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A kind of preparation method of refined oxalic acid

A technology for refining oxalic acid and oxalic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of unstable product quality of oxalic acid, poor product quality stability, high consumption and production costs, and achieve a good on-site operating environment, The effect of stable quality and lower production cost

Active Publication Date: 2016-05-25
SHANDONG FENGYUAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the quality of oxalic acid products is unstable, various consumption and production costs are high, and the operating site environment is poor. In addition, in the prior art, the crystallization process of refined oxalic acid generally adopts intermittent crystallization, and the number of intermittent crystallization equipment is large and occupies an area. Large area consumes more resources, then the production capacity is small, and the product quality stability is poor

Method used

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  • A kind of preparation method of refined oxalic acid

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Embodiment 1

[0024] A kind of preparation method of embodiment 1 refined oxalic acid, comprises the following steps:

[0025] (1) Dissolve the raw material oxalic acid in the sulfuric acid mother liquor at 36-38°Bé in the reaction kettle, and after fully dissolving, the oxalic acid mother liquor is obtained, and the temperature in the reaction kettle is 56-58°C;

[0026] (2) The oxalic acid mother liquor is continuously crystallized in the cooling crystallization device, so that the oxalic acid crystallizes into oxalic acid particles, and the temperature in the cooling crystallization device is 25°C;

[0027] (3) Centrifuge the material in the cooling crystallization device to obtain oxalic acid particles and waste liquid;

[0028] (4) Dry the oxalic acid particles at 65-70°C to obtain oxalic acid with a purity of 99.6%.

Embodiment 2

[0030] On the basis of Example 1, such as figure 1 As shown, the cooling crystallization device includes a crystallizer 7, and the crystallizer 7 is provided with a crystallizer material inlet 8 and a crystallizer material outlet 9, and the crystallizer material inlet 8 is connected with a precooler 1 and a crystallizer material outlet 9 is connected with a centrifuge 21, and the crystallizer 7 is also provided with a crystallizer interlayer 10 and an overflow port 13, and the crystallizer interlayer 10 is provided with a crystallizer cold water inlet 11 and a crystallizer cold water outlet 12, and the overflow The flow port 13 is connected with the material inlet 8 of the crystallizer through a circulation pump 14 and a pipeline.

[0031] The crystallizer 7 is connected with a heating and flushing device, and the heating and flushing device includes a heat supply box 15, and the heat supply box 15 is connected with the material inlet 8 of the crystallizer through a pipeline. ...

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Abstract

The invention relates to a preparation method of refined oxalic acid. The preparation method comprises steps as follows: (1), a raw material, namely, oxalic acid is dissolved in a sulfuric acid mother solution with Baume degree of 36-38 in a reaction kettle, an oxalic acid mother solution is obtained after sufficient dissolving, and the temperature in the reaction kettle is 56-58 DEG C; (2), the oxalic acid mother solution is fed into a cooling crystallization device for continuous crystallization, oxalic acid is crystallized to form oxalic acid particles, and the temperature in the cooling crystallization device is 20-28 DEG C; (3), substances in the cooling crystallization device are subjected to centrifugal separation, and oxalic acid particles and a waste liquid are obtained; and (4), the oxalic acid particles are dried at the temperature of 65-70 DEG C, and the oxalic acid with purity of 99.6% is obtained. In the preparation method, the oxalic acid is sufficiently dissolved, and due to the appropriate dissolving temperature, odor polluting the environment cannot be produced through decomposition of the oxalic acid.

Description

technical field [0001] The invention relates to a method for preparing refined oxalic acid, in particular to a method for purifying industrial oxalic acid, belonging to the field of oxalic acid production. Background technique [0002] The world's oxalic acid production is mainly concentrated in Asia, 33% is used in the pharmaceutical industry; 25% is used in the rare earth industry; 35% is used in the metal processing and aluminum industry; the remaining 7% is used in oxalate esters, dye intermediates and other industries. With the expansion of the application field of oxalic acid, especially the increase in the number of oxalate esters used in pesticides and pharmaceutical intermediates, and the development of new techniques for producing vanillin with glyoxylic acid, the demand for oxalic acid will continue to grow steadily. [0003] Refined oxalic acid is produced by recrystallization and purification on the basis of industrial oxalic acid. With the increase of demand fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/43C07C55/06
CPCC07C51/42C07C51/43C07C55/06
Inventor 赵光辉李桂臣贾继友
Owner SHANDONG FENGYUAN CHEM CO LTD