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4,6-diaminoresorcinol hydrochlorate preparation method

A technology of diaminoresorcinol hydrochloride and dihydroxybenzene, which is applied in 4 fields, can solve the problems of cumbersome organic solvent recovery, etc., and achieve the effects of easy processing, reduced environmental protection costs, and high yield

Inactive Publication Date: 2006-04-26
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem that the present invention needs to solve is to disclose a kind of new preparation method of 4,6-diaminoresorcinol hydrochloride, to overcome the shortcoming of loaded down with trivial details and the recovery of expensive organic solvent existing in the prior art

Method used

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  • 4,6-diaminoresorcinol hydrochlorate preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Grind coconut shell activated carbon and sieve to obtain 300-400 mesh activated carbon powder. Add a certain amount of activated carbon to nitric acid with a weight concentration of 10%, stir in a water bath at 80°C for 2 hours, then filter and wash with distilled water to obtain Neutral; then treated with water vapor, dried and set aside. Dissolve nickel nitrate in deionized water to make 2.1×10 -1 mol / L nickel nitrate solution, add 10g of activated carbon treated above to 37ml nickel nitrate aqueous solution, impregnate for 2h, age in air for 24h, dry in air at 100-110°C for 24h, and bake in a muffle furnace at 250°C for 5h , That is, 5% (wt) NiO / C is obtained for use. Dissolve chloroplatinic acid in deionized water to make 1.7×10 -2 mol / L chloroplatinic acid solution. Add activated carbon loaded with Ni to 278ml of chloroplatinic acid aqueous solution, soak for 2 hours, then add 8ml of formaldehyde for reduction, and at the same time add saturated sodium bicarbona...

Embodiment 2

[0029] The preparation of 3% NiO / C is the same as in Example 1. Dissolve palladium chloride in deionized water to make a 1.7×10 -2 mol / L palladium chloride solution. Add activated carbon loaded with Ni element into 278ml of palladium chloride aqueous solution, soak for 2 hours, then add 8ml of formaldehyde for reduction, and at the same time add saturated sodium bicarbonate solution dropwise, control the pH value to about 9, react until the pH value remains unchanged, filter After drying, a Pd-Ni / C catalyst with a Pd content of 5% is obtained.

[0030] Add 70g of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene, 350ml of water, 7g of the above 5%Pd-3%Cu / C, and 1g of ammonium acetate into a 1000ml reactor. Will N 2 Introduce air into this sealed reactor for three times, and then use H 2 Replace three times. h 2 The pressure reached 3Mpa, the temperature reached 80°C, and the reaction was carried out for 1 hour. After the reaction was completed, the reaction feed liquid was coole...

Embodiment 3

[0032] The processing of activated carbon is as described in Example 1. Dissolve cobalt nitrate in deionized water to make 2.1×10 -1 mol / L cobalt nitrate solution, add 10g of activated carbon to 39ml cobalt nitrate aqueous solution, impregnate for 2h, age in air for 24h, dry in air at 105°C for 24h, and roast in a muffle furnace at 250°C for 5h, namely Get 5% (wt) CoO / C for use. According to the loading method of Pt in Example 1, a 5%Pt-5%Co / C catalyst was prepared.

[0033] Add 70g of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene, 350ml of water, 7g of 5%Pt-5%Co / C, and 2g of ammonium formate into a 1000ml reactor. Will N 2 Introduce air into this sealed reactor for three times, and then use H 2 Replace three times. h 2 The pressure reached 0.9Mpa, the temperature was raised to 30°C, the heating was stopped, and the temperature was automatically raised to 90°C as the reaction progressed, and the reaction was carried out for 5 hours. After the reaction was completed, the reac...

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Abstract

The preparation process of 4, 6-diamino resorcinol hydrochloride includes the following steps: dissolving 4, 6-dinitro-2-chloro-1, 3-dihydroxy benzene in water to form water solution, adding dechloronating promoter, and reaction with hydrogen in the presence of rare metal and transition metal catalyst. The process is one economic process with high yield and high quality of 4, 6-diamino resorcinol hydrochloride, with the yield reaching 99 %, and has easy treatment of the reaction waste water. Therefore, the process of the present invention has excellent industrial production application foreground.

Description

technical field [0001] The invention relates to a preparation method of 4,6-diaminoresorcinol hydrochloride, which is prepared by catalytic hydrogenation of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene to 4 , 6-diaminoresorcinol hydrochloride. Background technique [0002] 4,6-Diaminoresorcinol hydrochloride is an important structural unit of various macromolecules, especially polybenzoxazoles (cf. Wolf et al., "Macromolecules" 1981, 14:915). [0003] Its structural formula is as follows: [0004] [0005] US5399768 and US5371281 and US925358 describe the method for preparing 4,6-diaminoresorcinol through catalytic hydrogenation of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene, an obvious one of said method The disadvantage is the heterogeneous catalytic hydrogenation of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene in organic solvents with batch hydrogenation over Pd / C catalysts, due to the recovery and recycling of organic solvents Process is essential, which will involve expen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/80C07C213/02
Inventor 王幸宜李到金中豪
Owner EAST CHINA UNIV OF SCI & TECH
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