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Catalytic preparation method of isopropanolamine

A technology of isopropanolamine and catalyst, applied in the field of preparation of isopropanolamine products, can solve problems such as multiple reactors, unfavorable industrialization promotion and application, increase in investment amount of synthetic equipment and complexity of process control, etc. Side reactions, stable and efficient catalysis, the effect of improving yield

Active Publication Date: 2020-12-15
山东达民化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are few by-products in the product obtained by the preparation method, the above preparation method requires multiple reactors, which greatly increases the investment amount of the synthesis equipment and the complexity of process control, which is not conducive to industrialization and application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0057] Preparation of Pd / Au / La-ZSM Catalyst

[0058] S1: Dissolve chloroauric acid and ammonium chloropalladate in deionized water to make solutions with a concentration of 5 mM respectively, and set aside;

[0059] S2: Put 200mL of ZSM-5 zeolite into a beaker, add 500mL of 20% ethanol solution, and add 5M hydrochloric acid to make the hydrochloric acid content about 20g, activate at 40°C for 2 hours;

[0060] S3: Disperse the activated ZSM-5 zeolite in ethanol aqueous solution of mercaptoethylamine, let it stand at 40°C overnight, filter, wash with deionized water 3 times, and dry at 50°C for 4 hours;

[0061] S4: Put the ZSM-5 zeolite obtained in the previous step into the reaction bottle, add 500 mL of deionized water to the bottle, pass nitrogen gas into the reaction bottle for 2 minutes to remove oxygen, add 50 mL of the chloroauric acid solution prepared above and chloropalladium acid Ammonium solution 50mL, incubate under ultrasound for 10min, continue to sonicate, and...

Embodiment 1

[0068] Preparation of isopropanolamine products based on triisopropanolamine

[0069] (S1): 1 kg of liquid ammonia was prepared at room temperature into saturated ammonia water and added to the autoclave, which was filled with 200 g of Pd / Au / La-ZSM catalyst prepared by the method described in Preparation Example 1 and 50 g of montmorillonite in advance. Loaded phosphotungstic acid (Keggin type, tungsten load 0.5wt%) and 35g ammonium carbonate;

[0070] (S2): Close the reactor, pass nitrogen into the reactor to remove the air, pressurize 10.7kg of propylene oxide from the metering tank to 0.15Mpa, then pour it into the reactor from the feed port, raise the temperature to 60°C, and stir for 2 hour; then heat up to 70°C, continue to spray 1.8kg of saturated ammonia water at about 5°C through the atomization spray feeding port, and the spray feeding time is 10-12min. Reaction solution 1;

[0071] (S3): Cool the reaction solution, send the reaction solution 1 to the deamination t...

Embodiment 2

[0074] Same as Example 1, the difference is that the amount of catalyst used in step S1 is: 300g of Pd / Au / La-ZSM catalyst, 110g of phosphotungstic acid supported by montmorillonite, other preparation materials and methods are the same as in Example 1, and the prepared product contains three The content of isopropanolamine is 95.2%.

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Abstract

The invention discloses a Pd / Au / La-ZSM catalyst for preparing isopropanolamine by amination reaction, which takes ZSM-5 zeolite as a carrier and enables metal Pd and metal Au obtained by reduction ofan ammonium chloropalladate and chloroauric acid solution to be stably enriched on the surface of the ZSM-5 zeolite through zeolite activation and surface modification. And after the La is loaded, thereaction for preparing isopropanolamine can be effectively promoted. The invention also discloses a preparation method of isopropanolamine by using the catalyst and the cocatalyst, and in an isopropanolamine product obtained by rectifying the product, the content of triisopropanolamine can reach 90% or above.

Description

technical field [0001] The invention belongs to the technical field of catalyst and chemical product production, and in particular relates to a preparation method of an isopropanolamine product containing a high-content triisopropanolamine component. Background technique [0002] Isopropanolamine and ethanolamine are alkanolamine homologues, both of which can be used as compound synthesis intermediates, processing aids for food industry, and emulsifiers. Isopropanolamine has more excellent properties than ethanolamine, and is less harmful to the environment and humans, and has gradually become a green chemical product. As countries around the world pay more and more attention to environmental issues, the application of ethanolamine is being gradually restricted. For example, the "Pollutant Emission and Transfer Registration System" in developed countries has listed ethanolamine as a harmful substance and restricted its use, thereby accelerating the use of ethanolamine by iso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/44B01J37/16B01J37/18B01J37/02C07C215/08C07C213/04B01J31/18C04B24/12C04B103/52
CPCB01J29/44B01J37/16B01J37/18B01J37/0205C07C213/04C04B24/122B01J2229/186B01J2229/20B01J2229/40B01J2229/37B01J27/188B01J31/1845C04B2103/52B01J35/19C07C215/08
Inventor 于如军陈国华郭文杰
Owner 山东达民化工股份有限公司
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