Synthesizing method of 3,3'-dimethyl-4,4'-diamido-dicyclohexyl methane
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A technology of diaminodicyclohexylmethane and diaminodicyclohexyl is applied in the field of fine chemical synthesis, which can solve the problem of high equipment requirements, and achieve the effects of prolonging the process cost, eliminating waste of resources and having good reaction atom economy.
Inactive Publication Date: 2011-04-27
JIANGSU QINGQUAN CHEM CO LTD +1
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Embodiment 1
[0030] Example 1 Put 226g MDT, 226g MACM, 11.3g Ru / SiO into the hydrogenation kettle 2 , and add 0.11g CaO, and replace with nitrogen and hydrogen after feeding. Start stirring, raise the temperature to 120°C, and control the temperature between 120-140°C and the pressure between 2.0-4.0MPa. The hydrogen absorption is completed after 32 hours of reaction, continue to keep warm for 2 hours, cool to 40°C, discharge, filter, Then product is distilled under 10mmHg vacuum, obtains product 219g, content 99.6%, yield 92%.
Embodiment 2
[0031] Example 2 Put 226g MDT, 226g MACM, 11.3g Ru / SiO into the hydrogenation kettle 2, and add 0.09gBaO, and replace with nitrogen and hydrogen after feeding. Start stirring, raise the temperature to 135°C, and control the temperature between 140-160°C and the pressure between 2.0-4.0MPa. After 22 hours of reaction, the hydrogen absorption is completed, continue to keep warm for 1.5h, cool to 40°C, discharge, and filter , Then distill the product under 10mmHg vacuum, obtain product 226.6g, content 99.5%, yield 99.5%.
Embodiment 3
[0032] Example 3 Put 226g MDT, 271g MACM, 18.1g Ru / SiO in the hydrogenation kettle 2 , and add 0.12gMgO, and replace with nitrogen and hydrogen after feeding. Start stirring, raise the temperature to 135°C, and control the temperature between 140-160°C and the pressure between 4.0-6.0MPa. The hydrogen absorption is completed after 17 hours of reaction, continue to keep warm for 2.5h, cool to 40°C, discharge, and filter , Then distill the product under 10mmHg vacuum, obtain product 236.1g, content 99.7%, yield 99.2%.
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Abstract
The invention relates to a synthesizing method of 3,3'-dimethyl-4,4'-diamido-dicyclohexyl methane (MACM), belonging to the technical field of fine chemical synthesis. The synthesizing method comprises the following steps of: placing the MACM and 3,3'-dimethyl-4,4'-diamido-diphenyl methane (MDT) in a hydrogenation kettle according to the ratio of 1.0:(1.0-4.0), adding a Ru compound catalyst, adding trace alkaline earth metal assistant, performing hydrogenation reaction at the temperature of 120-190 DEG C and the pressure of 2.0-10.0MPa, cooling, discharging and filtering and rectifying to obtain pure MACM product. The invention has the advantages of low reaction temperature, low pressure, low requirement for devices, easy and simple operation, good product purity, high yield, good economical efficiency of reaction atom and no process waste water and gas in the whole technical process, technically and greatly reduces the generation source of three wastes, is environmental-friendly and has better industrial application prospect.
Description
technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a synthesis method of 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane. Background technique [0002] 3,3'-Dimethyl-4,4'-diaminodicyclohexylmethane is widely used in the synthesis of high-quality polyurethane, epoxy resin and polyamide, such as aerospace industry, wind power generation and other industries. The polyurethane synthesized by MACM not only has the elasticity of rubber, but also has the strength of plastic and excellent processing performance, especially in terms of sound insulation, heat insulation, wear resistance, oil resistance, elasticity, etc. It has non-toxic, light weight, excellent mechanical strength, wear resistance and good corrosion resistance; when applied to epoxy resin, it has a series of excellent properties such as strong adhesion, excellent electrical insulation, stable chemical properties and good processing p...
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