Technique for co-production of dimethyl carbonate and oxamide

A technology of dimethyl carbonate and process method, which is applied in the field of organic catalytic synthesis, can solve the problems of low utilization rate of ammonia gas, increase of equipment and process cost, and decrease of reaction equilibrium constant, so as to avoid the increase of process and equipment cost and improve Atom economy, the effect of avoiding inefficiency loss

Active Publication Date: 2017-05-17
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

This is because the generation of a large amount of methanol not only dilutes the raw material, reduces the reaction rate, but also reduces the reaction equilibrium constant, making it difficult to move the equilibrium to the product direction.
In addition, a large number of effective methoxy groups can only generate methanol with low added value after being replaced by amino groups, and the atom economy of the reaction is poor; the amino groups are derived from ammonia molecules in the gas phase, which makes the reaction only possible in gas-liquid Two-phase interface, the utilization rate of ammonia gas is very low, and the ammonia gas that is too late to react cannot be discharged directly, and a special ammonia corrosion-resistant device is required for recycling, which leads to an increase in equipment and process costs

Method used

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  • Technique for co-production of dimethyl carbonate and oxamide
  • Technique for co-production of dimethyl carbonate and oxamide
  • Technique for co-production of dimethyl carbonate and oxamide

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh 11.8g of dimethyl oxalate, 6g of urea, and 6.4g of anhydrous methanol and fill them into a stirred autoclave. The molar ratio of methanol, urea, and dimethyl oxalate is 2:1:1. Then weigh 1g CuO / CaO-In 2 o 3 -CdO catalyst is loaded into the reactor, the mass ratio of catalyst and dimethyl oxalate is 8.5%, CuO accounts for 50% of the total mass of the catalyst in the catalyst, CaO accounts for 5% of the total mass of the catalyst, In2 o 3 It accounts for 40% of the total mass of the catalyst, and CdO accounts for 10% of the total mass of the catalyst. Access to N 2 After the air in the kettle was replaced, the pressure was increased to 1 MPa, the temperature was raised to 70° C. and the temperature was continuously stirred at 100 rpm for 1 hour. Then the temperature was raised to 150° C., and the reaction was continued for 5 h at a stirring speed of 100 rpm. Finally, turn off the heating. After the temperature in the reactor drops to room temperature, open the g...

Embodiment 2

[0029] With embodiment 1, difference is that reaction pressure is 3MPa. The product analysis results are shown in Table 1.

Embodiment 3

[0031] Same as Example 1, except that the reaction temperature is 180°C. The product analysis results are shown in Table 1.

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Abstract

The invention discloses a technique for co-production of dimethyl carbonate and oxamide. According to the method, urea and dimethyl oxalate are taken as raw materials, and two products of the dimethyl carbonate and oxamide are obtained by simultaneous synthesis through ester-ammonia exchange reaction under the action of a catalyst. According to the method, amino in the urea and methoxyl in the dimethyl oxalate can be efficiently recombined, so that losses of two groups in forms of ammonia gas and methanol are avoided; the problems of low raw material utilization rate and poor atom economy in a raw material conversion path in the original process of synthesizing the dimethyl carbonate through urea alcoholysis and the original process of synthesizing the oxamide through dimethyl oxalate ammonolysis are mainly solved; and meanwhile, the adverse effects of by-products of the ammonia gas generated in the urea alcoholysis process and the methanol generated in the dimethyl oxalate ammonolysis process on reaction balance are effectively eliminated.

Description

technical field [0001] The invention belongs to the technical field of organic catalytic synthesis, and relates to a process method for co-producing dimethyl carbonate and oxamide by utilizing the amino group of urea and the methoxy group of dimethyl oxalate to efficiently recombine. Background technique [0002] As an important emerging organic chemical intermediate, dimethyl carbonate has attracted the attention of many researchers in the fields of medicine, biology and energy due to its green and environmental protection characteristics. Dimethyl carbonate is mainly used to synthesize polycarbonate and other bulk chemical raw materials; it can replace highly toxic phosgene to participate in the methylation and carbonylation process of organic synthesis; as an additive, it can improve the antiknock performance of gasoline. The initial production method of dimethyl carbonate is phosgene method, but the toxicity and corrosiveness of phosgene limit the application of this met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/00C07C69/96C07C231/10C07C233/56
CPCY02P20/584C07C68/00C07C231/10C07C69/96C07C233/56
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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