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Metal supported MOFs catalyst as well as preparation method and application thereof to PMDPTA synthesis

A catalyst and metal technology, applied in the field of metal-loaded MOFs catalyst and its preparation, can solve the problems of complex and difficult synthesis process, easy oxidation and storage, etc., and achieve the effect of simple preparation method, low cost, and green production rate

Active Publication Date: 2018-03-09
ZHENXING FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the W-3 type Raney Ni catalyst still has defects such as complicated synthesis process, easy oxidation and difficult storage.

Method used

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  • Metal supported MOFs catalyst as well as preparation method and application thereof to PMDPTA synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 0.016g of palladium chloride in 5mL of acetone to prepare a homogeneous palladium chloride in acetone solution; add the solution dropwise to 10g of activated MIL-101 and disperse it in 50mL of acetone, stir at room temperature for 24h, and filter to obtain the precursor; body placed in a quartz boat, in H 2 0.1%Pd / MIL-101 catalyst was obtained after reduction under atmosphere for 2h.

Embodiment 2

[0032] N,N-bis(2-cyanoethyl)methylamine (30mL), ethanol (150mL), sodium hydroxide (0.18g) and the catalyst (6g) prepared in Example 1 were added in a 300mL autoclave, and the After the kettle is sealed, the air in the kettle is replaced with nitrogen, three times and then replaced with hydrogen three times. The reaction mixture was reacted at a pressure of 2.0 MPa, a rotational speed of 500 rpm and a temperature of 90° C. for 6 h, and the reaction was stopped. After cooling down to room temperature, the mixture was suction-filtered, and the filtrate was concentrated to obtain 13.5 g of N,N-bis(3-aminopropyl)methylamine, with a yield of 45.0%.

[0033] N,N-bis(3-aminopropyl)methylamine (14.5g), methanol (150mL), formaldehyde solution (40.6g) and the catalyst (3g) prepared in Example 1 were added in a 300mL autoclave, and the After the kettle is sealed, the air in the kettle is replaced with nitrogen, three times and then replaced with hydrogen three times. The reaction mixtur...

Embodiment 3

[0035] Dissolve 0.16 palladium nitrate in 25 mL of acetone to prepare a homogeneous palladium nitrate in acetone solution; add the solution dropwise to 10 g of activated MIL-101 and disperse it in 50 mL of acetone, stir at room temperature for 24 hours, and filter to obtain the precursor; place the precursor in Quartz boat, the H 2 1%Pd / MIL-101 catalyst was obtained after reduction under atmosphere for 2h.

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Abstract

The invention provides a metal supported MOFs catalyst as well as a preparation method and application thereof to PMDPTA synthesis and specifically relates to the technical field of catalysts. The catalyst comprises a carrier and an active component; the carrier is an MOFs material; and the active component is single metal or a composite metal particle. The catalyst is prepared by using an excessimpregnation method comprising the steps: stirring at least one solution in metal chloride or metal nitrate and the MOFs material at room temperature for 24h, and carrying out suction filtration to obtain a catalyst precursor; and making the catalyst precursor and a reducing agent generate an effect to obtain the metal supported MOFs catalyst. The preparation method of the catalyst has the advantages such as simple preparation process and stable structure. The catalyst is used for synthesizing PMDPTA and has the advantages such as low cost, high product yield, greenness and environment friendliness.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a metal-loaded MOFs catalyst, a preparation method thereof, and an application in PMDPTA synthesis. Background technique [0002] Polyurethane (PU) is a kind of high molecular polymer containing carbamate group (-NH-CO-O-) in the molecule, which occupies an important position in many fields such as shipbuilding, construction, electromechanical, and light industry. Most common polyurethane materials exist in the form of foam. Polyurethane foam is formed by gradual polymerization of dibasic or polyisocyanate and polyol compound under the action of a catalyst. Among them, the catalyst can not only accelerate the reaction, but also control the speed of the reaction, affect the fluidity of the reaction mixture and the physical and chemical properties of the product, thus playing a vital role in the formation of polyurethane foam. The more commonly used catalysts include organometa...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C209/60C07C211/14
CPCB01J31/1691C07C209/48C07C209/60C07C253/30C07C211/14C07C255/24
Inventor 柯友斌张晓静
Owner ZHENXING FINE CHEM CO LTD
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