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Method and apparatus for crystallization

一种结晶、晶体的技术，应用在结晶分离、溶液结晶、分离方法等方向，能够解决过滤操作耗费时间等问题

Inactive Publication Date: 2006-02-08
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] As a result, the existing neutralization crystallization method can only obtain crystals with a small average particle size and bulk density, so there are problems, for example, when the crystals obtained by crystallization are taken out by filtration, the filtration operation takes time. Wait

Method used

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  • Method and apparatus for crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0162] Add 12.02 grams of salicylic acid, 15.17 grams of 8 mol / liter (20°C) sodium hydroxide aqueous solution and 499.87 grams of water, salicylic acid is completely dissolved and made raw material organic acid salt solution (reaction stock solution).

[0163] Next, set the stirring speed of the above-mentioned three swept wings to 370rpm, and use a quantitative pump at an internal temperature of 30°C to add 19.14 grams of 6 mol / liter dropwise to the surface of the solution in the above-mentioned detachable flask in 29 minutes (20°C) hydrochloric acid. At 7 minutes after the start of hydrochloric acid dropwise addition, sharp precipitation of crystals was observed with the naked eye.

[0164] Next, after adding 11.02 g of 8 mol / liter sodium hydroxide aqueous solution (20° C.) to the surface of the solution in the above-mentioned detachable flask over 8 minutes, the solution surface in the above-mentioned detachable flask was dripped with a quantitative pump for 20 minutes. A...

Embodiment 2

[0171] In a 500 ml removable flask (reaction vessel) equipped with three swept wings (stirrer) with a radius of 23 mm, add 14.62 g of adipic acid, 17.53 g of 8 mol / L (20° C.) sodium hydroxide solution and 199.01 grams of water made the raw material organic acid salt solution (reaction stock solution) after adipic acid was completely dissolved.

[0172] Next, set the stirring speed of the above-mentioned three swept wings at 171rpm, and use a dropping funnel (dropper) at an internal temperature of 30°C to drop 40.26 grams of 6 to the lower part of the above-mentioned removable flask in 40 minutes. mol / L (20°C) hydrochloric acid.

[0173] At the 16th minute after the addition of hydrochloric acid, dropwise add 15.95 g of 8 mol / L (20° C.) sodium hydroxide using a dropping funnel to the liquid level of the reaction solution in the above-mentioned detachable flask simultaneously with the addition of the above-mentioned acid. The aqueous solution was used for 24 minutes for the dro...

Embodiment 3

[0182] In a 1000 ml removable flask (first reaction vessel) equipped with three swept wings (stirrer) with a radius of 30 mm, add 50.13 g of biotin, 35.88 g of 8 mol / L (20°C) sodium hydroxide Aqueous solution and 600.1 gram of water, after making biotin dissolve completely, serve as raw material organic acid salt solution (reaction stock solution). The stirring revolutions of the above three swept wings were set at 300 rpm. And in the 500 milliliters of detachable flasks (the second reaction vessel) that are equipped with the swept wing (stirrer) of three radiuses 23 millimeters, add 100.22 grams of water, the stirring revolution number of above-mentioned three swept wings is set at 350rpm. An immersion tube was installed in the first reaction vessel, and the contents (reaction liquid) in the first reaction vessel were pumped at a rate of 32.8 ml / min onto the liquid surface of the contents in the second reaction vessel. Simultaneously above-mentioned second reaction vessel i...

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Abstract

The present invention is a method which is capable of producing crystals having a mean particle diameter larger than conventionally produced crystals, by carrying out a crystallizing method so-called neutralization crystallization. An ingredient organic acid salt solution is supplied as a reaction initial liquid in a reaction vessel ( 2 ). An acid is supplied via a dropping tube ( 10 ) to the ingredient organic acid salt solution, so that crystals of a targeted organic acid is precipitated. Then, the base is supplied in the reaction vessel ( 2 ) via a dropping tube ( 15 ), thereby partially dissolving the crystals being precipitated. The acid is further supplied from the dropping tube ( 10 ) for carrying out the crystallization.

Description

technical field [0001] The present invention relates to a crystallization method of an organic acid comprising adding an acid to an organic acid salt solution to crystallize the organic acid, and a crystallization device suitable for the method. Background technique [0002] Crystallization of poorly water-soluble or insoluble organic acids such as carboxylic acids is generally carried out by a reaction crystallization method called neutralization crystallization in which salts are crystallized by reacting with acids in the presence of water. [0003] This so-called neutralization crystallization method, for example, is known to add an acid to an aqueous solution of a water-soluble salt of a crystalline organic acid such as adipic acid and nicotinic acid to produce the organic acid crystal (for example, refer to Document 1: Wang Fang 2 "Monitoring pH Swing Crystallization of Notice Acid by the Use of Attennuated Total Reflection Fourier Transform Infrared Spectrometry", Ind....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/02B01D9/00
CPCB01D9/005B01D9/02C07B63/00C07C51/43
Inventor 铃木信二大久保尚人
Owner SUMITOMO CHEM CO LTD
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