Preparation method of 3,3',4,4'-tetraaminobibenzene
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A technology of tetraaminobiphenyl and nitrobenzene, which is applied in the field of preparation of chemical intermediates, can solve problems such as difficult handling, serious pollution, and difficult industrial production, and achieve low environmental pollution, high quality, and simple post-processing. Effect
Active Publication Date: 2018-06-29
ZHEJIANG DINGLONG TECH
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[0004] After experimental verification of the above scheme, it is found that a large amount of residue and waste water will be generated in
Method used
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Embodiment 1
[0028] Take 106g of o-chloronitrobenzene and 32g of 43% liquid caustic soda, add 0.4g of 1,4-naphthoquinone and 20g of water, raise the temperature to 56°C, add 314g of 43% liquid caustic soda and 224g of formaldehyde in double drops, react for 7 hours, then add 250g water, cooled to room temperature, and filtered. Add 0.94g sodium dodecylbenzenesulfonate, 0.56g 1,4-naphthoquinone, 0.94g aluminum-nickel alloy, 226g water, 55.2g 43% liquid caustic soda to the filter cake, stir and heat up to 56°C, then add hydrazine hydrate dropwise 50g, the dropwise addition time is 7h, after the addition, continue to keep warm for 0.5h. After the reaction, 100ml of cold water was added, cooled to room temperature, dried by suction filtration, and recrystallized with absolute ethanol to obtain a reduced product (reduced material). Stir 124g of concentrated hydrochloric acid and 34.3g of water to cool down to 5°C, slowly add a batch of reducing materials, keep at 5°C for 2h, then raise the tem...
Embodiment 2～8
[0030] The reaction process is as in Example 1, changing process parameters, such as condensation reaction temperature, o-chloronitrobenzene, liquid caustic soda, weight ratio of formaldehyde, reduction reaction temperature, weight ratio of condensate to hydrazine hydrate, rearrangement product, ammonia water, ammonia 3,3',4,4'-tetraaminobiphenyl was prepared according to the weight ratio of gas, and the IR of the product was consistent with the standard spectrum of 3,3',4,4'-tetraaminobiphenyl. The result of embodiment 2~8 is as shown in table 1:
[0031] Table 1
[0032]
[0033] The invention reduces environmental pollution while improving product quality, makes product production clean and environmentally friendly, and makes the product more suitable for mass production.
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Abstract
The invention relates to a preparation method of 3,3',4,4'-tetraaminobibenzene, which includes the steps of: (1) with an o-chloronitrobenzene compound, alkali, and an aldehyde compound as raw materials, performing a condensation reaction in a certain solvent with a 1,4-naphthoquinone compound as a catalyst; (2) adding the 1,4-naphthoquinone compound and Al/Ni alloy, as a reduction catalyst, to thecondensation product, and adding a sodium dodecyl benzene sulfonate compound as an emulsifier to perform a reaction with hydrazine hydrate to obtain a hydrogenated reaction solution, and performing temperature-reduced crystallization and re-crystallization, then performing temperature-reduced filtration or skimming concentration to obtain a hydrogenated product; (3) performing rearrangement reaction to the hydrogenated product under acidic conditions to obtain a rearrangement product; (4) with a copper salt compound as a catalyst, performing a reaction to the rearrangement product with ammonia water and ammonia gas at high temperature under high pressure, and cooling and filtering the product to obtain the 3,3',4,4'-tetraaminobibenzene. The method can improve quality of the product and reduce environment friendly, achieves cleanness and environmental protection of production and is suitable for large-scale production.
Description
technical field [0001] The invention relates to a preparation method of a chemical intermediate, in particular to a preparation method of high-quality 3,3',4,4'-tetraaminobiphenyl. Background technique [0002] 3,3’,4,4’-Tetraaminobiphenyl belongs to biphenyl compounds and can be used as an intermediate in the production of yellow and orange dyes. [0003] The preparation methods reported about 3,3',4,4'-tetraaminobiphenyl generally adopt electrolytic reduction, catalytic hydrogenation, and chemical reduction. Use glucose alkaline aqueous solution to reduce o-nitrochlorobenzene to 2,2'-dichloroazobenzene, and then use zinc powder to prepare 2,2'-dichlorohydroazobenzene. In acidic pure solution The middle rearrangement is 3,3'dichlorobenzidine, and the amine is added to get 3,3',4,4'-tetraaminobenzidine. [0004] After experimental verification of the above scheme, it is found that a large amount of residue and waste water will be generated in the post-treatment process by ...
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