Copper-based catalyst prepared by ammonia distillation method and application of copper-based catalyst in oxidation carbonylation synthesis of alkyl carbonate

A copper-based catalyst and catalyst technology, applied in the direction of molecular sieve catalysts, physical/chemical process catalysts, carbonate/haloformate preparation, etc., can solve problems such as equipment corrosion, catalyst deactivation, chlorine loss, etc., to achieve the elimination of activity Decrease, good stability, the effect of stable active components

Active Publication Date: 2013-05-08
TIANJIN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the research on this reaction system mainly focuses on the design and development of catalysts, in which CuCl is supported on carbon supports. 2 -PdCl 2 The Wacker-type catalyst has better initial activity and selectivity, but at the same time there are problems of catalyst deactivation and equipmen

Method used

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  • Copper-based catalyst prepared by ammonia distillation method and application of copper-based catalyst in oxidation carbonylation synthesis of alkyl carbonate
  • Copper-based catalyst prepared by ammonia distillation method and application of copper-based catalyst in oxidation carbonylation synthesis of alkyl carbonate

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Embodiment 1

[0024] Using copper acetate as the precursor, the process of preparing the catalyst by distilling ammonia is as follows: Weigh Cu(CH 3 COO) 2 ·H 2 O3.1g was added to a three-necked flask, then 70mL of distilled water was added, and after stirring until it was completely dissolved, 16mL of ammonia water (commercially available) with a mass fraction of 25% was slowly added dropwise to adjust the pH of the solution to 11~12, sealed and vigorously stirred for 30min, The stirring speed is 120 rpm. Then weigh 9g of commercially available NaY molecular sieve powder (Shanghai Xinnian Petrochemical Auxiliary Co., Ltd., n(SiO 2 ) / n(Al 2 o 3 )=10) Add 30mL of distilled water into a three-necked flask, stir vigorously at 20-25°C for 8h, and the stirring speed is 240 rpm. Use a super constant temperature water bath to raise the temperature to 80°C, and place the three-neck flask open, so that the ammonia in the system is evaporated until the slurry is neutral and stops stirring at 120...

Embodiment 2-4

[0027] In the case that other experimental conditions are exactly the same as in Example 1, copper acetate was changed to copper nitrate, copper chloride and copper sulfate to ensure that the Cu loading accounted for 10% of the total catalyst mass. The obtained Cu-Y molecular sieve catalyst XRD spectrogram is as figure 2 As shown (XRD adopts the Rigaku D / max2500v / pc diffractometer of Japan Rigaku, and uses Cu / K-alphal rays as the light source for measurement. The target is a copper target, the 2θ angle measurement range is 3~90°, and the scanning speed is 8° / min, the test samples are all powder, the same below).

Embodiment 5-7

[0029] Under the completely identical situation of other experimental conditions and embodiment 2, the loading capacity of Cu is changed to 1wt.%, 3wt.%, 6wt.%, the Cu-Y molecular sieve catalyst XRD spectrogram that obtains is as follows figure 1 shown. Depend on figure 1 It can be seen that when the loading reaches or exceeds 10wt.%, metallic copper and Cu appear in the catalyst system 3 o 4 The appearance of a small amount of copper and its oxide crystals is beneficial to the catalyst activity.

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Abstract

The invention discloses a copper-based catalyst prepared by an ammonia distillation method and an application of the copper-based catalyst in a reaction system for oxidation carbonylation synthesis of alkyl carbonate. The use of a chlorine-containing compound is completely avoided in the preparation process of the catalyst, so that the problems of equipment corrosion and deactivation caused by chlorine loss are completely solved; and the catalyst prepared by the ammonia distillation method is high in selectivity, long in service life, low in preparation cost and relatively simple in process.

Description

technical field [0001] The invention belongs to the catalytic technical field of gas-phase synthesis of dialkyl carbonate, and more specifically, relates to a method for synthesizing dimethyl carbonate (DMC) or diethyl carbonate (DEC) by gas-phase carbonyl oxidation carbonylation of methanol or ethanol Catalyst and method for its preparation. Background technique [0002] Alkyl carbonates, especially dimethyl carbonate and diethyl carbonate, are green chemicals with a wide range of uses. Because low-chain alkyl carbonates have low toxicity, biodegradability and active chemical properties, they can be used as carbonylation reagents and alkylation reagents to replace toxic substances such as phosgene and halogenated hydrocarbons, and participate in important organic synthesis reactions. It is used in many fields such as synthetic pesticides, medicines, paints, spices, etc., and has good industrial prospects. In recent years, DMC and DEC as oxygen-containing additives can eff...

Claims

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Application Information

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IPC IPC(8): B01J29/14B01J29/76C07C69/96C07C68/00
Inventor 黄守莹马新宾闫冰王胜平赵玉军
Owner TIANJIN UNIV
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