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Method for preparing acetylpropionic acid by using magnetic solid super acidic catalyst cassava starch

A solid super acid, tapioca starch technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve difficult purification, low yield of levulinic acid, and no separation of catalysts and raw materials is mentioned. specific methods, etc., to achieve the effect of significant economic benefits, low cost, and cost reduction

Active Publication Date: 2015-04-15
平南县科学技术情报研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the levulinic acid productive rate of this method is not high, is difficult to purify
In addition, the invention does not mention the specific method for separating the catalyst from the raw material

Method used

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  • Method for preparing acetylpropionic acid by using magnetic solid super acidic catalyst cassava starch

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of method utilizing magnetic solid superacid catalyzed cassava starch to prepare levulinic acid comprises the following steps:

[0032](1) Mixing: 300g tapioca starch, 700g water and 2g magnetic matrix Fe 3 o 4 Supported solid superacid SO 4 2- / ZrO 2 (FSZ) put into the preprocessor and mix evenly to form a starch slurry with a pH of 1.5 and magnetic Fe 3 o 4 The mass fraction of the loading amount is 0.9%;

[0033] (2) Hydrolysis reaction: Put the mixed starch slurry into a closed hydrolysis reactor, pass in steam, heat up to 150°C at a rate of 20°C per minute, keep warm for 100 minutes, and control the pressure at 2.0MPa;

[0034] (3) Solid-liquid separation: reduce the temperature of the hydrolysis reactor to about 50°C, discharge the hydrolyzate, and use a magnetic separator to separate the hydrolyzate mainly containing levulinic acid and formic acid from the magnetic solid acid. Strong acid is added to the preprocessor in step (1) for recycling, and t...

Embodiment 2

[0042] A kind of method utilizing magnetic solid superacid catalyzed cassava starch to prepare levulinic acid comprises the following steps:

[0043] (1) Mixing: 450g tapioca starch, 550g water and 4g magnetic matrix Fe 3 o 4 Supported solid superacid SO 4 2- / ZrO 2 (FSZ) into the preprocessor and mix evenly to form a starch slurry with a pH of 1.4 and magnetic Fe 3 o 4 The mass fraction of the loading amount is 1.0%;

[0044] (2) Hydrolysis reaction: put the mixed starch slurry into a closed hydrolysis reactor, pass in steam, heat up to 153°C at a rate of 20°C per minute, keep it warm for 80 minutes, and control the pressure at 2.2MPa;

[0045] (3) Solid-liquid separation: lower the temperature of the hydrolysis reactor to 50°C, discharge the hydrolyzate, and use a magnetic separator to separate the hydrolyzate mainly containing levulinic acid and formic acid from the magnetic solid acid, and the obtained magnetic solid superacid Adding step (1) to the preprocessor for...

Embodiment 3

[0053] A kind of method utilizing magnetic solid superacid catalyzed cassava starch to prepare levulinic acid comprises the following steps:

[0054] (1) Slurry mixing: mix 250g tapioca starch, 750g water and 1.5g magnetic matrix Fe 3 o 4 Supported solid superacid SO 4 2- / ZrO 2 (FSZ) put into the preprocessor and mix evenly to form a starch slurry with pH 1.3 and magnetic Fe 3 o 4 The mass fraction of the loading amount is 1.2%;

[0055] (2) Hydrolysis reaction: Put the mixed starch slurry into a closed hydrolysis reactor, pass in steam, heat up to 155°C at a rate of 20°C per minute, keep warm for 70 minutes, and control the pressure at 2.5MPa;

[0056] (3) Solid-liquid separation: lower the temperature of the hydrolysis reactor to 50°C, discharge the hydrolyzate, and use a magnetic separator to separate the hydrolyzate mainly containing levulinic acid and formic acid from the magnetic solid acid, and the obtained magnetic solid superacid Adding step (1) to the preproc...

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Abstract

The invention discloses a method for preparing acetylpropionic acid by using magnetic solid super acidic catalyst cassava starch, which comprises the following steps: 1)slurry mixing: placing cassava starch, water and the magnetic solid super acid in a preprocessor for uniformly mixing to form a starch slurry; 2)hydrolysis reaction: placing uniformly mixed starch slurry in a sealed hydrolysis reactor, heating to the temperature of 150-155 DEG C and reacting for 70min-100min, and keeping the pressure at 2.0MPa-2.5MPa; and 3)performing solid-liquid separation on the obtained reaction product, neutralizing to the pH value of 2.5-3.0, performing press filtration and ion exchange, and eluting and distilling to obtain the finished product acetylpropionic acid. According to the invention, cassava starch is taken as the raw material, the magnetic solid super acid which is capable of easily separating, circularly using and recovering can be selected, the yield of the product acetylpropionic acid is high, the purification is easy, the process is simple, the energy can be saved, the cost is low, the method provided by the invention is friendly to environment, and accords with circular economy requirement.

Description

technical field [0001] The invention belongs to the field of preparing levulinic acid from starch, in particular to a method for preparing levulinic acid from cassava starch catalyzed by a magnetic solid superacid. Background technique [0002] Levulinic acid, alias L-tranic acid, molecular formula CH 3 COCH 2 CH 2 COOH, molecular weight 116.12. Levulinic acid has good reactivity. It can undergo chemical reactions such as salt formation, esterification, hydrogenation, oxidation, and condensation to produce a variety of products with different functions, including bulk chemicals, fuels, new materials, resins, medicines, Pesticides, spices, solvents, paints and inks, rubber and plastic additives, lubricating oil additives, surfactants, etc. The raw material for producing levulinic acid can be furfuryl alcohol, or 5-carbon sugar mainly composed of xylose and hemicellulose, cellulose and starch mainly composed of glucose (cassava, sweet potato, potato and other root starches...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/185C07C51/00
Inventor 王建平陈克强章朝晖蔡小刚王仕宁
Owner 平南县科学技术情报研究所