of toluene diisocyanate. Toluene diisocyanate is an important raw material for the preparation of polyurethane. [0003] In the existing literature reports on the synthesis of carbamates from amines and organic carbonates, most of them are about the catalysts and processes used in the preparation. US2003162995 discloses a method for preparing carbamate using organic or inorganic salts of metals such as Zn, Sn, Pb, and Cu as catalysts. The preparation process is given, but the used catalysts are no longer recycled. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/02C07C229/54C01G9/02
Inventor 王延吉王桂荣王淑芳赵新强
Owner HEBEI UNIV OF TECH
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