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Catalytical hydrogenation process to produce II acid

A catalytic hydrogenation and process technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as high cost

Active Publication Date: 2006-08-02
JIANGSU JIHUA CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Platinum is an excellent catalyst, but it is expensive

Method used

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  • Catalytical hydrogenation process to produce II acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Amino value is 25g / L nitro-T acid and its salt solution adjustment pH is 7.5, changes in the autoclave, adds the catalyzer that is 0.5% by nitro-T acid weight measurement, and this catalyzer is the composite nickel containing 20% ​​cobalt Cobalt catalyst, first react at 100-105°C for 2 hours under a hydrogen pressure of 1.0-2.0MPa under high-speed stirring, and then feed hydrogen to a pressure of 2.5MPa and further catalyze the reaction at 120°C for 2 hours, and then detect the amino acid by HPLC Conversion >95.

Embodiment 2～10

[0031] Examples 2-10 (catalytic hydrogenation reaction temperature, time, and reaction in the following examples refer to the second step reaction, and the first step hydrogenation reaction strips are all reacted at 100-105° C. for 2 hours under a hydrogen pressure of 1.0-2.0 MPa) :

[0032] Reality

Embodiment 11

[0034] Nitro-T acid HPLC content>98 nitrous acid concentration adjustment of solution is 35g / L, adds in autoclave, adds solid sodium hydroxide and is 50% of nitro-T acid weight measurement, adds methyl alcohol to be nitro-T acid weight measurement 45% of the metered amount, alkali fusion at 185°C for 2 hours, the alkali melt can be obtained. The alkali fusion conversion rate of amino T acid detected by HPLC is greater than 96%.

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Abstract

The present invention relates to catalytical hydrogenation process to produce H acid, and solves the technological problem of providing one new type of catalyst to lower the reaction pressure, reaction temperature and production cost effectively. The process includes the following steps: 1. regulating the nitroso value of nitro T acid and its solution as material to 15-45 g / L and the pH value to 7-10; 2. catalytical hydrogenation through adding the regulated solution and Ni-Co catalyst with Co content of 0.5-25 wt% and in the amount of 0.1-5 wt% of nitro T acid into high pressure reactor, introducing H2 of 1.0-4.5 Mpa pressure at 90-220 deg.c, and hydrogenating catalytically for 2-5 hr to obtain amino T acid and its solution; 3. alkali fusing; and 4. acid out to obtain the product.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a process for producing H acid by catalytic hydrogenation. Background technique [0002] H acid (formula I) is an intermediate for the preparation of water-soluble dyes and is widely used. [0003] (Formula I). [0004] JP 50142546 discloses the early production process: the main steps are as follows (1) trisulfonation of naphthalene to obtain naphthalene 1,3,6-trisulfonic acid, (2) nitration of naphthalene 3,6,8-trisulfonic acid, Obtain nitro T acid (formula II), (3) alkali neutralization, (4) use iron powder to reduce nitro T acid to obtain amino T acid (formula III), (6) alkali-melt amino T acid to obtain H acid, ( 5) Acid precipitation of H acid. DE 3020441 improved it by using ammonia water to neutralize instead of alkali neutralization. After the reduction of iron powder, sodium salt was used to replace the ammonium salt of the reduced product with sodium salt, which w...

Claims

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Application Information

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IPC IPC(8): C07C303/22C07C309/50B01J23/74
Inventor 樊军简卫陈美芬
Owner JIANGSU JIHUA CHEMICAL CO LTD
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