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Purification method of 6-hydroxyl-2-naphthoic acid
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A purification method, naphthoic acid technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of difficult removal and high production cost, and achieve the effect of good product quality, less loss and lower production cost
Active Publication Date: 2013-05-01
QUZHOU YINGTE HIGH MOLECULAR MATERIAL CO LTD
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[0007] The present invention provides a kind of macroporous adsorption resin adsorption, which overcomes the shortcomings of difficult removal of 2-naphthol and polymer and high production cost in the process of purifying 6-hydroxy-2-naphthoic acid in the prior art, and has low production cost and high product quality. Purification method of high-quality 6-hydroxyl-2-naphthoic acid
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Embodiment 1
[0035] A kind of purification method of 6-hydroxy-2-naphthoic acid, the method is as follows:
[0036] Put 2000kg of 6-hydroxy-2-naphthoic acid carboxylation feed solution into a 20000L neutralization tank (the carboxylation feed solution is mainly composed of 6-hydroxy-2-naphthoic acid potassium, 2-naphthol potassium and polymer, etc.) , add 5000kg of water, stir evenly, the temperature is 35°C, add 30% sulfuric acid aqueous solution, adjust the pH to 6.8-7.2, stir and cool to 25-30°C, centrifuge to remove part of 2-naphthol.
[0037] The feed liquid maintains a pH of 6.8-7.2, and enters the XDA-1 macroporous adsorption resin for adsorption. Since 2-naphthol and polymers are in a free state and are adsorbed on the resin, 6-hydroxy-2-naphthoic acid potassium is in an organic salt state and is not adsorbed.
[0038] Put the feed liquid from which 2-naphthol and polymer have been removed into a 20,000L acid analysis kettle, and add 30% sulfuric acid aqueous solution for acid an...
Embodiment 2
[0041] A kind of purification method of 6-hydroxy-2-naphthoic acid, the method is as follows:
[0042] Put 2000kg of 6-hydroxy-2-naphthoic acid carboxylation feed solution into a 20000L neutralization tank (the carboxylation feed solution is mainly composed of 6-hydroxy-2-naphthoic acid potassium, 2-naphthol potassium and polymer, etc.) , add 5000kg of water, stir evenly, the temperature is 35°C, add 30% sulfuric acid aqueous solution, adjust the pH to 6.5-6.8, stir and cool to 25-30°C, centrifuge to remove part of 2-naphthol.
[0043] The feed liquid maintains a pH of 6.5-6.8, and enters the XDA-1 macroporous adsorption resin for adsorption. Since 2-naphthol and polymers are in a free state and are adsorbed on the resin, 6-hydroxy-2-naphthoic acid potassium is in an organic salt state and is not adsorbed.
[0044] Put the feed liquid from which 2-naphthol and polymer have been removed into a 20,000L acid analysis kettle, and add 30% sulfuric acid aqueous solution for acid an...
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Abstract
The invention relates to a purification method of a fine chemical product and discloses a purification method of 6-hydroxyl-2-naphthoic acid. The method comprises the following steps: pouring 6-hydroxyl-2-naphthoic acid carboxylation feed solution in a neutralization kettle, adding water to stir evenly, keeping the temperature to 35 DEG C, adding 30% sulphuric acid solution, adjusting the pH value to 6.0-8.0, stirring and cooling to 25-30 DEG C, centrifuging to dewater and remove partial 2-naphthol; adsorbing with XDA series resin to remove 2-naphthol and polymer; pouring the obtained feed solution in an acid precipitation kettle, adding sulphuric acid solution, adjusting the pH value to 3.5-4.5 to precipitate 6-hydroxyl-2-naphthoic acid; centrifuging to dewater and obtain a 6-hydroxyl-2-naphthoic acid coarse product; and pouring the coarse product in a decoloring kettle, adding 6-8 times of refining medium while adding a defined amount of activated carbon, heating to dissolve the coarse product, refluxing and stirring for 60 minutes, filtering, cooling to crystallize, and centrifuging to dewater and obtain a 6-hydroxyl-2-naphthoic acid refined product. The method has low production cost and high product quality.
Description
Technical field [0001] The present invention involves the purification method of fine chemical products, and especially involves a purification method of 6-hydroxy-2-pyrine. Background technique [0002] 6-Hydroxy-2-Naphthoic Acid (6-Hydroxy-2-Naphthoic Acid) is an important organic intermediate of engineering plastics and medicine, especially for monomers for special temperature-resistant synthetic materials.It can also be used as an intermediate of plastic and polyester fibers, and uses 2,6 acid as the main raw material to create the world's highest -end high -temperature polymer material. [0003] Before the present invention is made, the purification of public technology purification 6-hydroxyl-2 pyrine is mainly the following method: [0004] The patent applied for the "6-hydroxyl-2-cylindrite crystal and its preparation method" in China in 2000 in 2000; the application (patent) number is 00802360.3; the public date is February 2002On the 13th, the open number was CN 1335832...
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Application Information
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Patent Type & Authority Patents(China)
IPC IPC(8): C07C65/11C07C51/43C07C51/47
Inventor 冯永胜郭小忠郭水林王炜斌叶新华毛红梅杨双土邱志国
Owner QUZHOU YINGTE HIGH MOLECULAR MATERIAL CO LTD