Solid acid catalyst as well as preparation method thereof and preparation method of hydroxy phenylglycine

A solid acid catalyst and ammoniating agent technology, which is applied in the direction of catalyst activation/preparation, organic compound preparation, cyanide reaction preparation, etc., can solve the problems of long process route, long reaction time, cumbersome operation, etc., to reduce pollution, The effect of high reuse rate and low dosage

Active Publication Date: 2019-05-17
ZHENGZHOU UNIV
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  • Application Information

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Problems solved by technology

For example, U.S. Patent No. 4,175,206 uses glyoxylic acid, phenol and ammonium acetate as raw materials to synthesize p-hydroxyphenylglycine by a one-pot method. The reaction is carried out at 30-35°C for 48 hours, and the product yield is 50.4%. long, low yield
Jin Tongshou (Synthesis of Semi-synthetic Antibiotic Side Chain (IV) Synthesis of D/L-p-Hydroxyphenylglycine with Ammonizing Agent [J]. Journal of Hebei University (Natural Science Edition). 1998,18(3): 250-252) using sulfamic acid as the ammoniating agent of the reaction, reacting at 50°C for 2h, then reacting at 70°C for 4h, and then alkalized to obtain the crude product, and then refi

Method used

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  • Solid acid catalyst as well as preparation method thereof and preparation method of hydroxy phenylglycine
  • Solid acid catalyst as well as preparation method thereof and preparation method of hydroxy phenylglycine
  • Solid acid catalyst as well as preparation method thereof and preparation method of hydroxy phenylglycine

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preparation example Construction

[0028] The invention provides a kind of preparation method of solid acid catalyst, comprises the following steps:

[0029] Perform hydrothermal synthesis reaction of silica sol, aluminum hydroxide and inorganic strong base to obtain hydrothermal synthesis product system;

[0030] performing an ion exchange reaction with the hydrothermal synthesis product system and ammonium nitrate solution to obtain a solid acid catalyst precursor;

[0031] The solid acid catalyst precursor is calcined to obtain a solid acid catalyst.

[0032] In the invention, silica sol, aluminum hydroxide and inorganic strong base are subjected to hydrothermal synthesis reaction to obtain a hydrothermal synthesis product system.

[0033] In the present invention, the hydrothermal synthesis reaction of silica sol, aluminum hydroxide and inorganic strong base preferably specifically includes first mixing the silica sol and aluminum hydroxide uniformly to obtain a gel, and then adding The inorganic strong b...

Embodiment 1

[0050] Mix 1.0 mol of silica sol, 160 mol of aluminum hydroxide and 0.2 mol of sodium hydroxide, and carry out hydrothermal synthesis reaction at 200°C for 40 hours to obtain a hydrothermal synthesis product system; add 100 mL of 0.3 mol / L of ammonium nitrate solution, carried out ion exchange reaction 3 times at 70°C, dried at 120°C for 6h to obtain a solid acid catalyst precursor; roasted the solid acid catalyst precursor at 520°C for 5h, and ground to The particle size is 0.8 μm, and a solid acid catalyst is obtained, and the acidity of the solid acid catalyst is H 0 ≤-3, the acid content is 1.56mmol / g cat.

Embodiment 2

[0052] Mix 1.0 mol of silica sol, 20 mol of aluminum hydroxide and 0.03 mol of sodium hydroxide, and conduct a hydrothermal synthesis reaction at 150°C for 12 hours to obtain a hydrothermal synthesis product system; add 50 mL of 0.1 mol / L ammonium nitrate solution, ion exchange reaction was carried out 3 times at 60°C, and dried at 100°C for 8h to obtain a solid acid catalyst precursor; the solid acid catalyst precursor was roasted at 450°C for 3h, and ground to The particle size is 0.5 μm, and a solid acid catalyst is obtained, and the solid acid catalyst H 0 ≤-3, the acid content is 1.35mmol / g cat.

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Abstract

The invention relates to the technical field of organic synthesis, in particular to a solid acid catalyst as well as a preparation method thereof and a preparation method of hydroxy phenylglycine. Theinvention provides the preparation method of the solid acid catalyst; the preparation method comprises the following steps that ludox, aluminum hydroxide and inorganic strong alkali are subjected tohydrothermal synthesis reaction, so that a hydrothermal synthesis product system is obtained; the hydrothermal synthesis product system and ammonium nitrate solution are subjected to ionic exchange reaction, so that a solid acid catalyst precursor is obtained; and the solid acid catalyst is roasted, so that the solid acid catalyst is obtained. The solid acid catalyst provided by the invention is used for preparing hydroxy phenylglycine, the yield of hydroxy phenylglycine is as high as 75.2%, the product purity reaches up to 99.3%, and the activated solid acid catalyst has an excellent catalytic effect after being recycled for ten times. The solid acid catalyst provided by the invention has high acidity, high catalytic efficiency and high recycling rate, meanwhile, the preparation method issimple, no template is used, and the solid acid catalyst is environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a solid acid catalyst, a preparation method thereof, and a preparation method of p-hydroxyphenylglycine. Background technique [0002] p-Hydroxyphenylglycine is an important pharmaceutical intermediate, mainly used in the production of β-lactam semi-synthetic antibiotics. In the synthetic production of broad-spectrum antibiotics such as amoxicillin (amoxicillin), cefadroxil (Ouyi), and cefoperazone, p-hydroxyphenylglycine is an essential side chain acid. [0003] At present, most of the catalysts used in the synthesis of p-hydroxyphenylglycine are sulfuric acid or organic sulfonic acid catalysts. For example, Chinese patent CN101362703B discloses a synthesis method of p-hydroxyphenylglycine, using benzenesulfonic acid, p-toluenesulfonic acid or o-toluenesulfonic acid as a catalyst to prepare p-hydroxyphenylglycine with a yield of 56-65%. Chinese patent CN102050752A di...

Claims

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Application Information

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IPC IPC(8): B01J21/12B01J37/10B01J37/30C07C229/36C07C227/10
Inventor 刘宏民赵兵谢建中马立英汤英刘光耀郭文阁王超刘超魏浩明
Owner ZHENGZHOU UNIV
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