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Method for preparing 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride

A technology of tetraaminonaphthalene tin chloride and hydrochloride is applied in the preparation of amino compounds, the preparation of organic compounds, chemical instruments and methods, etc., and can solve the problems of difficult industrialized scale-up production, cumbersome post-processing, and many by-products, etc. Achieve the effect of increased fiber surface energy, good wettability and low cost

Active Publication Date: 2015-01-07
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the technical problems that there are many by-products in the preparation of 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride by the existing method, the cost is high, the yield is low, the post-treatment is cumbersome, and it is difficult to scale up production in an industrialized manner. , thereby providing a preparation method of 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride

Method used

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  • Method for preparing 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride
  • Method for preparing 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride
  • Method for preparing 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride

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specific Embodiment approach 1

[0018] Specific embodiment 1: The preparation method of 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride in this embodiment is carried out according to the following steps:

[0019] 1. Using 1,5-dinitronaphthalene as the starting material, add it to the reaction flask at room temperature, add the nitrating reagent, and then heat to 40~100℃, keep the reaction temperature for 2~5h, and then cool to room temperature. The reaction mixture is then poured into an ice-water mixture, stirred, filtered, and washed with water until it is neutral to obtain crude 1,4,5,8-tetranitronaphthalene, and the solvent is recrystallized to obtain high purity 1,4, 5,8-Tetranitronaphthalene.

[0020] 2. Add organic solvent to the 1,4,5,8-tetranitronaphthalene obtained in step 1, then add concentrated hydrochloric acid and catalytic promoter, add reducing agent at a temperature of 30-40℃, keep it for 2~3h , Then heated to 50~100℃ for catalytic reduction reaction for 3~5h, cooled to room temperatur...

specific Embodiment approach 2

[0024] Specific embodiment two: This embodiment is different from specific embodiment one in that: the nitrating agent described in step one is a mixed solution of concentrated sulfuric acid and fuming nitric acid, a mixed solution of concentrated sulfuric acid and potassium nitrate or fuming nitric acid. Others are the same as the first embodiment.

specific Embodiment approach 3

[0025] Specific embodiment three: This embodiment is different from specific embodiment one or two in that: in step one, it is heated to 50-80° C. and kept for 3 to 4 hours for reaction. Others are the same as the first or second embodiment.

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Abstract

The invention discloses a method for preparing 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride and relates to a method for preparing hydrochloride. The method aims at solving the technical problems of more by-products, high cost, low yield, tedious after-treatment and difficulty in industrial large-scale production of the existing method for preparing 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride. The method disclosed by the invention comprises the following steps: firstly, preparing high-purity 1,4,5,8-tetranitronaphthalene; and secondly, preparing high-purity 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride. Due to the method, high-purity 1,4,5,8-tetranitronaphthalene which is difficult to synthesize by virtue of the conventional method can be successfully prepared and 1,4,5,8-tetraaminonaphthalene tin chloride hydrochloride is prepared from stannous chloride and concentrated hydrochloric acid in high efficiency by virtue of adding catalytic addictives and the operation process is simplified. The method has the advantages of inexpensive and available selected raw materials, high yield, low cost and environmental friendliness and is suitable for industrial scale-up. The method is applied in the field of preparation of organic intermediate.

Description

Technical field [0001] The invention relates to a preparation method of hydrochloride. Background technique [0002] According to the relationship between structure and performance, the research and development team headed by Wolf synthesized polyparaphenylene benzobisoxazole (PBO) fiber from the perspective of molecular design. Rigid macromolecular structure and large main chain bond energy. After liquid crystal spinning, the macromolecular chain is highly oriented along the axial direction and highly crystalline, which makes PBO fibers have excellent comprehensive properties (Shen Xinyuan. Advanced Polymer Materials [M]. Beijing: China Textile Publishing Society, 2006.156-157). However, due to the relatively weak interaction force between the PBO polymer molecules, its resistance to compression and torsion is relatively poor. The fiber surface has weak polarity and strong inertness and poor bonding ability with resin. If the surface is not modified during use, there will be a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/58C07C209/36C08G69/26
Inventor 杨蕾黄玉东张小飞王阳张华
Owner HARBIN INST OF TECH
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