Improved production process of 1,3-Dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone

A technology of dimethylpropylene urea and production process, applied in 1 field, can solve the problems of waste acid waste water pollution, formic acid corrosion and the like, and achieves the advantages of solving the corrosion problem, advanced production technology and process, and solving the problem of production cost and environmental pollution. Effect

Inactive Publication Date: 2009-10-14
SHANXI HOOKIN PHARMA & CHEM
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Problems solved by technology

[0003] The present invention provides an improved 1,3-dimethylpropylene urea production process in order to solve the deficiencies in the above-mentioned background technology, which complet

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  • Improved production process of 1,3-Dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone
  • Improved production process of 1,3-Dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone

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Embodiment Construction

[0011] see figure 1 , in a 500L high-pressure reactor, add 62KG of urea (or 88kg of CO2), 60kg of deionized water, and 74KG of propylenediamine. After feeding, close the valve and replace it with nitrogen several times, then flush nitrogen at 1.5MPa, and start slowly Slowly raise the temperature to 250°C, keep the pressure of the reactor at 6MPa, react for 6 hours, cool down and release the pressure, recover the gas to obtain a solid pyrimidone, recrystallize with deionized water to obtain a pyrimidone intermediate with a content greater than 98%, and prepare for the following use in one step.

[0012] In a 2000L autoclave, add 200KG of the intermediate pyrimidinone produced in the front, 1kg of acidic Pd / C catalyst (catalyst formula 1Fe2O3.2Cr2O3.SO4+3Pd / Al2O3), 1500kg of 45% formaldehyde solution, and add the material , close the valve of the autoclave, replace with nitrogen several times, then pass in hydrogen, keep the temperature at 200 ° C, the pressure at 6 MPa, and th...

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Abstract

The invention relates to an improved production process of 1, 3-Dimethyl-3, 4, 5, 6-tetrahydro-2(1H)-pyrimidinone, which is improved on the basis of a prior production process of 1, 3-Dimethyl-3, 4, 5, 6-tetrahydro-2(1H)-pyrimidinone. In the invention, in a step of synthesizing pyrimidone midbody, a carbon dioxide (or urea)high-temperature and high-pressure method is adopted so as to solve the problems of production process of pyrimidone midbody, environmental pollution of organic solvent and production cost; in a step of N-methylation, formaldehyde is used as a reactant to carry out hydrogenation to finish the N-methylation under the condition of an acidic catalyst, so that the problem of corrosion of methanoic acid and the problem of pollution of waste acid and waste water in the prior art are thoroughly solved. The production process is advanced, has no pollution and accords with green high-new fine chemical engineering manufacturing technique which is emphatically supported by the nation.

Description

1. Technical field: [0001] The invention relates to a production process of dimethylpropylene urea, in particular to an improved production process of 1,3-dimethylpropylene urea. 2. Background technology: [0002] At present, there are existing methods for producing 1,3-dimethylpropylene urea in China. Generally, propylenediamine and urea are reacted under normal pressure to obtain a pyrimidinone intermediate, which is then subjected to N-methylation reaction with formaldehyde and formic acid. , obtained by two-step synthesis. There are many shortcomings in this method. First, the production of pyrimidone intermediates is unstable, the yield is not high, the loss of solvent application is large, and a large amount of organic solvents volatilize into the atmosphere to cause environmental pollution, and the production cost is high. Secondly, in N-methylation This one-step reaction, due to the use of formic acid, corrodes the equipment, and produces a large amount of low-conce...

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Application Information

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IPC IPC(8): C07D239/36
CPCY02P20/584
Inventor 牛小庆
Owner SHANXI HOOKIN PHARMA & CHEM
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