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Modified catalyst, preparation method thereof and method for preparing N,N-dimethyl-1,3-propanediamine

A catalyst and modification technology, applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of increasing operating risks and equipment investment, rapid deactivation of catalysts, and difficulty in disposal of waste liquids. Improve product selectivity and conversion, reduce deamination side reactions, and reduce the effect of adsorption capacity

Active Publication Date: 2020-11-03
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patents CN 101321722 A and CN 100369886C all disclose the method for the production of DMAPA by the batch method. The hydrogenation reaction adopts Raney nickel catalyst, and the caustic alkali aqueous solution of 12-16% of the catalyst mass is added as the inhibitor in the reaction, which is easy to cause Corrosion of equipment and difficult disposal of waste liquid
However, the catalyst has high requirements on the purity of the raw material DMAPN, and the 2-(dimethylaminomethyl)glutaronitrile in the raw material will cause rapid deactivation of the catalyst. In addition, the reaction also requires the introduction of a large amount of liquid ammonia as an inhibitor, which increases the risk of operation and equipment investment

Method used

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  • Modified catalyst, preparation method thereof and method for preparing N,N-dimethyl-1,3-propanediamine
  • Modified catalyst, preparation method thereof and method for preparing N,N-dimethyl-1,3-propanediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) Preparation of O-LDH modified hydrotalcite carrier:

[0051] Firstly, N-100 magnesium aluminum hydrotalcite was calcined in air atmosphere at 500℃ for 2h to prepare MgAl-LDO. In addition, 2.0 g of triethylenediamine was dissolved in 500 mL of deionized water, 200 g of the above-prepared MgAl-LDO was added, stirred at room temperature for 15 h for intercalation modification of bifunctional organics, and filtered and dried to obtain triethylenediamine-modified carrier O -LDH.

[0052] (2) Co-Cu / O-LDH catalyst precursor preparation:

[0053] 266g Co(NO 3 ) 2 ·6H 2 O and 20.5g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 1L deionized water, and 200 g of the modified carrier O-LDH prepared in step (1) was gradually added under stirring conditions, stirred at room temperature for 12 h, and dried at 100 °C for 6 h after standing still. Put the dried solid in a muffle furnace, raise the temperature to 300° C. at a rate of 3° C. / min, and keep it for 6 hours to obtain catalys...

Embodiment 2

[0060] (1) Preparation of O-LDH modified hydrotalcite carrier:

[0061] Dissolve 153.6g of magnesium nitrate hexahydrate and 80.7g of ferric nitrate nonahydrate in 2L of deionized water, quickly drop 2M NaOH lye to adjust the pH of the solution to 12, stir at 500rpm and 150°C for 2h, filter and After drying at ℃ for 12 hours, the magnesium iron hydrotalcite MgFe-LDH was obtained.

[0062] Then the MgFe-LDH was calcined in an air atmosphere at 450°C for 2h to prepare MgFe-LDO. In addition, 12 g of adipamide was dissolved in 1 L of deionized water, and 200 g of the above-prepared MgFe-LDO was added, stirred at room temperature for 15 h to carry out intercalation modification of bifunctional organic matter, filtered and dried to obtain the adipamide-modified carrier O- LDH.

[0063] (2) Co-Cu / O-LDH catalyst precursor preparation:

[0064] 123.3g Co(NO 3 ) 2 ·6H 2 O and 19.0g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 1L deionized water, and 200 g of the modified carrier O-LDH ...

Embodiment 3

[0070] (1) Preparation of O-LDH modified hydrotalcite carrier:

[0071] Firstly, N-100 magnesium aluminum hydrotalcite was calcined in an air atmosphere at 500°C for 3h to prepare MgAl-LDO. In addition, 6.8 g of 2,6-toluenediamine was dissolved in 1 L of deionized water, 200 g of the above-prepared MgAl-LDO was added, stirred at room temperature for 12 hours for intercalation modification of bifunctional organics, and filtered and dried to obtain 2,6-toluenediamine-modified Sex carrier O-LDH.

[0072] (2) Co-Ni / O-LDH catalyst preparation:

[0073] 98.7g Co(NO 3 ) 2 ·6H 2 O and 6.6g Ni(NO 3 ) 2 ·6H 2 O was dissolved in 1 L of deionized water, and 200 g of the modified carrier O-LDH prepared in Example 3 was gradually added under stirring conditions, stirred at room temperature for 12 h, and dried at 100 °C for 6 h after standing still. Put the dried solid in a muffle furnace, raise the temperature to 300° C. at a rate of 3° C. / min, and keep it for 6 hours to obtain cata...

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Abstract

The invention discloses a modified catalyst, a preparation method thereof and a method for preparing N,N-dimethyl-1,3-propanediamine. The catalyst comprises an active component and a bifunctional organic matter modified carrier, the general formula of the catalyst is M / O-LDH, M represents the active component, and O-LDH represents the bifunctional organic matter modified hydrotalcite carrier; thehydrotalcite carrier is modified by a bifunctional organic matter. The modified catalyst provided by the invention is used for preparing DMAPA through DMAPN hydrogenation. The DMAPA prepared by adopting the catalyst has few side reactions, the DMAPA can be prepared with high selectivity without adding liquid ammonia or caustic alkali as an inhibitor, and the catalyst is high in activity and long in service lifetime.

Description

technical field [0001] The invention relates to the field of organic catalysis, and more specifically relates to a modified catalyst, a preparation method thereof, and a method for preparing N,N-dimethyl-1,3-propanediamine. Background technique [0002] N,N-Dimethyl-1,3-propanediamine (hereinafter referred to as DMAPA) is one of the important varieties of aliphatic amine compounds and an important intermediate of organic raw materials. It is widely used in daily chemicals, pesticides, dyes, resins, etc. widely used. At present, most of DMAPA in China is mainly used to prepare betaine and amidopropyl dimethylamine, which are used in daily chemical products such as shampoo, shower gel, baby shower gel, hair conditioner, liquid soap and detergent. In addition, DMAPA is also used as a polyurethane catalyst, epoxy resin curing agent and accelerator, and the production of dyes. The mainstream synthetic route of DMAPA is: (1) using dimethylamine and acrylonitrile as raw materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J31/04C07C209/48C07C211/09
CPCB01J31/0254B01J31/0202B01J31/04C07C209/48B01J2231/641C07C211/09
Inventor 姜瑞航张聪颖刘振国张立娟刘志鹏杨晓坤
Owner WANHUA CHEM GRP CO LTD
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