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Catalyst for CO gas-phase coupling synthesis of dimethyl carbonate, preparation method and application of the catalyst

A dimethyl carbonate and catalyst technology, applied in the field of organic synthesis, can solve the problems of catalytic performance to be improved, increased processing cost, short service life, etc., and achieve the effects of long service life, improved catalytic performance and long service life

Active Publication Date: 2021-02-02
NINGBO JINYUANDONG PETROCHEM ENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The catalysts used in the above-mentioned patents all contain noble metals (platinum or palladium), which not only have a short service life and high preparation costs, but also require additional processes to treat the noble metals after the catalyst is used, which increases the processing cost; in addition, The catalytic properties (such as stability) of the above-mentioned catalysts also need to be improved

Method used

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  • Catalyst for CO gas-phase coupling synthesis of dimethyl carbonate, preparation method and application of the catalyst
  • Catalyst for CO gas-phase coupling synthesis of dimethyl carbonate, preparation method and application of the catalyst
  • Catalyst for CO gas-phase coupling synthesis of dimethyl carbonate, preparation method and application of the catalyst

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preparation example Construction

[0031] The preparation method of above-mentioned catalyst, it comprises the following steps:

[0032] 1) PdCl 2 , CuCl 2 , the chloride of the alkali metal element and the solvent are mixed to form a solution, and the solvent is water and / or alcohol, and the chloride of the alkali metal element includes but not limited to lithium chloride, sodium chloride, potassium chloride and rubidium chloride One or more; adding hydrochloric acid to adjust the pH value to 0.5-4;

[0033] 2) Add γ-Al 2 o 3 The carrier is added to the solution in the above steps, dried after immersion at room temperature, and then roasted to obtain the catalyst product; the method of evaporating and drying the solvent is ultrasonic, heating or drying in a drying oven, the roasting temperature is 200 ° C, and the roasting time is more than 2 hours .

[0034] In some embodiments, the PdCl in the step 1) 2 The concentration is 10-500mmol / L, CuCl 2The concentration is 15-800mmol / L, and the concentration o...

Embodiment 1

[0042] 10mmolPdCl 2 , 16.7mmolCuCl 2 , 150mmol lithium chloride, and 100g water were mixed to form a solution, and hydrochloric acid was added to adjust the pH to 0.8. 100g carrier γ-Al 2 o 3 Balls (γ-Al in spherical form 2 o 3 Carrier) was added to the above solution, immersed at room temperature for 48 hours, evaporated and dried in a drying oven at 120°C, and then calcined at 200°C for 10 hours. Catalyst sample No. 1 was obtained, wherein the loading rate of Pd was 1.0wt%, and the loading rate of Cu was 1.0wt%.

Embodiment 2

[0044] 2.5mmolPdCl 2 , 4.2 mmol CuCl 2 , 500mmol lithium chloride, and 100g methanol were mixed to form a solution, and hydrochloric acid was added to adjust the pH to 1. 100g carrier γ-Al 2 o 3 Add the balls into the above solution, soak at room temperature for 48 hours, evaporate and dry in a drying oven at 120°C, and then bake at 200°C for 10 hours. Catalyst sample No. 2 was obtained, wherein the loading rate of Pd was 0.25wt%, and the loading rate of Cu was 0.25wt%.

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Abstract

The invention discloses a catalyst for gas phase synthesis of dimethyl carbonate by CO and methyl nitrite under low temperature and low pressure conditions, a preparation method of the catalyst and an application thereof. The catalyst is γ-Al 2 o 3 A wacker-type catalyst that supports Pd‑Cl‑Cu and is doped with alkali metal elements; the γ‑Al of the catalyst 2 o 3 The specific surface area of ​​the carrier is 20‑200m 2 / g, the pore volume is 0.1‑1.5m 2 / g, the pore size is 3-20nm; the alkali metal element is one or more of Li, Na, K, Rb, and the alkali metal element content is 0.1wt%-5.0wt%. The catalyst of the present invention can be applied to CO and methyl nitrite gas-phase synthesis of dimethyl carbonate under low temperature and low pressure conditions. When it is used at low pressure and low temperature, it has high selectivity and space-time yield, and is suitable for industrialized CO and nitrite. Dimethyl carbonate is synthesized from methyl nitrate in low-temperature and low-pressure gas phase; and it has a longer service life than common noble metal catalysts.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a catalyst for gas-phase synthesis of dimethyl carbonate by CO and methyl nitrite under low-temperature and low-pressure conditions, a preparation method of the catalyst and an application thereof. Background technique [0002] Dimethyl carbonate (DMC) is an important organic chemical raw material and a cornerstone chemical in organic synthesis. Dimethyl carbonate contains multiple functional groups such as methoxy, methyl and carbonyl, and its chemical properties are very active. It is widely used in agricultural medicine, dyes, lubricating oil, synthetic materials, additives, electronic chemicals, etc. At present, the methods for synthesizing dimethyl carbonate mainly include: phosgene method, methanol oxidative carbonylation method, transesterification method, urea alcoholysis method, CO2 and methanol direct synthesis method. [0003] CO and methyl nitri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/13B01J35/10C07C68/00C07C69/96
CPCB01J27/135B01J35/1014B01J35/1019B01J35/1047B01J35/1061C07C68/00C07C69/96
Inventor 项裕桥臧未一刘太泽邵迪陈嘉梁
Owner NINGBO JINYUANDONG PETROCHEM ENG TECH
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