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Activated carbon load single valence state cuprous oxide chloride-free catalyst, preparation method, and application in oxidate oxo synthesis dimethyl carbonate

A technology of cuprous oxide and activated carbon, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carbonate/haloformate, etc., can solve the problem of activity stability, unstable active components, and cannot be prepared Valence state and other issues, to achieve the effect of good stability, single valence state, and stable active components

Inactive Publication Date: 2013-05-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the Wacker-type chlorine-containing catalyst supported by activated carbon has the highest reactivity and selectivity, but because chlorine will be lost during the preparation and reaction process, the catalyst not only has activity stability problems, but the generated hydrogen chloride will also cause corrosion to equipment.
The chlorine-free catalyst supported by activated carbon prepared by pyrolysis of copper acetate shows a good catalytic effect in the process of oxidative carbonyl synthesis of carbonate, but because this catalyst preparation method cannot prepare a copper catalyst with a single valence state, during the reaction process The active ingredient is not stable

Method used

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  • Activated carbon load single valence state cuprous oxide chloride-free catalyst, preparation method, and application in oxidate oxo synthesis dimethyl carbonate
  • Activated carbon load single valence state cuprous oxide chloride-free catalyst, preparation method, and application in oxidate oxo synthesis dimethyl carbonate
  • Activated carbon load single valence state cuprous oxide chloride-free catalyst, preparation method, and application in oxidate oxo synthesis dimethyl carbonate

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Experimental program
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Effect test

preparation example Construction

[0019] 1) Preparation of activated carbon-loaded copper acetate: prepare a certain concentration (0.04-0.075M) of copper acetate aqueous solution in a 100ml volumetric flask, weigh several grams of activated carbon, and place the prepared copper acetate aqueous solution and activated carbon together in an eggplant type In the flask, stir vigorously at 180-220 rpm for 20-24 hours, remove the water solvent under reduced pressure, and dry in an oven at 80-100°C for 8-12 hours to obtain an activated carbon-loaded copper acetate sample, which is denoted as Cu( OAc) 2 / AC.

[0020] Preparation of activated carbon-supported single-valence cuprous oxide catalyst: Measure 100-120ml of ethylene glycol, and mix the prepared Cu(OAc) 2 / AC samples were ultrasonically dispersed in ethylene glycol solution for 10-20 minutes, then transferred the suspension into a three-necked flask, stirred at 100-120 rpm and heated to 140°C, then added 5-6ml of water, and heated to 180°C, reflux at this t...

Embodiment 1

[0022] The preparation method of activated carbon supported single-valence cuprous oxide catalyst is as follows:

[0023] Preparation of activated carbon-loaded copper acetate: prepare 0.05M copper acetate aqueous solution in a 100ml volumetric flask, weigh 3g of activated carbon, put the prepared copper acetate aqueous solution and activated carbon together in an eggplant-shaped flask, and stir vigorously at 200 rpm Stir for 24 hours, remove the water solvent under reduced pressure, and dry in an oven at 90°C for 8 hours to obtain a sample of activated carbon-supported copper acetate, which is denoted as Cu(OAc) 2 / AC.

[0024] Preparation of activated carbon-supported single-valence cuprous oxide catalyst: Measure 110ml of ethylene glycol, and prepare Cu(OAc) 2 / AC samples were ultrasonically dispersed in ethylene glycol solution for 10 minutes, then the suspension was transferred to a three-necked flask, stirred at 100 rpm and heated to 140°C, then added 5ml of water, heat...

Embodiment 2～5

[0026] Under the situation that other experimental conditions are exactly the same as Example 1, the copper acetate aqueous solution concentration is changed into 0.04M, 0.06M, 0.068M, 0.075M. That is to adjust the loading amount of the catalyst. The catalysts finally obtained were tested by ICP-OES, and the actual loadings of copper were 12.74wt%, 15.29wt%, 18.79wt%, and 20.12wt%, respectively. The optimal catalyst loading can be obtained by comparing the activity test.

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Abstract

The invention provides an activated carbon load single valence state cuprous oxide chloride-free catalyst used for oxidating oxo synthesis carbonic ester, and a preparation method of the catalyst. The catalyst is a chloride-free catalyst taking activated carbon as a carrier; the active constituent of load is single valence state cuprous oxide, and the load capacity accounts for 12 to 22wt% of the carrier (copper is taken as the criteria). The preparation process comprises preparation of activated carbon load cupric acetate and preparation of activated carbon load single valence state cuprous oxide catalyst. The invention has the advantages that the preparation method of the catalyst is simple, the price is low, no chlorine exists when the catalyst provided by the invention is in use, the valence state of the active constituent is single and stable, sintering can not occur easily, and the product of dimethyl carbonate is high in selectivity, high in catalytic activity and the like.

Description

technical field [0001] The invention belongs to gas-phase synthesis catalytic technology for synthesizing carbonates, and more specifically relates to an activated carbon-loaded single-valence cuprous oxide chlorine-free catalyst for oxidative carbonyl synthesis of dimethyl carbonate and a preparation method thereof. Background technique [0002] As an environmentally friendly green chemical, dimethyl carbonate (DMC) is currently widely used in many fields such as pesticides, medicines, coatings, spices, energy, electronics, etc., and has good industrial prospects. DMC has the advantages of low toxicity, biodegradability, and active chemical properties. The molecular formula of DMC contains methyl, methoxy, methoxycarbonyl, and carbonyl groups. It is widely used as a substitute for these groups in synthesis reactions. It can replace phosgene as a carbonylation reagent, greatly reducing environmental pollution. At the same time, due to its high oxygen content, DMC is also on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07C69/96C07C68/00
Inventor 闫冰马新宾王胜平黄守莹孟庆森
Owner TIANJIN UNIV
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