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Preparation and application of noble metal atom cluster catalyst for acetylene hydrochlorination

A noble metal, atomic cluster technology, applied in metal/metal oxide/metal hydroxide catalyst, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc. problem, to achieve uniform size, prevent agglomeration, and achieve the effect of high yield

Active Publication Date: 2021-01-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Traditional nanoparticle catalysts are polydisperse, which makes it difficult to link the internal structure from the apparent catalytic activity

Method used

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  • Preparation and application of noble metal atom cluster catalyst for acetylene hydrochlorination
  • Preparation and application of noble metal atom cluster catalyst for acetylene hydrochlorination
  • Preparation and application of noble metal atom cluster catalyst for acetylene hydrochlorination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Au 25 (PhC 2 h 4 S) 18 Preparation of / AC catalyst

[0034] Weigh 60 mg of HAuCl 4 4H 2 O was added to a 50mL three-necked flask, and 15mL THF was added, and the solution was golden yellow. Add TOAB 92mg (TOAB: HAuCl 4 4H 2 O=1.16mol:1mol), the solution gradually deepened from golden yellow to orange red. After stirring for 30min, add PhCH 2 CH 2 SH 97μL (PhCH 2 CH 2 SH: HAuCl 4 4H 2 O=5mol:1mol), stirred at 25°C for one hour, added NaBH 4 (4mL ice water) 55mg (NaBH 4 : HAuCl 4 4H 2 O=10mol:1mol). Stir for three hours to stop the reaction. Wash the product with n-hexane and methanol, dissolve the precipitate with dichloromethane, remove insoluble matter, and obtain Au after drying 25 (PhC 2 h 4 S) 18 .

[0035] Activated carbon treated with hydrochloric acid was dispersed with dichloromethane, and Au dissolved in dichloromethane was added dropwise. 25 (PhC 2 h 4 S) 18, stirred overnight at 25°C, and dried by centrifugation to obtain Au 25 / A...

Embodiment 2

[0038] Au 11 (PPh 2 Py) 7 Br 3 Preparation of / AC catalyst

[0039] Weigh 240mgHAuCl 4 and 306mgPPh 2 Py, add 0.0105mL H 2 O, the solvent is ethanol, after stirring at 25°C for 9.5h, washing with ethanol and drying to obtain Au I (PPh 2 Py)Cl. Weigh 40mg [Au I (PPh 2 Py)Cl] and 85 mg tetra-n-octylammonium bromide (TOAB: HAuCl 4 4H 2 O=1.16mol: 1mol) was dissolved in 10mL ethanol and stirred in a round bottom flask (600rpm / min), then NaBH 4 (15.2 mg, NaBH 4 : HAuCl 4 4H 2 O=5mol:1mol) was dissolved in 1mL of ethanol, and slowly added dropwise. After reacting for 12 h, the mixture was poured into 10 mL of water, centrifuged by a centrifuge at 4000 rpm to obtain a black solid, which was washed several times with n-hexane / dichloromethane (v / v=5 / 1) to remove excess PPh 2 Py ligand and TOAB. Finally, the precipitate obtained above was extracted with 2 mL of methanol, centrifuged again (10,000 rpm, 5 min) to remove insoluble matter, and the obtained solution was dri...

Embodiment 3

[0043] Au 144 (C 6 h 13 S) 60 Preparation of / AC catalyst

[0044] Weigh 60 mg of HAuCl 4 4H 2 O was added to a 50mL three-necked flask, and 15mL of methanol was added, and the solution was golden yellow. Add TOAB 92mg (TOAB: HAuCl 4 4H 2 O=1.16mol:1mol), the solution gradually deepened from golden yellow to orange red. After stirring for 30 min, add C 6 h 13 SH 87μL (C 6 h 13 SH: HAuCl 4 4H 2 O=5mol:1mol), stirred at room temperature at 25°C for one hour, added NaBH 4 (4mL ice water) 55mg (NaBH 4 : HAuCl 4 4H 2 O=10mol:1mol). Stir at 25°C for five hours to stop the reaction. Wash the product with methanol, wash with acetone, dissolve the precipitate with dichloromethane, remove insoluble matter, and obtain Au after drying 144 (C 6 h 13 S) 60 .

[0045] Activated carbon treated with hydrochloric acid was dispersed with dichloromethane, and Au dissolved in dichloromethane was added dropwise. 144 (C 6 h 13 S) 60 , stirred overnight at 25°C, and dried ...

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Abstract

The invention provides a noble metal atom cluster and a catalyst; the atom cluster is a noble metal atom cluster structure protected by an organic ligand, the structural formula is An(SR)m or An(PB)mCx, A is noble metal, B is an organic group coordinated with phosphorus (P), and C is halogen; SR is at least one of phenethyl mercaptan, 2-naphthalene mercaptan, hexanethiol or adamantane mercaptan, n=2-200, m=10-200 and x=2-20. Mercaptan and triphenylphosphine (diphenyl-2-pyridylphosphine) are used as protective agents, S and P atoms can well stabilize atom clusters and prevent the atom clustersfrom agglomeration, and the catalyst is excellent in stability, green, environment-friendly and recyclable, and has manipulation in industrial applications.

Description

technical field [0001] The invention relates to a supported noble metal atom cluster catalyst used for acetylene hydrochlorination to synthesize vinyl chloride, a preparation method and application thereof, and belongs to the field of catalyst preparation technology and application in organic synthesis. Background technique [0002] Vinyl chloride, referred to as VCM, is a monomer for the synthesis of polyvinyl chloride (PVC). PVC is one of the five general-purpose resins (PVC, PE, PP, PS and ABS) in the world. It has good physical and mechanical properties and is used in the production of construction, packaging and electronic materials. With the rapid development of the world economy and the continuous improvement of people's living standards, the demand for PVC materials is also increasing year by year. At present, there are mainly three methods for industrial production of vinyl chloride: acetylene method, ethylene method and ethane method. my country is a country with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/18B01J23/52C07C21/06C07C17/08
CPCB01J31/226B01J31/189B01J23/52C07C17/08B01J2531/18B01J2531/0222B01J2231/32B01J35/393B01J35/23C07C21/06
Inventor 李杲李志敏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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