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A synthesis method and nonanediamine technology are applied in chemical instruments and methods, preparation of carboxylic acid amides, preparation of organic compounds, etc., and can solve problems such as high requirements for production equipment, inability to apply in the field of food, and not yet achieved localization, etc. The effect of increasing productivity
Active Publication Date: 2018-11-02
BEIJING RISUN TECH CO LTD
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[0019] Aiming at the problems that the existing nonanediamine production process produces a large amount of "three wastes", the content of nonanediamine is low, it cannot be used in the food field, the req
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Embodiment 1
[0057]
[0058] step 1:
[0059] Add 140 ml of methanol and 174 grams of undecanedioic acid into a 500 ml three-necked flask, and slowly add 201 grams of thionyl chloride at room temperature. The temperature was raised to reflux and the reaction was continued for 90 minutes. After the reaction system was naturally cooled to 25°C, the solvent was removed by a rotary evaporator to obtain 192.62 grams of dimethyl undecanedate (GC=99.2%), which was directly used for the next step reaction raw material.
[0060] Step 2:
[0061] Add 192.62 grams of dimethyl undecanedioate, 140 milliliters of methanol, and 12.63 grams of ammonia water (mass fraction=25%) into a 500 ml three-necked flask, and stir and react at 40° C. for 1 hour. The solvent was removed to obtain the intermediate of the second step: 160.5 g of undecanediamide.
[0062] Step 3:
[0063] Add 21.4 grams of undecanediamide to the freshly prepared aqueous solution of sodium hypochlorite (composed of 0.2 mol of sodiu...
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Abstract
The invention provides a synthetic method of 1,9-diaminononane. The method comprises the following steps: firstly, carrying out condensation reaction on undecanoic acid and transforming the undecanoicacid into a derivative of the undecanoic acid; then carrying out ammoniation to generate undecendiamide, and then carrying out Hofmann rearrangement reaction to generate a target product 1,9-diaminononane. The method disclosed by the invention has the advantages that raw materials are inexpensive and easily obtained and have a sufficient supply, and high-temperature and high-pressure reaction conditions are not involved, and a production process has more security. Compared with an abroad production technology, the synthetic method disclosed by the invention has the advantages of less side reaction, high purity of the product, less reaction steps and low requirement on equipment. Compared with a production process reported by domestic companies, the synthetic method has the advantages of less three wastes, and meanwhile, hydrogenation reaction is not involved, and the synthetic method has higher reaction security.
Description
technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis method of nonanediamine. Background technique [0002] Nonanediamine is also known as 1,9-diaminononane, 1,9-nonanediamine, nonyldiamine, English name 1,9-Nonanediamine, 1,9-Diaminononane, 1,9-Nonamethylene -diamine. [0003] Nonanediamine is mainly used as the raw material of PA9T. PA9T resin is a new type of heat-resistant polyamide resin. At present, this heat-resistant resin is in the stage of market development. Only a few manufacturers can realize industrialization, and there is no domestic industrialization report. PA9T has many advantages such as excellent low water absorption, high rigidity, resistance to pharmaceutical solvents, toughness, heat resistance, dimensional stability and excellent formability. Compared with common high-performance plastics, such as polyphenylene sulfide (PPS), PA46, PA6T, etc., it has some other performance advanta...
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