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Process method of co-production of oxamide and carbamic acid ester through ammonia ester exchange method

The technology of carbamate and process method is applied in the field of co-production of oxamide and carbamate by transesterification method, which can solve the problems of by-products affecting the reaction process and single product, and avoid the increase of process and equipment costs. , the effect of uninhibited conversion, avoiding process and equipment costs

Active Publication Date: 2016-03-02
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process aims to solve the problems of single product and by-products affecting the reaction process in the synthesis of oxamide by aminolysis of oxalic acid diester and the synthesis of carbamate by alcoholysis of urea.

Method used

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  • Process method of co-production of oxamide and carbamic acid ester through ammonia ester exchange method
  • Process method of co-production of oxamide and carbamic acid ester through ammonia ester exchange method
  • Process method of co-production of oxamide and carbamic acid ester through ammonia ester exchange method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 10g of dimethyl oxalate, 10g of urea and 10g of methanol and fill them into a 100ml reaction vessel that is airtight and pressure-resistant and equipped with a heating and stirring device, and feed N into the reactor. 2 Replace the air in the kettle for 3 consecutive replacements, and finally feed in N 2 Pressurize to 0.5MPa, set the temperature at 70°C, stir and heat to dissolve the raw materials completely and mix them evenly. The reaction temperature was set at 150° C., the stirring speed was set at 100 rpm, and the reaction was continued for 12 hours until the temperature in the reaction kettle dropped to room temperature. Open the tail gas venting needle valve to reduce the pressure in the reactor to 0.1 MPa. Open the reaction kettle, take out the reacted mixture, and place it in a flask of a rotary evaporator. Set the vacuum degree to 3mmHg, the temperature to 80°C, and the rotation speed to 100rpm. Distill under reduced pressure for 5 hours to collect 8.5...

Embodiment 2

[0037] Same as the embodiment of Example 1, the difference is that the reaction pressure is 0.7 MPa, and the amount of methanol added is 20 g. Product analysis results are shown in Table 1

Embodiment 3

[0039] Same as the embodiment of Example 1, the difference is that the reaction pressure is 0.7 MPa, and the amount of methanol added is 30 g. Product analysis results are shown in Table 1

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Abstract

The invention discloses a process method of co-production of oxamide and carbamic acid ester through an ammonia ester exchange method. According to the process method, urea and oxalic acid diethyl serve as raw materials, and two products, namely the oxamide and the carbamic acid ester, can be obtained at the same time through a series of ammonia ester exchange reactions. By means of the process, the problems that products are singular, and by-products affect the reaction process in an original technology for synthesizing oxamide through oxalic acid diethyl ammonolysis and a technology for synthesizing carbamic acid ester through urea alcoholysis are solved; besides, due to the fact that urea is obtained through CO<2> and NH<3> synthesis, NH<3> is replaced with urea, and the process method has active significance in converting CO<2> into high added-value chemicals and efficiently utilizing CO<2>.

Description

technical field [0001] The invention belongs to the technical field of oxamide synthesis technology and carbamate synthesis technology, and relates to a process for co-producing oxamide and carbamate by transesterification method in which oxalic acid diester and urea participate together. Background technique [0002] Oxamide is a urea-formaldehyde slow-release fertilizer, non-toxic and easy to store, with a nitrogen content of 31.8% and a solubility in water of 0.016%. It gradually decomposes and releases ammoniacal nitrogen and carbon dioxide during the biodegradation process. Oxamide is not easy to leaching, which not only improves the utilization rate of chemical fertilizers, reduces the frequency of fertilization, but also avoids the pollution of water resources. Its gradual and slow-release characteristics are in line with the growth law of crops. One-time large-scale application will not burn crops or cause abnormal growth of crops due to excessive absorption, and mee...

Claims

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Application Information

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IPC IPC(8): C07C233/56C07C231/10C07C271/12C07C269/00
Inventor 姚元根乔路阳周张锋
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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