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Production process of granular 2,4,6-tri(amino caproyl)-1,3,5-triazine having low chlorine content
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A technology of aminocaproic acid base and aminocaproic acid salt, which is applied in the field of organic synthesis, can solve the problems of difficult separation and high chloride ion content, and achieve the effect of reducing the content of chloride ions, which is beneficial to industrial production, and is convenient for solid-liquid separation and washing
Active Publication Date: 2014-04-09
ZHEJIANG JINKE CHEM
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Abstract
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Problems solved by technology
[0005] The purpose of the present invention is to solve the problems of difficult solid-liquid separation and high chloride ion content of 2,4,6-tris(aminocaproic acid)-1,3,5 triazine emulsion slurry in the prior art, and provide a 2,4,6-tris(aminocaproic acid)-1,3,5-triazine direct granulation process
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Examples
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Effect test
Embodiment 1
[0016] Add 1.5L of tap water at 15°C to a 6L beaker, add dropwise 38% hydrochloric acid into the beaker to make the Ph value of the 15°C liquid in the beaker 0.1, and stir slowly; add 326g of 38% hydrochloric acid and the concentration 3500 g of 0.27mol / kg 2,4,6-tris(aminocaproic acid)-1,3,5 triazine solution was added dropwise into the beaker at the same time, the hydrogen ions in the acid and 2,4,6-tris(aminocaproic acid) acid base)-1,3,5-triazine with a molar ratio of 3.6:1, after 90 minutes of dropwise addition, stir for 5 minutes, and filter the material for solid-liquid separation; the filter cake is rinsed with 3L of water and dried to obtain Granular product 835g, wherein the water mass fraction is 50%, and the chloride ion content is 150mg / kg.
Embodiment 2
[0018] Add 1.5L of tap water at 35°C to a 6L beaker, add concentrated sulfuric acid with a mass fraction of 98% to the beaker dropwise, so that the Ph value of the liquid at 35°C in the beaker is 1.0, and stir slowly; add 213g of concentrated sulfuric acid with a mass fraction of 98% Add 3500 g of 2,4,6-tris(aminocaproate)-1,3,5 triazine solution with a concentration of 0.27mol / kg dropwise into the beaker at the same time, the hydrogen ions in the acid and 2,4,6-tris( The molar ratio of aminocaproic acid salt base)-1,3,5 triazine is 4.5:1, after 90 minutes of dropwise addition, stir for 5 minutes, and the solid-liquid separation of the filtered material; the filter cake is rinsed with 3L of water and drained Finally, 810 g of granular products were obtained, wherein the moisture mass fraction was 50%, and the chloride ion content was 46 mg / kg.
Embodiment 3
[0020] Add 1.5L of tap water at 60°C to a 6L beaker, add concentrated nitric acid with a mass fraction of 98% to the beaker dropwise, so that the Ph value of the 60°C liquid in the beaker is 3.5, and stir slowly; add 182g of concentrated nitric acid with a mass fraction of 98% Add 3500 g of 2,4,6-tris(aminocaproate)-1,3,5 triazine solution with a concentration of 0.27mol / kg dropwise into the beaker at the same time, the hydrogen ions in the acid and 2,4,6-tris( Aminocaproic acid salt base)-1,3,5-triazine molar ratio is 3.0:1, after 90 minutes of dropwise addition, stir for 5 minutes, filter the material with suction to separate the solid from the liquid; rinse the filter cake with 3L of water, pump After drying, 830 g of granular products were obtained, wherein the water mass fraction was 50%, and the chloride ion content was 58 mg / kg.
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Abstract
The invention discloses a production process of granular 2,4,6-tri(amino caproyl)-1,3,5-triazine having low chlorine content, which is characterized in that the production process comprises the steps of: a reaction is carried out by dropping strong acid and a 2,4,6-tri(amino caproate-yl)-1,3,5-triazine solution at the same time into an acid base solution of pH 0.1-3.5, wherein a molar ration of hydrogen ions in the strong acid to 2,4,6-tri(amino caproate-yl)-1,3,5-triazine is 3.0-4.5:1, and the reaction temperature is 15-60 DEG C, solid-liquid separation of materials is carried out after the reaction, a filter cake is washed by water and dried to obtain finished product of granular 2,4,6-tri(amino caproyl)-1,3,5-triazine having low chlorine content. According to the invention, granular 2,4,6-tri(amino caproyl)-1,3,5-triazine can be directly synthesized, solid-liquid separation and washing are easier to perform, the amount of wash water is reduced by lowering chlorine ions content of the product, the discharge amount of waste water is reduced, complex processes in solid-liquid separation of emulsion solution with high viscosity is avoided with the assist of the production process of the invention. Furthermore, the production process of the invention is favorable to industrial production, and has greater significance for environmental protection.
Description
technical field [0001] The invention relates to the technical field of organic synthesis, in particular to the production process of granular low chlorine content 2,4,6-tris(aminocaproyl)-1,3,5 triazine. Background technique [0002] 2,4,6-tris(aminocaproic acid group)-1,3,5 triazine belongs to organic amine carboxylic acid compound, it can protect various metals from rusting, excellent hard water stability, very low foam The advantages of tendency and good air release are mainly used to make environmentally friendly water-soluble metal cutting fluids. [0003] Because chloride ions will corrode metals under acidic conditions, the content of chloride ions in metal cutting fluids is required to be low. It is generally required that the chloride ion content in 2,4,6-tris(aminocaproic acid)-1,3,5 triazine be less than 150mg / kg. [0004] Chinese invention patent application CN101973949A introduces a preparation method of 2,4,6-tris(aminocaproyl)-1,3,5-triazine, which uses hydr...
Claims
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Application Information
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