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Compounding method for 4,4'-diaminodiphenylmethane

A technique for the synthesis of diaminodiphenylmethane, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of high industrial production costs, limited application range, harsh reactions, etc. Short, simple process, safe production effect

Inactive Publication Date: 2016-02-03
高大元
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem mainly solved by the present invention: there are many synthesis methods for 4,4'-diaminodiphenylmethane and its derivatives at present, but there are still limited application range, harsh reaction, long cycle and industrial production cost in the synthesis process High problem, providing a synthetic method of 4,4'-diaminodiphenylmethane

Method used

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  • Compounding method for 4,4'-diaminodiphenylmethane

Examples

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example 1

[0022] First, put 150g of nitrobenzene into the reaction kettle, add 200mL of formaldehyde solution with a mass fraction of 45% to it, heat up to 85°C with sealing, and the pressure rises to 1.2MPa. After stirring and reacting for 30min, slowly add 80mL of % hydrogen chloride solution and 30mL sulfuric acid solution with a mass fraction of 70%, keep the temperature constant, continue to stir for 30min, cool down to 25°C, and obtain p-nitrobenzaldehyde after filtration; then take 100g of phenol and put it into the , condensing tube, dropping funnel and thermometer in the four-necked flask, slowly drop 50mL of HNO with a mass concentration of 62% in the form of dropwise addition 3 solution and 30 mL of 70% H 2 SO 4 The solution was added dropwise within 30 minutes, then stirred evenly, heated to 105°C in a water bath, sealed with nitrogen, and the air in the container was discharged. After 15 minutes of reaction, the four-neck bottle was moved to an ice bath. Lower the tempera...

example 2

[0025] First, put 180g of nitrobenzene into the reaction kettle, add 230mL of formaldehyde solution with a mass fraction of 45% to it, seal the temperature to 90°C, and raise the pressure to 1.3MPa. After stirring for 40min, slowly add 83mL of a 35% formaldehyde solution % hydrogen chloride solution and 35mL sulfuric acid solution with a mass fraction of 70%, keep the temperature constant, continue to stir for 40min, cool down to 28°C, and obtain p-nitrobenzaldehyde after filtration; then take 130g phenol and put it into a , condensing tube, dropping funnel and thermometer, slowly drop 70mL of HNO with a mass concentration of 62% in the form of dropwise addition 3 solution and 35 mL of 70% H 2 SO 4The solution was added dropwise within 35 minutes, then stirred evenly, heated to 110°C in a water bath, sealed with nitrogen, and the air in the container was discharged. After 18 minutes of reaction, the four-necked bottle was moved to an ice bath. Lower the temperature to 7°C an...

example 3

[0028] First, put 200g of nitrobenzene into the reaction kettle, add 250mL of formaldehyde solution with a mass fraction of 45% to it, seal the temperature to 100°C, and raise the pressure to 1.5MPa. After stirring for 50min, slowly add 85mL of a 35% formaldehyde solution. % hydrogen chloride solution and 40mL sulfuric acid solution with a mass fraction of 70%, keep the temperature constant, continue to stir for 50min, cool down to 30°C, and obtain p-nitrobenzaldehyde after filtration; then take 150g of phenol and put it into the , condensing tube, dropping funnel and thermometer, slowly drop 80mL of HNO with a mass concentration of 62% in the form of dropwise addition 3 solution and 40 mL of 70% H 2 SO 4 The solution was added dropwise within 40 minutes, then stirred evenly, heated to 115°C in a water bath, sealed with nitrogen, and the air in the container was exhausted. After 20 minutes of reaction, the four-necked bottle was moved to an ice bath. Lower the temperature to...

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Abstract

The invention discloses a compounding method for 4,4'-diaminodiphenylmethane and belongs to the technical field of organic compounding. The compounding method comprises the following steps: firstly, adding formaldehyde solution, hydrogen chloride solution and sulfuric acid solution into nitrobenzene, thereby generating p-nitrobenzaldehyde; adding HNO3 solution and H2SO4 solution into phenol, and then uniformly stirring, and performing water bath temperature rise and ice bath temperature decrease, thereby acquiring p-nitrophenol; mixing p-nitrobenzaldehyde and p-nitrophenol which are acquired at two times, and adding Fe, thereby further generating 4,4'-dinitrobenzene methyl alcohol; lastly, adding zinc powder and hydrogen peroxide solution into acquired 4,4'-dinitrobenzene methyl alcohol, performing centrifugal separation, distilling and drying, thereby acquiring 4,4'-diaminodiphenylmethane. The embodiment proves that the method has a certain universality, the reaction is mild, the technique is simple, the requirement for production equipment is low and the yield of prepared 4,4'-diaminodiphenylmethane reaches more than or equal to 85%.

Description

technical field [0001] The invention discloses a synthesis method of 4,4'-diaminodiphenylmethane, which belongs to the technical field of organic synthesis. Background technique [0002] 4,4'-Diaminodiphenylmethane derivatives are an important class of organic synthesis intermediates, mainly used in the production of polyisocyanate compounds, curing agents for epoxy resins, chain extenders for polyurethane elastomers and antioxidants for rubber agent etc. At the same time, 4,4'-diaminodiphenylmethane derivatives are also important fine chemical products and can be used as detection reagents for tungsten. [0003] There are many synthetic methods of 4,4'-diaminodiphenylmethane and its derivatives, which are usually realized through the condensation of N,N-dialkylaniline and formaldehyde, and the reaction of diphenylmethanediamine and dimethyl carbonate. For example, the patent application No. 200810054844.9 "A Method for Heterogeneously Synthesizing 4,4'-Tetramethyldiaminod...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/50
Inventor 高大元张帆
Owner 高大元
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