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Preparation method of 4,4`-diaminobibenzyl-2,2`-disulfonic acid

A disulfonic acid and diamino technology, which is applied in the direction of sulfonic acid preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of many side reactions, high reaction temperature, and aggravation, so as to improve chemical selectivity, The effect of reducing production cost and reducing dosage

Inactive Publication Date: 2020-03-31
ZHEJIANG UNIV
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  • Claims
  • Application Information

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Problems solved by technology

The method can be carried out under normal pressure, but the amount of hydrazine hydrate is large, the reaction temperature is high, there are many side reactions, and the product yield is low
In this reaction, if the amount of hydrazine hydrate is reduced or the reaction temperature is lowered, the product yield will be exacerbated

Method used

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  • Preparation method of 4,4`-diaminobibenzyl-2,2`-disulfonic acid
  • Preparation method of 4,4`-diaminobibenzyl-2,2`-disulfonic acid
  • Preparation method of 4,4`-diaminobibenzyl-2,2`-disulfonic acid

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preparation example Construction

[0037] The preparation method of iron-nickel composite carrier type catalyst:

[0038] 30g FeCl 3 Add 100g of distilled water, adjust the pH to 1.0 with concentrated hydrochloric acid (mass concentration is about 37%), as iron impregnation solution; 2 Dissolve in 100g of distilled water as nickel impregnating solution; mix iron impregnating solution and nickel impregnating solution with 100g activated carbon and stir for 12 hours, then stir and reflux for 1 hour in a constant temperature water bath at 45°C, and use 1% NaOH aqueous solution Adjust the pH to 9-10, raise the temperature to 80°C, add NaOH, keep the pH constant, stir for 8h, filter, and burn the obtained solid at 400°C for 3h to obtain the corresponding iron-nickel composite catalyst (iron-nickel composite support catalyst) . The details are described in Table 1 below.

[0039] Table 1

[0040]

[0041] Note: 15% Fe 2 o 3 -5% NiO / C catalyst, Fe 2 o 3 The mass of NiO is 15% of the total mass of the compos...

Embodiment 1

[0042] Embodiment 1, a kind of preparation method of DADB comprises the steps:

[0043] 1), add 12.9g (0.03mol) DNS in the 250ml three-necked flask, 70ml ethylene glycol, 0.645g iron-nickel composite catalyst (15%Fe 2 o 3 -5%NiO / C), heated to 100°C, slowly dripped 7.1g (85wt% 0.12mol) hydrazine hydrate, and controlled the system temperature ≤ 105°C during the dropwise addition; after all the hydrazine hydrate was added dropwise, the temperature was raised to 140°C , insulation reaction 2h.

[0044] 2), after the reaction of step 2) finishes, be cooled to room temperature, filter, the filter cake of filtering gained is naturally dried to constant weight, as recyclable iron-nickel composite catalyst;

[0045] Add 10mol / l concentrated hydrochloric acid to the filtrate obtained by filtration, until the pH is 2-3, a white solid is precipitated, and the solid is obtained by filtration and dried (dried at 60°C to constant weight) to obtain DADB as the product (purity is 99 %).

Embodiment 2～9

[0046] Embodiment 2~9, change DNS and hydrazine hydrate molar ratio, catalyst consumption, reaction time and reaction temperature in embodiment 1, all the other contents are equal to embodiment 1, obtain embodiment 2~9 respectively, specific process parameter and gained DADB The yields are shown in Table 2.

[0047] Table 2

[0048]

[0049]

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Abstract

The invention discloses a preparation method of 4,4'-diaminodiphenyl-2,2'-disulfonic acid. The preparation method comprises the following steps: mixing a DNS, a iron-nickel composite carrier-type catalyst and a solvent in a reactor; then dropwise adding hydrazine hydrate for carrying out a reaction, wherein the solvent is ethylene glycol or diethylene glycol; and after the reaction is finished, carrying out cooling to room temperature, carrying out filtering, adjusting the pH value of the filtrate to 2-3, and drying the separated solid to obtain the 4,4'-diaminodiphenyl-2,2'-disulfonic acid. According to the method, the reaction can be carried out under normal pressure, a precious metal catalyst is not needed, production cost is low, and the yield is high.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 4,4'-diaminobibenzyl-2,2'-disulfonic acid. Background technique [0002] 4,4'-diaminobibenzyl-2,2'-disulfonic acid, referred to as DADB, its molecular formula is C 14 h 16 N 2 o 6 S 2 , with a molecular weight of 372 and a structural formula as shown in formula 1, is an important chemical intermediate and has important applications in the dye industry. [0003] [0004] Judging from the domestic and foreign literature reported so far, the main preparation method of DADB is to use 4,4'-dinitrostilbene 2,2'-disulfonic acid (DNS) as raw material, and then reduce to obtain the product, according to the reducing agent The differences are mainly divided into the following categories: [0005] Literature (Shiyou Huagong, 32(11), 941-943; 2003) reported a method for preparing DADB using DNS and hydrogen as raw materials, water as a solvent, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/22C07C309/46B01J23/745
CPCB01J23/745C07C303/22C07C309/46Y02P20/584
Inventor 陈新志曹忠阮诗想钱超周少东
Owner ZHEJIANG UNIV
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