Long-life catalyst for synthesis of propylene carbonate and preparation method thereof

A technology of acrylate carbonate and catalyst, which is applied in the field of long-life catalyst and its preparation, can solve the problems of difficult separation of homogeneous catalyst, easy loss of active components, loss of active components, etc., and achieves low loss rate, long catalyst life, The effect of high catalytic activity

Active Publication Date: 2016-06-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] However, there are many problems in the catalysts currently used. The homogeneous catalysts are not easy to separate, and the catalysts supported by inorganic ions such as alkali metal ions have the

Method used

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  • Long-life catalyst for synthesis of propylene carbonate and preparation method thereof
  • Long-life catalyst for synthesis of propylene carbonate and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) 11 g of imidazo[1,2-a]pyrazine and 19 g of 1,2-dibromoethane were dissolved in 30 g of methanol, and refluxed at 50°C for 2 days. Then the product is concentrated by distillation to obtain an oily long-chain domidazole compound.

[0035] (2) Reflux 20 g of domisole compound and 40 g of chloromethyl polystyrene microspheres in 200 g of toluene for 2 days. After filtering, it was washed three times with toluene and propylene carbonate respectively, and then dried in vacuum at 70° C. for 24 hours to obtain active component A1.

[0036] (3) Grinding and mixing 20 grams of active component A with 10 grams of zinc chloride, 20 grams of resorcinol formaldehyde resin, and 2 grams of urotropine, and crushing them into powders below 120 mesh. The powder is compressed into tablets, the pressure of the compression molding is 12 MPa, and the time of holding under pressure is 3 minutes. Active precursor B1 was prepared.

[0037] (4) The active precursor B was heated at 180 °C ...

Embodiment 2

[0040] (1) 11 g of imidazo[1,2-a]pyrazine and 19 g of 1,2-dibromoethane were dissolved in 30 g of methanol, and refluxed at 50°C for 4 days. Then the product is concentrated by distillation to obtain an oily long-chain domidazole compound.

[0041] (2) Reflux 20 g of domidazole compound and 40 g of chloromethyl polystyrene microspheres in 200 g of toluene for 1 day. After filtration, it was washed three times with toluene and propylene carbonate respectively, and then dried in vacuum at 70° C. for 24 hours to obtain active component A2.

[0042] (3) Grind and mix 20 grams of active component A2 with 15 grams of zinc bromide, 20 grams of resorcinol formaldehyde resin, and 2 grams of urotropine, and grind them into powders below 120 mesh. The powder is compressed into tablets, the pressure of the compression molding is 12 MPa, and the time of holding under pressure is 3 minutes. Active precursor B2 was prepared.

[0043] (4) The active precursor B2 was heated at 180 °C for 2 ...

Embodiment 3

[0046] (1) 11 g of imidazo[1,2-a]pyrazine and 19 g of 1,2-dibromoethane were dissolved in 30 g of methanol, and refluxed at 50°C for 2 days. Then the product is concentrated by distillation to obtain an oily long-chain domidazole compound.

[0047] (2) Reflux 20 g of domidazole compound and 40 g of chloromethyl polystyrene microspheres in 200 g of toluene for 3 days. After filtering, it was washed three times with toluene and propylene carbonate respectively, and then dried under vacuum at 70°C for 24 hours to obtain active component A3.

[0048] (3) Grinding and mixing 20 grams of active component A3 with 30 grams of zinc bromide, 20 grams of resorcinol formaldehyde resin, and 2 grams of urotropine, and crushing them into powders below 120 mesh. The powder is compressed into tablets, the pressure of the compression molding is 12 MPa, and the time of holding under pressure is 3 minutes. Active precursor B3 was prepared.

[0049] (4) The active precursor B3 was heated at 180...

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Abstract

The invention discloses a preparation method of a high efficiency catalyst for synthesis of propylene carbonate. The method comprises the steps of: (1) dissolving imidazo[1, 2-a]pyrazine and dibromoalkane in methanol, then subjecting the product to distillation concentration to remove methanol so as to obtain a polyimidazole compound; (2) subjecting the polyimidazole compound prepared by step (1) and chloromethylated polystyrene to backflow in a toluene solvent for 1-3 days, performing filtration and washing, and then conducting vacuum drying at 60-80DEG C for 12-24h to obtain an active component A; (3) smashing the active component A with a zinc salt, resorcinol formaldehyde resin and urotropine together, performing mixing, and conducting tabletting molding to obtain an active precursor B; (4) heating the active precursor B under nitrogen protection to obtain an active precursor P; and (5) soaking the active precursor P in dibromoalkane, and carrying out soaking, separation, washing, drying and smashing so as to obtain a catalyst C. The catalyst prepared by the method has difficultly losable active component.

Description

technical field [0001] The invention relates to a long-life catalyst for synthesizing propylene carbonate and a preparation method thereof, in particular to a CO on a fixed bed reactor 2 Preparation method of catalyst for preparing propylene carbonate with propylene oxide. Background technique [0002] The cycloaddition of propylene oxide and carbon dioxide to form propylene carbonate is an exothermic and volume-reducing reaction, and the product propylene carbonate is an organic solvent with excellent performance and an intermediate in organic synthesis. The reaction is to achieve CO 2 an important way to reduce emissions. [0003] KI and TEABr are the most commonly used homogeneous catalysts. It has high conversion and selectivity at high pressure. Quaternary ammonium and quaternary phosphonium salts such as octadecyltrimethylammonium bromide and tricyclohexylphosphine are good catalysts. Increasing the ionization degree of the catalyst KI in the reaction can improve ...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07D317/36C07D317/38
Inventor 方向晨张志智孙万富张喜文孙潇磊杨超陈楠鲁娇
Owner CHINA PETROLEUM & CHEM CORP
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