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

An oxalic acid diester, chemical reaction technology, applied in the preparation of carboxylate/lactone, inorganic chemistry, phosphorus compounds, etc., can solve the problems of lead-containing sewage and sodium sulfate solution utilization and recovery difficulties, etc.

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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Sodium oxalate after dehydrogenation of sodium formate plus ethanol as a solvent is made into a solution, and 10Kg of prepared sodium oxalate solution and 0.2-10Kg of recycled ethanol are added into a glass reactor with a jacket, stirring, and condensation reflux device, and slowly put in React 9Kg of 85wt% phosphoric acid for 2 hours, then throw 3Kg of phosphorus pentoxide, react for 2 hours, stop stirring and settle for 4 hours. Then take out the middle supernatant and return to the sodium oxalate preparation solution. Then add 0.2-15Kg of ethanol and start stirring for 4 hours, stop stirring and settle for 4 hours, the supernatant is taken out by siphon and designated as solution 2#. Then add 0.2-15Kg of ethanol and start stirring for 4 hours, stop stirring and settle for 4 hours, take out the supernatant and define it as solution 3#. Repeat the above method to obtain solution 4-6#. The solid phase enters the vacuum distillation and drying equipment, and sodium pho...

Embodiment 2

[0046] 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 ethanol are added into a stainless steel reaction kettle with a jacket, stirring, and condensation reflux device, and slowly put in Pyrophosphoric acid 1250Kg was reacted for 8 hours, put into a closed vacuum drum suction filter, and the solid phase was made into a solution and entered into the next set of closed vacuum drum suction filter, so that the closed vacuum drum suction filter was carried out three times, and the solid phase entered Vacuum distillation and drying equipment, the high-temperature gas phase is condensed to obtain a liquid phase solution for reaction, and after drying, sodium phosphate is sent to downstream products. The solution obtained by suction filtration for the first time was distilled to obtain oxalic acid and diethyl oxalate, and the liquid phase obtained by repeating ...

Embodiment 3

[0050] 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 1250Kg of pyrophosphoric acid for 5 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 enter the solid phase The next set of closed vacuum drum suction filter, such as one or two times of suction filtration of the clos...

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Abstract

The invention discloses a chemical reaction system for producing oxalic acid diester and oxalic acid 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 the 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 oxalic acid is added, the reaction is carried out, and then, the solid and liquid separation is carried out, wherein the solid phase is phosphate, and the oxalic acid diester is rich in the liquid phase; and in the third reaction unit, the oxalic acid diester-rich liquid phase 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 disclosed by the invention 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 from sodium ions and with higher additional values are generated, 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/06C07C51/02C07C51/09C01B25/30C07C31/20C07C29/149C07C233/56C07C231/02
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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