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A technology of solvent and monomethylamine, which is applied in the field of organic chemical synthesis, can solve the problems of low product yield, large amount of waste water, high water content, etc., and achieve the effects of increased yield, reduced waste water, and low water content
Inactive Publication Date: 2015-06-24
JIANGSU DAOBO CHEM
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However, there are many shortcomings in this process, the product yield is low, only about 70%, the amount of wa
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Embodiment 1
[0015] Put 400g of 5w% liquid caustic soda into the reactor, then add 40g of 1,4-dihydroxyanthraquinone, 3g of hydrosulfite, 17.2g of monomethylamine, close the reaction system, start to heat up to 70°C, keep it warm for 12h, and the reaction is over , start to filter, wash until the filtrate is clear, dry, and weigh. After HPLC detection, the purity of the finished product is 95%, and the yield is 92%. After inspection, the color light and intensity are all qualified.
Embodiment 2
[0017] Put 400g of 6.5w% liquid caustic soda into the reactor, then add 40g of 1,4-dihydroxyanthraquinone, 3g of hydrosulfite, 17.2g of monomethylamine, close the reaction system, start to heat up to 70°C, keep warm for 12h, and react At the end, start to filter, wash until the filtrate is clear, dry, and weigh. After HPLC detection, the purity of the finished product is 96%, and the yield is 90%. After inspection, the color light and intensity are all qualified.
Embodiment 3
[0019] Put 400g of 8w% liquid caustic soda into the reactor, then add 40g of 1,4-dihydroxyanthraquinone, 3g of hydrosulfite, 17.2g of monomethylamine, close the reaction system, start to heat up to 70°C, keep it warm for 12h, and the reaction is over , start to filter, wash until the filtrate is clear, dry, and weigh. After HPLC detection, the purity of the finished product is 96%, and the yield is 88%. After inspection, the color light and intensity are all qualified.
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Abstract
The invention discloses a method for preparing solvent blue 78. The method comprises the following steps: adding liquid caustic soda and 1,4-dihydroxyanthraquinone into a reactor, uniformly stirring, adding sodium hydrosulfite and monomethyl amine, sealing the reactor, heating, carrying out heat insulation for several hours, cooling to normal temperature after the reaction ends, filtering, washing, and drying to obtain a finished product. Compared with the prior art, the method has the following advantages: 1, the yield increases by near 20%; 2, the water content is small, easy drying is realized, and the drying time of 1t of a material is shortened to 12h from original 2d, so energy consumption is greatly reduced; and 3, environmental protection, energy saving and great reduction of wastewater are realized.
Description
technical field [0001] The invention relates to a method for synthesizing solvent blue, in particular to a method for synthesizing solvent blue 78, which belongs to the field of organic chemical synthesis. Background technique [0002] Solvent blue 78, also known as transparent blue GP, chemical name, 1,4-bis(methylamino)anthraquinone, has the same chemical structure as disperse blue 14, CAS: 2475-44-7. Solvent blue 78 is mainly used for the coloring of various thermoplastics, resins and polyester raw pulp, and is also used in the manufacture of fireworks. Its structural formula is: [0003] [0004] The main synthetic route of solvent blue 78 is: 1, 4-dihydroxyanthraquinone and monomethylamine are used as the main raw materials, and the two are condensed under the catalysis of zinc powder, and the reaction formula is as follows: [0005] [0006] At present, this method is adopted by most enterprises at home and abroad. However, there are many disadvantages in this...
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