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Process for preparing 4, 6-diamino resorcin

A technology of diaminoresorcinol and dihydroxybenzene, which is applied in 4 fields, can solve the problems that rare metal catalysts cannot be recycled economically, and achieve the prospect of large-scale industrial production, the effect of catalyst activity not being reduced, and high yield

Inactive Publication Date: 2005-01-26
山东泰山染料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to disclose a new preparation method of 4,6-diaminoresorcinol, so as to overcome the disadvantage that the rare metal catalysts in the prior art cannot be recycled economically.

Method used

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  • Process for preparing 4, 6-diamino resorcin

Examples

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Embodiment 1

[0024] Grind coconut shell activated carbon and sieve to obtain 350 mesh activated carbon powder, add a certain amount of activated carbon to 10% nitric acid, stir in 80°C water bath for 2 hours, then filter, wash with distilled water to become neutral; then steam Process, dry, and reserve.

[0025] Dissolve copper nitrate in deionized water to make 2.1×10 -1 mol / L copper nitrate solution, add 10g of activated carbon treated above to 37ml copper nitrate aqueous solution, soak for 2h, age in air for 24h, dry in air at 100-110°C for 24h, and bake in muffle furnace at 250°C for 5h , that is, to obtain 5% (wt) CuO / C for use. Dissolve chloroplatinic acid in deionized water to make 1.7×10 -2 mol / L chloroplatinic acid solution. Add activated carbon loaded with Cu 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 bicarbonate solution dropwise, control the pH value to about 9, rea...

Embodiment 2

[0029] The preparation of 3% CuO / 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 Cu to 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-Cu / C catalyst with a Pd content of 5% is obtained.

[0030] Add 70 g of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene, 350 ml of propanol, and 7 g of the above 5% Pd-3% Cu / C into a 1000 ml 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 reaches 3Mpa and the temperature reaches 80°C. After the reaction, the reaction feed liquid was cooled to room temperature, filtered, and the catalyst was left in the reactor for re...

Embodiment 3

[0033] 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 100-110°C for 24h, and bake in muffle furnace at 250°C for 5h , that is, to obtain 5% (wt) CoO / C for use. According to the Pt loading method in Example 1, a 5%Pt-5%Co / C catalyst was prepared.

[0034] Add 70g of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene, 350ml of benzene, and 7g of 5%Pt-5%Co / C 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 reaches 0.9Mpa and the temperature reaches 30°C. After the reaction, the reaction feed liquid was cooled to room temperature, filtered, and the catalyst was left in the reactor for reuse. The filtrate contained 4,6-diaminoresorcinol. According to liquid chroma...

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Abstract

The invention discloses a process for preparing 4, 6-diamino resorcinol comprising the steps of, subjecting 4,6-dinitro-2-chlorin-1,3-dihydroxy benzene to catalytic hydrogenation with hydrogen under normal or medium pressure at normal temperature or heating condition, in organic solvent and at the presence of rare metals and transient metallic oxide catalyst, then collecting 4,6-diamino resorcinol from the reactant through the conventional methods.

Description

technical field [0001] The invention relates to a preparation method of 4,6-diaminoresorcinol, in particular to the preparation of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene by catalytic hydrogenation as a raw material , 6-diaminoresorcinol method. Background technique [0002] 4,6-Diaminoresorcinol 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 that the heterogeneous catalytic hydrogenation of 4,6-dinitro-2-chloro-1,3-dihydroxybenzene in batch hydrogenation over Pd / C catalysts cannot make expensive rare metal catalysts due to catalyst chlorine poisoning. Recycle economically. Contents of the invent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C215/80
Inventor 夏恩将夏恩胜岳岩吴言强夏念成张静
Owner 山东泰山染料股份有限公司
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