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A technology of diisopropylamine and diisopropyl, which is applied in the field of chemical synthesis, can solve the problems of high reaction temperature, complex process operation, high risk, etc., and achieve the effect of high yield and simple process
Inactive Publication Date: 2009-11-25
HANGZHOU XINDE ENVIRONMENTAL PROTECTION TECH
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[0004] 1) Add ethylene oxide to the ethanol solution of diisopropylamine. After the absorption, the finished product is collected by fractional distillation. The reaction temperature of this route is high, and the material loss is large, it is difficult to control, and it is dangerous
[0005] 2) Add chloroethanol dropwise to the diisopropylamine solution, after the addition, react at 100°C for 8 hours, then neutralize, layer, extract, and fractionate to obtain the finished product. This route takes a long time to rea...
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Embodiment 1
[0016] Embodiment 1: the synthetic method of this diisopropyl ethyl (alcohol) amine
[0017] (1) Using diisopropylamine and ethylene oxide as raw materials, zinc chloride and tetramethylammonium hydroxide as catalysts, and water as a circulating medium for reaction aging.
[0018] (2), the reaction is carried out in two phases of gas and liquid, and it is produced in a single kettle. The specific operating conditions are pressure: normal pressure, temperature: 50-180 ° C, ethylene oxide gas space velocity: 50-100kg / h, diisopropylamine: ethylene oxide molar ratio is 1-1.5, catalyst dosage: 0.5-1 weight of diisopropylamine.
[0019] (3) Diisopropylamine is weighed into the reaction kettle, and then put into the prepared catalyst. After fully mixing, the mixing temperature is controlled to be normal temperature, and ethylene oxide is introduced at normal temperature and pressure according to the specified flow rate, and the heat preservation reaction is completed. After two hou...
Embodiment 2
[0020] Embodiment 2: make according to the method described in embodiment 1
[0021] Table 1 Reaction and aging conditions of diisopropylamine and ethylene oxide
[0022]
[0023] Note: EO is ethylene oxide, DEA is diisopropylamine, APHA is the color standard unit
[0024] It can be known from Table 1 that the reaction temperature of ethylene oxide and diisopropylamine is 180°C. After the reaction, it can be aged at 210-250°C for 6-12 hours. From example 6 and example 7 of table 1, it can be seen that after the reaction, without aging treatment, although it can also be separated by distillation, the product obtained is except that the color is dark, and the standing time is also short.
Embodiment 3
[0025] Embodiment 3: make according to the method described in embodiment 1
[0026] Table 2 Process conditions and reaction results of water as circulating solution
[0027]
[0028] As can be seen from Table 2, water can be used as a circulating solution to obtain a high conversion rate of material ethylene oxide and a high selectivity of diisopropyl ethyl (alcohol) amine.
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Abstract
The invention relates to a method for synthetizing N,N-diisopropylethylamine; the method comprises the steps as follows: taking diisopropylamine, epoxy ethane as the raw material, taking zinc chloride, tetramethyl ammonium hydroxide as the catalyst, taking the water as the circulating medium, reacting and aging; the reaction is carried out under gas and liquid phases utilizing single kettle production; the specific operating conditions being normal pressure, the temperature being 50 to 180 degrees centigrade, the air speed of ethylene oxide gas being 50 to 100 kg/h, the mol ratio between diisopropylamine and epoxy ethane being 1-1.5, the dosage of the catalyst being 0.5-1 weight of diisopropylamine; thermal reacting for two hours, then discharging and filtering to remove the solid catalyst, evaporating diisopropylamine and moisture under normal pressure, adding with activated carbon dipping with Ru, Pt or Pd elements, decompressing, rectifying, collecting the products. The invention has the advantages of taking the water solution of the diisopropylamine as the main reaction line, adding with little catalyst into the water solution of the diisopropylamine, and reacting through the epoxy ethane under normal pressure, having excellent reaction effect.
Description
technical field [0001] The invention relates to a chemical synthesis method, mainly a synthesis method of N, N-diisopropyl ethyl (alcohol) amine using diisopropylamine as a raw material. Background technique [0002] N, N-diisopropyl ethyl (alcohol) amine is a widely used organic synthesis intermediate, and is the main raw material for synthesizing pesticide synergists (the synergist and pesticides are mixed, which can improve the insecticidal effect and reduce environmental pollution), and can also be used as an intermediate for the synthesis of dyes, pigments, surfactants, and pesticides, as well as raw materials for the production of stabilizers, preservatives, vulcanization accelerators, antioxidants, flotation agents, and emulsifiers. The current synthetic method has low equipment investment, low conversion rate, poor selectivity and high production cost. [0003] At present, the synthetic method of N, N-diisopropyl ethyl (alcohol) amine mainly contains following four ...
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