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P-aminophenyl-beta-hydroxyethyl sulfone preparation method

A technology of p-aminophenyl and hydroxyethyl sulfone, which is applied in the field of preparation of β-hydroxyethyl sulfone, can solve the problems of difficult catalyst recovery, high production cost, and low product yield, and achieve easy recovery and short reaction time , the effect of small dosage

Inactive Publication Date: 2009-02-11
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of high production cost, difficult catalyst recovery, low product yield and environmental pollution in the existing preparation process of p-aminophenyl-β-hydroxyethyl sulfone; and a kind of p-aminophenyl -The preparation method of β-hydroxyethyl sulfone

Method used

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specific Embodiment approach 1

[0013] Specific embodiment one: the preparation method of p-aminophenyl-β-hydroxyethyl sulfone in this embodiment is completed by the following reaction: p-nitrophenyl-β-hydroxyethyl sulfide, nickel aluminum alloy catalyst Mix with solvent, pass in nitrogen to remove the air, then pass in hydrogen to control the pressure of hydrogen to 0.5~6MPa, while stirring at a speed of 500~1000r / min, and raise the temperature to 40~100°C, react for 4~12h, then filter and distill and drying to obtain p-aminophenyl-beta-hydroxyethyl sulfone; wherein the consumption of nickel-aluminum alloy catalyst is 0.5%~5% of p-nitrophenyl-beta-hydroxyethyl sulfide quality, and the solvent consumption is p-nitrophenyl 1 to 5 times the mass of phenyl-β-hydroxyethyl sulfide; the solvent is one of water, methanol, ethanol, propanol, butanol, dimethylformamide or a mixture of several of them.

[0014] In this embodiment, when the solvent is a mixture, various mixtures are mixed in any ratio. In this embodim...

specific Embodiment approach 2

[0019] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the nickel-aluminum alloy catalyst is made by the following method: 1. The nickel-aluminum alloy powder containing 40% to 70% nickel, organic Adhesives, inorganic adhesives, extrusion aids and peptizers are mixed to obtain jelly; 2. The jelly is directly kneaded and shaped, dried under an infrared lamp, and then dried at 120°C for 12 hours, and then Roast at 400-450°C for 1-3 hours, heat up to 500-600°C for 2-4 hours, and heat up at 800-900°C for 2-5 hours; 3. Crush the product in step 2 and sieve out a particle size of 40 ~60 mesh particles, the sieved particles are leached in the activator at 50~90°C for 6~36h, the stirring speed is 50~80r / min during the leaching process, and the water is continuously replenished during the leaching process to maintain a constant solution volume, and then Washing with deoxidized and deionized water until the pH value of the leached water is 7 to 8 to obtain ...

specific Embodiment approach 3

[0021] Embodiment 3: This embodiment is different from Embodiment 2 in that the molecular weight of the organic binder is 30,000-300,000. Others are the same as in the second embodiment.

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Abstract

The invention relates to a method for preparing p-aminophenyl-beta-hydroxyethyl sulfone, in particular to a method for preparing beta-hydroxyethyl sulfone. The method solves the problems of high production cost, difficulty in catalyst recycling, low product yield and serious pollution to the environment existed in the prior art for preparing the p-aminophenyl-beta-hydroxyethyl sulfone. The method is as follows: p-aminophenyl-beta-hydroxyethyl sulfide and nickel aluminium alloy catalyst and solvent are added in a hydrogenation reactor; after nitrogen which removes off the air is introduced, hydrogen is introduced and the pressure of the hydrogen is controlled at 0.5MPa to 6MPa; meanwhile, stirring is carried out at the speed of 500r / min to 1000r / min and the temperature is raised to 40 DEG C to 100 DEG C for reaction for 4h to 12h; after filtration, distillation and drying, the p-aminophenyl-beta-hydroxyethyl sulfone is obtained. The method has the advantages of low production cost, easy-recycling catalyst, high product yield, high product pureness and less pollution to the environment. The pureness of the product is more than 97 percent and the yield is more than 95 percent (calculated by nitro compounds).

Description

technical field [0001] The invention relates to a preparation method of β-hydroxyethyl sulfone. Background technique [0002] p-Aminophenyl-β-hydroxyethylsulfone is an important intermediate of vinylsulfone-type reactive dyes, and is generally prepared by reducing p-nitrophenyl-β-hydroxyethyl sulfide with iron powder. At present, the iron powder reduction method is generally used in China, and its biggest disadvantage is that a large amount of iron sludge and waste water containing aromatic amines are generated, causing environmental pollution. In order to develop an environment-friendly process, people try to replace the original iron powder reduction process with catalytic hydrogenation. The key to catalytic hydrogenation is to develop a catalyst with excellent performance. At present, the application of catalysts in the catalytic hydrogenation reduction method is roughly divided into noble metal hydrogenation catalysts and non-noble metal hydrogenation catalysts. Preci...

Claims

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Application Information

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IPC IPC(8): C07C317/36C07C315/04
CPCY02P20/584
Inventor 胡永玲韩大维田勇
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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