Method for preparing toluene diamino butyl formate
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A technology of butyl toluene dicarbamate and toluene diamine, which is applied in the field of preparation of butyl toluene dicarbamate, can solve the problems of difficult separation of catalysts, easy deactivation of catalysts, and impact on production costs, so as to avoid adverse effects and reuse Good performance and lower production cost
Inactive Publication Date: 2012-09-12
HEBEI UNIV OF TECH
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[0006] In the above-mentioned existing literature reports that directly utilize toluene diamine, urea and butanol to synthesize butyl toluene dicarbamate, a multi-stage reaction is adopted, the catalyst used is not environmentally friendly, the catalyst is easily deactivated when exposed to the environment, or the catalyst is used as a
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Embodiment 1
[0022] Add 0.095mol 2,6-toluenediamine, 0.19mol urea, 0.95mol n-butanol, and 0.580g Hβ molecular sieve roasted at 300°C to the reactor in sequence, then seal the reactor, and heat it to the temperature of The reaction was carried out at 130°C for 10 hours. After the reaction, the temperature was lowered, the material was discharged, and the catalyst was separated by filtration at 30°C. The composition of the filtrate was analyzed by high performance liquid chromatography, and the yield of the product butyl toluene dicarbamate was 3.5%.
Embodiment 2
[0024] In the reactor, add 0.02mol molar ratio of 2,4-diaminotoluene: 2,6-diaminotoluene=80:20 mixture, 0.08mol urea, 1.4mol n-butanol, 0.732g roasted at 400°C HY molecular sieve, then seal the reaction kettle, under the condition of stirring, heat to 170°C to react, react for 1 hour, after the reaction, cool down, discharge, filter and separate the catalyst at 50°C, and analyze the filtrate with high performance liquid chromatography Composition, the measured yield of product butyl toluene dicarbamate is 25.0%.
Embodiment 3
[0026] 0.03mol molar ratio of 2,4-diaminotoluene: 2,6-diaminotoluene=65:35 mixture, 0.18mol urea, 1.5mol n-butanol, 1.098g roasted γ-Al 2 o 3 Catalyst, then seal the reaction kettle, under stirring condition, be heated to the temperature and react under 190 ℃, react for 6 hours, cool down after the reaction finishes, discharge, and filter and separate the catalyzer at 80 ℃, analyze the filtrate composition with high performance liquid chromatography, The yield of the product butyl toluene dicarbamate was measured to be 62.8%.
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Abstract
The invention relates to a method for preparing toluene diamino butyl formate, which comprises the following steps: adding toluene diamine, urea, butanols and a catalyst in a reaction vessel, wherein the mol ratio of the reaction components is characterized in that toluene diamine to urea to butanols is 1:2-10:10-90, and the catalyst amount accounts for 5%-60% of mass of toluene diamine, sealing the reaction vessel after charging, under the stirring condition, heating to the temperature of 130-250 DEG C for reacting for 1-10 hours, cooling after finishing the reaction, discharging, filtering and separating the catalyst at the temperature of 30-90 DEG C to obtain the products toluene diamino butyl formate. No material addition and removal is provided during the reaction period, the operation is convenient by only requiring reaction temperature control; the reaction condition is mild; the used catalyst has the advantages of low price, high catalytic activity and high yield of the product as high as 81.8%; the catalyst and the reacted material are easy to be separated, the catalyst enables no deactivation and good repetitive usability.
Description
technical field [0001] The invention belongs to a method for preparing phenylcarbamate by urea catalytic reaction, in particular to a method for preparing butyl toluene dicarbamate by catalytic reaction of toluene diamine, urea and butanol. Background technique [0002] Toluene dicarbamate is an important organic compound, which can be used as pesticide and medicine, more importantly, as an intermediate for the synthesis of toluene diisocyanate (TDI), and toluene diisocyanate is an important raw material for the preparation of polyurethane. The traditional TDI production adopts the phosgene method, which has disadvantages such as the highly toxic raw material phosgene, the corrosion of equipment by the by-product hydrochloric acid, and the difficulty in removing residual chlorine in the product. At present, the non-phosgene route has become the focus of domestic and foreign researchers, and various non-phosgene synthesis methods for TDI have been reported in a large number o...
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