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Chemical reaction system for producing oxalic acid diester as main products by using sodium formate as raw materials

An oxalic acid diester, chemical reaction technology, applied in the preparation of carboxylate, carboxylate/lactone, organic chemistry, etc., to achieve the effect of saving steam and simple process

Inactive Publication Date: 2012-09-12
天津市碳一有机合成工程设计有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a chemical reaction system with sodium formate as raw material production and oxalic acid diester as the main product, which does not affect the environment, and there is no environmental problem of lead-containing sewage and other waste discharges, Sodium ions generate sodium sulfate that is easy to recycle, the process separation becomes simple and easy, and the production process achieves clean production, energy saving and environmental protection production process

Method used

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  • Chemical reaction system for producing oxalic acid diester as main products by using sodium formate as raw materials
  • Chemical reaction system for producing oxalic acid diester as main products by using sodium formate as raw materials
  • Chemical reaction system for producing oxalic acid diester as main products by using sodium formate as raw materials

Examples

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example 1

[0039] Sodium oxalate after dehydrogenation of sodium formate plus methanol as a solvent is made into a solution, and 15-20Kg of prepared sodium oxalate solution and 2-10Kg of recycled methanol are added into a stainless steel reaction kettle with a jacket, stirring, and condensation reflux device. Slowly add 7Kg of sulfur trioxide and 4Kg of dimethyl ether to react for 6 hours, stop stirring and settling for 2 hours, take out the upper clear liquid and set it as solution 1#, then take out the middle clear liquid and return it to sodium oxalate to prepare the solution. Then add 2-15Kg methanol and start stirring for 1 hour, stop stirring and settle for 2 hours, take out the supernatant liquid and set it as solution 2#, repeat the above method to obtain solution 4-6#, separate part of oxalic acid (trace amount) and dimethyl oxalate, Oxalic acid can be used as a product. Dimethyl oxalate is developed downstream by adding water to obtain oxalic acid, hydrogenation to obtain ethyl...

example 2

[0045] Sodium oxalate solution after dehydrogenation of sodium formate and solvent is made into a solution, and 1500Kg of prepared sodium oxalate solution and 200-1000Kg of recycled methanol are added into a stainless steel reaction kettle with a jacket, stirring, and condensation reflux device, and slowly put in Dimethyl sulfate 1100Kg reacts 8 hours, puts into airtight vacuum drum suction filter, solid phase is made into solution and enters next set of airtight vacuum drum suction filter, carries out airtight vacuum drum suction filter three times like this, solid The phase enters the vacuum distillation and drying equipment, and the high-temperature gas phase is condensed to obtain a liquid phase solution for reaction, and the sodium sulfate salt is dried after drying. The supernatant of the solution obtained by suction filtration for the first time is cooled to obtain crystallization of oxalic acid and dimethyl oxalate. After the supernatant is distilled, the residual liqui...

example 3

[0049] The solution is prepared by adding sodium oxalate after dehydrogenation of sodium formate and adding a solvent. Add 1500Kg of prepared sodium oxalate solution and 200-1000Kg of recycled methanol into a stainless steel reaction kettle with a jacket, stirring and condensing reflux device, and slowly put in React 650Kg of sulfur trioxide and 370Kg of dimethyl ether for 6 hours, stop stirring and settling for 3 hours, take out the clear night of the upper layer and set it as solution 1#, then take out the clear night of the middle layer and return it to sodium oxalate to prepare the solution. Then add 200-1500Kg methanol and start stirring for 0.5 hours, stop stirring and settle for 2 hours, take out the upper layer clear night and set it as solution 2#, then add 200-1500Kg methanol and start stirring for 0.5 hours, put it into a closed vacuum drum suction filter, and mix the solid phase The solution enters the next set of closed vacuum drum suction filter, and performs one ...

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Abstract

The invention discloses a chemical reaction system for producing oxalic acid diester as main products by using sodium formate as raw materials. The chemical reaction system comprises a first reaction unit, a second reaction unit and a third reaction unit, wherein sodium formate is subjected to dehydrogenation reaction to generate sodium oxalate in the first reaction unit; in the second reaction unit, the sodium oxalate is mixed with solvents, then, the sulfuric acid is added, and the liquid and solid separation is carried out after the reaction, wherein the solid phase is sulfate, and the liquid phase contains rich oxalic acid diester; and in the third reaction unit, the liquid phase containing rich oxalic acid diester is subjected to distillation separation, then, the oxalic acid diester is respectively subjected to hydrolysis, hydrogenolysis and ammonolysis, and oxalic acid, alcohol, glycol and oxamide are obtained. The chemical reaction system has the advantages that the influence on environment is avoided, the environment problems of lead-containing sewage and other waste discharge do not exist, phosphates with higher additional value s re generated by sodium ions, the process separation becomes simple, the implementation is easy, and the production process reaches the requirements of clean production and energy saving environment-friendly type production process.

Description

technical field [0001] The invention relates to a chemical reaction system, more specifically, relates to a reaction system for further chemical production using sodium formate as a raw material. Background technique [0002] The process of synthetic oxalic acid production in my country uses lead sulfate as a precipitant to react with sodium oxalate to form lead oxalate precipitation and sodium sulfate solution. The liquid and solid are clarified and separated. Lead oxalate and sulfuric acid are added to obtain oxalic acid and lead sulfate. The liquid-solid clarification and separation of solid-phase lead sulfate is rinsed many times, and the rinse solution and lead sulfate are used in the next cycle. Among them, sodium ions are converted into sodium sulfate solution, which is difficult to use and recycle, and causes The environmental problems of lead-containing sewage are undoubtedly contrary to the current environmental protection and conservation advocated. Therefore it ...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/08C07C55/06C07C51/09C07C31/20C07C29/149C07C233/56C07C231/02
Inventor 姜红远李东平蒋子琪王德明班志忠张伯年
Owner 天津市碳一有机合成工程设计有限公司
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