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Catalyst for catalyzing amine salt conversion, preparation method of the catalyst and preparation method of DAM

A technology for catalyzing amine salts and catalysts, which is applied in the field of preparation of diamines and polyamines. It can solve problems such as environmental protection discharge or recycling pressure, corrosion of acid-resistant equipment, and long-term stable operation of devices, so as to reduce activation energy and disperse Uniform, excellent catalytic effect

Active Publication Date: 2020-11-10
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, due to the addition of caustic soda, a large amount of waste brine containing organic amines is produced, which also causes great pressure on environmental protection discharge or recycling
Moreover, due to the particularity of the neutralization reaction, if the amount of caustic soda added is insufficient or the control is unstable, the excessively acidic reaction liquid will cause corrosion to the downstream equipment that is not resistant to acid, affecting the long-term stable operation of the device

Method used

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  • Catalyst for catalyzing amine salt conversion, preparation method of the catalyst and preparation method of DAM
  • Catalyst for catalyzing amine salt conversion, preparation method of the catalyst and preparation method of DAM

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Embodiment 1: the preparation of 1# catalyst

[0067] a) Preparation of nano-TiO 2 Carrier: Measure 24 mL of butyl titanate into a 1000 mL three-neck flask, add a mixed solution of 150 mL of ethanol and 150 mL of pure water, then add 30 mL of acetic acid, and stir for 10 min at 25°C and 300 r / min. Measure 180mL of ethanol solution containing 20wt% urea, slowly add it into the flask at a rate of 3.6mL / min, keep stirring at 300r / min, and heat the solution in the flask to 160°C at a heating rate of 10°C / min and maintain 160°C, after the addition of the urea-ethanol solution, cool to 50°C after 8 minutes, separate the precipitate, and use absolute ethanol to ultrasonically clean it 5 times, each time using 20mL of ethanol. Then the cleaned solid was dried in an oven at 160°C for 40min, and then calcined in a muffle furnace at 320°C for 2h to obtain TiO with an average particle size of 15nm. 2 carrier.

[0068] b) Loading active components: weigh 1.96g praseodymium nitrat...

Embodiment 2

[0069] Embodiment 2: the preparation of 2# catalyst

[0070] a) Preparation of nano-TiO 2 Carrier: Measure 20 mL of butyl titanate into a 1000 mL three-necked flask, add a mixed solution of 150 mL of ethanol and 150 mL of pure water, then add 40 mL of acetic acid, and stir for 10 min at 25°C and 300 r / min. Measure 180mL of ethanol solution dissolved with 18wt% urea, slowly add it into the flask at a rate of 3.6mL / min, keep stirring at 300r / min, and heat the solution in the flask to 160°C at a heating rate of 10°C / min and maintain 160°C, after the addition of the urea-ethanol solution, cool to 50°C after 6 minutes, separate the precipitate, and use absolute ethanol to ultrasonically clean it 3 times, each time using 30mL of ethanol. Then the cleaned solid was dried in an oven at 160°C for 50min, and then calcined in a muffle furnace at 320°C for 2.5h to obtain TiO with an average particle size of 48nm. 2 carrier.

[0071] b) Loading active components: weigh 2.45g praseodymiu...

Embodiment 3

[0072] Embodiment 3: the preparation of 3# catalyst

[0073] a) Preparation of nano-TiO 2 Carrier: Measure 42 mL of butyl titanate into a 1000 mL three-necked flask, add a mixed solution of 150 mL of ethanol and 150 mL of pure water, then add 30 mL of acetic acid, and stir for 10 min at 25°C and 300 r / min. Measure 180mL of ethanol solution containing 22wt% urea, slowly add it into the flask at a rate of 3.6mL / min, keep stirring at 300r / min, and heat the solution in the flask to 160°C at a heating rate of 10°C / min and maintain 160°C, after the addition of the urea ethanol solution, cool to 50°C after 10 minutes, separate the precipitate, and use absolute ethanol to ultrasonically clean it 3 times, each time using 40mL of ethanol. Then the cleaned solid was dried in an oven at 160°C for 40min, and then calcined in a muffle furnace at 320°C for 3h to obtain TiO with an average particle size of 29nm. 2 carrier.

[0074] b) Loading active components: weigh 2.94g praseodymium nit...

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Abstract

The invention relates to a catalyst for catalyzing amine salt conversion and a preparation method thereof, and a preparation method of DAM. The catalyst comprises a carrier and active components whichcomprise following four components: praseodymium oxide, cuprous oxide, chromium sesquioxide and tin oxide. The preparation method of the DAM comprises the following steps: (a) mixing aniline acid salt with a formaldehyde solution and performing a condensation reaction; (b) transferring H<+> in salified-state amino groups on diphenylmethane series diamine and polyamine in the reaction solution prepared in the step (a) to amino groups of aniline existing in a molecular form in the reaction solution prepared in the step (a) by adopting the catalyst, so that the diamine and the polyamine in the reaction solution are converted into the molecular form; and (c) carrying out phase splitting on the reaction liquid obtained in the step (b). According to the method disclosed by the invention, the manufacturing cost of diphenylmethane series diamine and polyamine (DAM) and the yield of effluent brine are remarkably reduced, and meanwhile, the stable quality of the DAM is ensured.

Description

technical field [0001] The invention relates to the technical field of preparation of diphenylmethane series diamines and polyamines, and mainly relates to a catalyst for catalyzing the conversion of amine salts and a preparation method thereof, and a preparation method of DAM. Background technique [0002] MDI is one of the main raw materials in the polyurethane industry. It is a well-known method in the industry to prepare polymethylenepolyphenylpolyamine (DAM) by reacting aniline and formaldehyde under an acidic catalyst, and then to react DAM with phosgene to synthesize MDI. [0003] In the traditional preparation process of diphenylmethane series diamines and polyamines (DAM), aniline and formaldehyde are condensed under the action of an acid catalyst to obtain diphenylmethane series containing diamines and polyamines (DAM) The acidic reaction mixture, and then completely neutralize the reaction solution containing DAM salt by lye, and separate into an organic phase an...

Claims

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Application Information

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IPC IPC(8): B01J23/86B01J35/02B01J35/10C07C209/78C07C209/84C07C211/50
CPCB01J23/002B01J23/868C07C209/78C07C209/84B01J2523/00B01J35/40B01J35/61B01J2523/17B01J2523/3718B01J2523/43B01J2523/47B01J2523/67C07C211/50Y02P20/52
Inventor 李永锋邢津铭章靓吴雪峰张宏科陈良进崔成成
Owner WANHUA CHEM GRP CO LTD
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