Method for synthesizing dialkyl carbonate from biomass-based furfural

A technology of dialkyl carbonate and biomass, which is applied in the field of preparation of dialkyl carbonate, can solve the problems of high corrosiveness of catalyst equipment, easy deactivation of catalyst, and high operational safety requirements, and achieves significant economic and social benefits, and the synthesis method Scientific environmental protection, the effect of reducing environmental pollution

Inactive Publication Date: 2019-02-12
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The traditional industrial production of dimethyl carbonate generally adopts the phosgene synthesis method, but the synthesis can only maintain small-scale industrial production, and these preparation methods require phosgene, high operational safety requirements, and serious environmental pollution, so they are gradually replaced by the methanol oxidative carbonylation method replaced by
However, the methanol oxidative carbonylation method is divided into a liquid phase method and a gas phase method: in the reaction process of the liquid phase method, methanol is both a raw material and a solvent, and the oxygen concentration is always kept below the explosive limit in the reaction process. The catalyst is highly corrosive to the equipment, the methanol circulation in the system is large, and the catalyst is easily deactivated. The gas phase method requires a fixed bed reactor, and the disadvantage is that the catalyst activity is low
Imre Weisz once proposed to synthesize dimethyl carbonate by reacting dimethyl sulfate and sodium carbonate in a tank reactor, using chlorobenzene as a catalyst, and refluxing at 150-210°C for 6 hours to obtain dicarbonate with a yield of 44%. Methyl ester (Weisz I, Havelka F, Pellek Z, Dimethyl and diethylcarbonates, Hung Teljes, 1977, 14:221~226), but because the yield of this process is low, chlorobenzene and dimethyl sulfate are highly toxic, so the Law has not been further developed

Method used

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  • Method for synthesizing dialkyl carbonate from biomass-based furfural

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Experimental program
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Embodiment 1

[0013] 1) Preparation of biomass-based furfural

[0014] Crush 100g of corn cobs to about 1mm, and soak them in 4% sulfuric acid aqueous solution at 120°C for 2 hours. The liquid-solid ratio (V / W) of dilute sulfuric acid to agricultural and forestry wastes is 10:1. The yield of pentose after hydrolysis is 78.67%. Prepare the obtained pentose sugar into a 0.4mol / L solution and put it into a reaction kettle, install a condensation distillation device, control the mass fraction of sulfuric acid to about 20%, the distillation temperature is 190°C, and the distillation time is 5h to obtain a 49% furfural solution.

[0015] 2) Synthesis of maleic anhydride

[0016] The first is the heteropoly acid MoWP / SiO 2 Catalyst preparation. Synthesis of MoWP heteropoly acid: configure 1mol / L ammonium molybdate aqueous solution, then slowly drop phosphoric acid into the ammonium molybdate solution according to the ratio of molybdenum and phosphorus substances to 0.9; weigh the ratio of tungs...

Embodiment 2

[0027] 1) Preparation of biomass-based furfural

[0028] 100g of waste bamboo was crushed to about 1mm, immersed in 5% sulfuric acid aqueous solution at 110°C for 2.5h, and the liquid-solid ratio (V / W) of dilute sulfuric acid to agricultural and forestry waste was 11:1. The yield of pentose after hydrolysis is 70.67%. Prepare the obtained pentose sugar into a 0.6mol / L solution and put it into a reaction kettle, install a condensation distillation device, control the mass fraction of sulfuric acid to about 25%, the distillation temperature is 180°C, and the distillation time is 6h to obtain a 46% furfural solution.

[0029] 2) Synthesis of maleic anhydride

[0030] The first is the heteropoly acid MoWP / SiO 2 Catalyst preparation. Synthesis of MoWP heteropoly acid: configure 1mol / L ammonium molybdate aqueous solution, then slowly add phosphoric acid to the ammonium molybdate solution according to the ratio of molybdenum and phosphorus to 0.85; weigh the ratio of tungsten and ...

Embodiment 3

[0041] 1) Preparation of biomass-based furfural

[0042] Crush 100g of waste wood to about 1 mm, and soak it in 3.5% sulfuric acid aqueous solution at 130°C for 3 hours. The liquid-solid ratio (V / W) of dilute sulfuric acid to agricultural and forestry waste is 13:1. The yield of pentose after hydrolysis is 75.25%. Prepare the obtained pentose sugar into a 0.5mol / L solution and put it into a reaction kettle, install a condensation distillation device, control the mass fraction of sulfuric acid to about 30%, the distillation temperature is 200°C, and the distillation time is 5.5h to obtain a 48.2% furfural solution.

[0043] 2) Synthesis of maleic anhydride

[0044] The first is the heteropoly acid MoWP / SiO 2 Catalyst preparation. Synthesis of MoWP heteropoly acid: configure 1mol / L ammonium molybdate aqueous solution, then slowly drop phosphoric acid into the ammonium molybdate solution according to the ratio of molybdenum and phosphorus substances to 0.9; weigh the ratio of ...

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Abstract

The invention belongs to a synthesis method of an ester type compound in organic chemistry and in particular relates to a method for synthesizing dialkyl carbonate from biomass-based furfural. The method comprises the following steps: firstly, taking agricultural and forest wastes as initial raw materials, carrying out acid hydrolysis and dehydration cyclization reaction and purifying to obtain furfural; carrying out oxidization reaction on the biomass-based furfural under the action of hydrogen peroxide and a catalyst to synthesize maleic anhydride; carrying out epoxidation reaction on the synthesized maleic anhydride under the action of the catalyst and the hydrogen peroxide to synthesize epoxysuccinic acid; carrying out cycloaddition reaction on the epoxysuccinic acid and CO2 to prepareannular carbonate; finally, carrying out ester exchange reaction on the synthesized annular carbonate and monohydric alcohol or polyhydric alcohol to prepare the dialkyl carbonate. According to the method provided by the invention, the cheap agricultural and forest wastes are used as the raw materials to produce the dialkyl carbonate; meanwhile, tartaric acid with high additional value is also produced; the production cost is saved and the environment pollution is reduced; a novel way is also provided for industrial production of the dialkyl carbonate and the tartaric acid and efficient and comprehensive utilization of the agricultural and forest wastes; the synthesis method has remarkable economic benefits and social benefits.

Description

technical field [0001] The invention relates to a method for preparing dialkyl carbonate, in particular to a new method for synthesizing dialkyl carbonate from biomass-based furfural and its application. Background technique [0002] Dialkyl carbonate is a non-toxic chemical raw material, because its molecule contains -CO, -COOCH 3 and -CH 3 , has good reactivity, can react with a variety of alcohols, phenols, amines and esters, is a widely used organic compound and a good solvent, there are many types of dialkyl carbonate, such as diethyl carbonate used in chemical production As a solvent for nitrocellulose, cellulose ether, synthetic resin and natural resin; ethyl methyl carbonate is an excellent solvent for lithium-ion battery electrolyte; pentaerythritol carbonate and trimethylolpropane carbonate can be used as lubricating oil. Therefore, dialkyl carbonate has high industrial application value and good market prospect. Among them, dimethyl carbonate is the most repres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96
CPCC07C68/06C07C51/285C07C68/04C07D307/60C07C69/96C07C59/10
Inventor 李学兵王忠李青洋林冠楠
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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