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Metal ruthenium monatomic catalyst for catalyzing hydrochlorination reaction of acetylene as well as preparation method and application of metal ruthenium monatomic catalyst

A technology of acetylene hydrochlorination and catalyst, which is applied in the direction of catalyst activation/preparation, organic compound/hydride/coordination complex catalyst, catalytic reaction, etc. It can solve the problems of easy agglomeration and poor dispersion of active components, and achieve Not easy to lose and agglomerate, improve atom utilization, improve catalytic activity and stability

Active Publication Date: 2021-07-27
新疆聚耕农业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, one of the most important reasons for the deactivation of Ru / AC catalysts prepared with ruthenium trichloride trihydrate as a precursor during the reaction process is the poor dispersion of the active components and the tendency to agglomerate during the reaction process.

Method used

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  • Metal ruthenium monatomic catalyst for catalyzing hydrochlorination reaction of acetylene as well as preparation method and application of metal ruthenium monatomic catalyst
  • Metal ruthenium monatomic catalyst for catalyzing hydrochlorination reaction of acetylene as well as preparation method and application of metal ruthenium monatomic catalyst
  • Metal ruthenium monatomic catalyst for catalyzing hydrochlorination reaction of acetylene as well as preparation method and application of metal ruthenium monatomic catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] The preparation method of the metal single-atom catalyst for catalyzing acetylene hydrochlorination is:

[0070] Carrier CN 1 Synthesis:

[0071] Firstly, 1 mL of aniline (0.01097 mol) was dissolved in deionized water containing 1.6 g of silica gel solution (Ludox AM-40, mass concentration: 30%), and 1.2 mol / L hydrochloric acid solution was added to adjust the pH to 3, followed by ultrasonication for 1 h. Add 4 mL of ammonium persulfate aqueous solution (an ammonium persulfate aqueous solution obtained by dissolving 0.52 g of ammonium persulfate, that is, 0.002279 mol of ammonium persulfate in 4 mL of deionized water), sonicate for 1 h and place at room temperature for 18 h to obtain the product. After the product was centrifuged, the precipitate was washed three times with ethanol and deionized water. After washing, centrifuge again, add 1mol / L ammonia water to the precipitate, leave it at room temperature for 18h and then centrifuge, wash the precipitate three times...

Embodiment 2

[0073] The preparation method of the metal single-atom catalyst for catalyzing acetylene hydrochlorination is:

[0074] Carrier CN 2 Synthesis:

[0075] Firstly, 3 mL of aniline (0.03291 mol) was dissolved in deionized water containing 1.6 g of silica gel solution (Ludox AM-40, mass concentration: 30%), and 2 mol / L hydrochloric acid solution was added to adjust the pH to 5, followed by ultrasonication for 2 h. Add 8 mL of ammonium persulfate aqueous solution (an ammonium persulfate aqueous solution obtained by dissolving 1.04 g of ammonium persulfate in 8 mL of deionized water), sonicate for 2 hours and then place at room temperature for 24 hours to obtain the product. After the product was centrifuged, the precipitate was washed 6 times with ethanol and deionized water. After washing, centrifuge again, add 3mol / L ammonia water to the precipitate, leave it at room temperature for 24h and then centrifuge, wash the precipitate three times with deionized water and centrifuge, t...

Embodiment 3

[0077] The preparation method of the metal single-atom catalyst for catalyzing acetylene hydrochlorination is:

[0078] Step 1, synthesis of carrier:

[0079] Adopt the method identical with embodiment 1 and parameter synthetic carrier CN 1 .

[0080] Step 2, ruthenium single-atom catalyst synthesis:

[0081] Take 4.5g carrier CN 1 Dissolve 10mL of aniline (0.1097mol) in nitromethane solution, add 0.2983g of RuCl3 ·3H 2 O (0.001438mol, which contains 0.1454g of Ru atoms) was stirred for 6 hours, then left at room temperature for 12 hours, washed with nitromethane solution for 3 times after centrifugation, and then dried in an oven at 80°C for 12 hours, and placed in a tube furnace at 800°C Roast under an inert gas atmosphere for 3 hours, take out the sample and add a mixed solution of ethanol and sodium hydroxide (volume ratio 1:1, 500 mL in total), stir for 6 hours, leave at room temperature for 12 hours, and centrifuge. After each washing 3 times, the ruthenium single-a...

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Abstract

The invention provides a preparation method of a metal ruthenium monatomic catalyst for catalyzing acetylene hydrochlorination reaction. The method comprises the following steps: dissolving an organic matter containing an amino structure in deionized water containing a silica gel solution, dispersing, adding ammonium persulfate, reacting, removing impurities from the product, drying, roasting, removing impurities after roasting, and obtaining a carrier; dissolving the carrier and a ligand in a low-boiling-point organic solvent, adding ruthenium trichloride trihydrate, carrying out coordination at room temperature, carrying out impurity removal and drying on a product, roasting, and carrying out impurity removal and drying after roasting. The invention also provides application of the catalyst in acetylene hydrochlorination reaction. Compared with the existing carbon-supported metal catalyst for acetylene hydrochlorination reaction, the metal monatomic catalyst has the advantages that the active components are anchored on the surface of the carrier, are in a monatomic dispersion state and are not easy to lose and agglomerate, the atom utilization rate is increased, acetylene and hydrogen chloride reactants are activated, and the catalytic activity and the stability of the existing metal catalyst are greatly improved.

Description

technical field [0001] The invention relates to a metal ruthenium single-atom catalyst for catalyzing acetylene hydrochlorination, a preparation method and application thereof. Background technique [0002] Polyvinyl chloride (PVC) is a polymer material produced by the polymerization of vinyl chloride (VCM). Its global usage ranks third among polymer materials and is widely used in industry, construction, agriculture, daily life and other fields. According to the method of obtaining VCM, it can be divided into acetylene method and ethylene method. Based on the energy characteristics of my country's "rich in coal, poor in oil, and low in gas", the proportion (82%) of the calcium carbide acetylene process with coal as the source far exceeds that of the ethylene process with petroleum resources as the source. However, the calcium carbide acetylene process is now Carbon-supported mercuric chloride is still used as an industrial catalyst to catalyze the hydrochlorination of acety...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J31/18B01J37/03B01J37/08C07C17/08C07C21/06
CPCB01J27/24B01J31/1805B01J37/031B01J37/082C07C17/08B01J2531/821B01J2231/32C07C21/06Y02P20/584
Inventor 张海洋李建张金利谢东阳李林峰蔡明李峰张苗苗姚丽莎代斌
Owner 新疆聚耕农业科技有限公司
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