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Catalyst for synthesizing dimethyl carbonate and preparation method thereof

A technology of dimethyl carbonate and catalyst, which is applied in the field of catalyst and its preparation for oxidative carbonylation of methanol to dimethyl carbonate, can solve the problems of low DMC yield and low conversion rate of methanol, and achieve high DMC yield and methanol High conversion effect

Inactive Publication Date: 2014-05-07
TAIYUAN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the solid catalysts adopted to synthesize dimethyl carbonate by methanol oxidative carbonylation mainly include: Cu-Ni series (such as: Cu-Ni / MWCNTs, Cu / NiO-V 2 o 5 / SiO 2 , Cu-Ni / TEG, Cu-Ni / AC+V, etc.), Zn-Zr series (such as ZrO 2 +CeO 2 , ZrO 2 etc.), alkoxy metal organic compound series (such as: Bu 2 Sn(OMe) 2 、Sn(OMe) 4 etc.) other series (such as: Ti 2 (OMe) 4 , Nb(OR) 5 、Ni(OAC) 2 、K 2 CO 3 / CH 3 I etc.), these catalysts or methanol conversion rate are low, or DMC productive rate is low

Method used

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  • Catalyst for synthesizing dimethyl carbonate and preparation method thereof
  • Catalyst for synthesizing dimethyl carbonate and preparation method thereof
  • Catalyst for synthesizing dimethyl carbonate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 Catalyst composition, preparation method and activity evaluation of the present invention

[0042] 1. Catalyst composition:

[0043] Active ingredient: CuO-CoO

[0044] Cocatalyst: K 2 o

[0045] Carrier: ZSM-5 (5A-molecular sieve)

[0046] 2. Preparation method:

[0047] (1) Prepare 100 mL each of 3 mol / L copper nitrate, cobalt nitrate and potassium nitrate respectively, and set aside.

[0048] (2) According to Cu(II): Co(II): K(I) is the proportion shown in Table 1 (the proportion shown in Table 1 is the ratio of moles, and the catalyst composition is selected by orthogonal test method) to take the above Put the stock solution into a 100mL beaker and mix it for later use.

[0049] (3) Weigh 10g ZSM-5 (among them, SiO 2 : Al 2 o 3 ≈2) into the mixture of (2).

[0050] (4) Put the beaker into an ultrasonic oscillator, set the temperature at 20° C., and the oscillation frequency at 60 Hz, and disperse for 6 hours. The purpose of dispersion is to m...

Embodiment 2

[0060] Embodiment 2: Catalyst preparation condition optimization experiment

[0061] Weigh K with a Cu / Co / K molar ratio of 1.00:0.75:0.03 2 1.0g of O-Cu-Co / ZSM-5 composite catalyst was loaded into a pressurized continuous fixed-bed differential reactor, and hydrogen gas was introduced at a flow rate of 5.0ml / min. The reduction temperature was 280°C, the reduction time was 2 hours, and the reduction pressure was 2MPa. Stop feeding hydrogen, switch to methanol, CO, O 2 , to evaluate the activity of the catalysts prepared under different conditions, the results are shown in Table 2-8.

[0062] The activity was evaluated using GC112A gas chromatograph and thermal conductivity cell detector. The conditions are: chromatographic column: GDX-502; detector: TCD; carrier gas: H 2 ;Carrier gas flow rate: 5.0mL min -1 ; Injector temperature: 150°C; Detector temperature: 150°C; Column temperature: 130°C. CO conversion and DMC (dimethyl carbonate) yield were calculated using the area...

Embodiment 3

[0092] Example 3 Catalyst Performance Evaluation Experiment

[0093] This example evaluates the influence of reaction time, reaction temperature, reaction pressure, and raw material ratio on the performance of the catalyst of the present invention, wherein the catalyst prepared in Example 1 above with K / Cu / Co=0.03:1.00:0.75 is taken as an example.

[0094] The catalyst of this embodiment is applied in the oxidative carbonylation synthesis of dimethyl carbonate with methanol, carbon monoxide and oxygen as raw materials, and the main reaction chemical formula is as follows:

[0095] 2CH 3 OH+CO+1 / 2O 2 →(CH 3 O) 2 CO+H 2 o

[0096] Methanol flow rate 0.21ml / min.

[0097] The specific performance evaluation experiments are as follows:

[0098] 1. Effect of reaction time on catalyst performance

[0099] When the reaction temperature is 165℃, CO / O 2 =10:1 (ratio of moles), when the reaction pressure is 0.2Mpa, the influence of different reaction times on the synthesis of...

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Abstract

The invention relates to a catalyst for synthesizing dimethyl carbonate from methanol through oxidization and carbonylation and a preparation method of the catalyst. The catalyst is composed of CuO-CoO as active ingredients, K2O as a cocatalyst, and a ZSM-5 molecular sieve as a carrier, wherein the molar ratio of Cu to Co to K is (1.00-1.20):(0.70-0.80):(0.02-0.04), preferably 1.00:0.75:0.03. The preparation method of the catalyst comprises the steps of: mixing soluble thermally-decomposable copper salt, cobalt salt and potassium salt at the molar ratio of Cu to Co to K being (1.00-1.20):(0.70-0.80):(0.02-0.04), preferably 1.00:0.75:0.03, then adding the ZSM-5 molecular sieve, ultrasonically dispersing, filtering, drying, calcining and aging to obtain the catalyst. The catalyst has high methanol conversion rate and good dimethyl carbonate selectivity.

Description

technical field [0001] The invention belongs to the field of catalysts, and relates to a catalyst for synthesizing dimethyl carbonate and a preparation method thereof, in particular to a catalyst for oxidative carbonylation of methanol to synthesize dimethyl carbonate and a preparation method thereof. Background technique [0002] Dimethyl carbonate (DMC) has high activity and high reactivity. It can be used as a substitute for highly toxic phosgene and dimethyl sulfate, and can also be used as a gasoline additive to increase the octane number. Its synthesis and application are increasingly received by people. Pay attention to. At present, there are three main industrial production methods of DMC: phosgene method, transesterification method and methanol oxidative carbonylation method. Oxidative carbonylation of methanol is currently the most important production method of DMC due to its cheap and easy-to-obtain raw materials, simple process and low environmental pollution. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/46C07C69/96C07C68/00
Inventor 张四方朱瑞涛董金龙任跃红李琳李军
Owner TAIYUAN NORMAL UNIV
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