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Solid base catalyst and preparation method and application of solid base catalyst

A solid base catalyst and potassium fluoride technology, applied in chemical instruments and methods, physical/chemical process catalysts, ether preparation, etc., can solve problems such as catalyst separation and post-processing difficulties, equipment corrosion and scaling, environmental pollution, etc.

Active Publication Date: 2013-02-06
上海泰坦科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Using sodium alkoxide or potassium alkoxide, as well as caustic alkali and amines as basic catalysts is a relatively classic industrial homogeneous catalytic synthesis method, which has the characteristics of good activity and high selectivity of basic catalysts, but there are corrosion and fouling of equipment, pipelines Blockage, catalyst separation and post-processing difficulties, etc., will also cause a certain degree of environmental pollution
Supported solid base catalysts have been further developed. Patent EP0189246 describes a kind of ion exchange resin with amino groups as a catalyst for synthesizing alcohol ethers, but its stability is poor; British Petroleum Corporation has synthesized anion double hydroxide clay catalysts, After repeated hydration and calcination, the catalytic activity has been improved, and the conversion rate of propylene oxide has reached 82%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Weigh Mg(NO 3 ) 2 , Al(NO 3 ) 3 and Zn(NO 3 ) 2 A total of 100 g, wherein the Mg / Al molar ratio is 3, and the zinc mass fraction accounts for 10% of the total mixture; the mixture is dissolved in 200 ml of deionized water to obtain solution A;

[0024] Take the molar ratio of NaOH and Na of 1:1 2 CO 3 , dissolved in deionized water, with 200 ml of saturated lye B.

[0025] Mix solution A and saturated lye solution B by the double-drop method, control the temperature at 60 °C, stir vigorously, keep pH 9-10, after the dropwise addition, statically crystallize at 80 °C for 12 hours, filter the precipitate, wash and dry to obtain zinc and magnesium Aluminum hydrotalcite.

[0026] (2) The zinc-magnesium-aluminum hydrotalcite was calcined at 600°C for 7 hours.

[0027] (3) Step (2) The calcined product is placed in a fixed bed reactor, and the mass space velocity is 3h -1 Water was poured into it and treated at 500° C. for 3 hours to obtain a hydrothermal treatm...

Embodiment 2

[0030] (1) Step (1) is the same as in Example 1.

[0031] (2) The zinc-magnesium-aluminum hydrotalcite obtained in step (1) was calcined at 500° C. for 8 hours.

[0032] (3) Step (2) The calcined product is placed in a fixed bed reactor, and the mass space velocity is 3h -1 Water was poured into it and treated at 500° C. for 3 hours to obtain a hydrothermal treatment product.

[0033] (4) The hydrothermal treatment product was immersed in a saturated potassium fluoride solution for 3 hours, and the temperature was controlled at 75°C; filtered, dried at 100°C, and activated at 280°C for 2 hours to obtain a catalyst. The content of potassium fluoride is 31%.

Embodiment 3

[0035] Methanol, propylene oxide and the catalyst prepared in Example 1 were added to a 200 ml autoclave, and the amount of the catalyst was 1 wt % of the reactant. The reaction was cooled to room temperature, filtered, and the filtrate was distilled to give the product. The molar ratio of methanol and propylene oxide was 3:1, the amount of catalyst was 1 wt % of the reactant, and the total amount of the reactant and the catalyst was 30 g.

[0036] The product was detected by GCMS as propylene glycol methyl ether. The PO conversion rate of the whole reaction was 98.2%, the ratio of primary and secondary ethers was 96.5:3.5, and the yield was 87.2%.

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PUM

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Abstract

The invention relates to the field of catalysts and organic synthesis, and discloses a solid base catalyst, namely zinc magnesium aluminum composite oxide, for catalytically preparing propylene glycol ether compound. The preparation method comprises the steps of preparing and roasting zinc magnesium aluminum volknerite, conducting hydrothermal treatment on roasted products, impregnating the roasted products to load a right amount of potassium fluoride, and conducting drying and activation. The solid base catalyst comprises the following components by weight percent: 65%-75% of zinc magnesium aluminum composite oxide and 25%-35% of potassium fluoride, wherein the mole ratio of magnesium to aluminum is 2.8-3.2, the mass ratio of zinc, magnesium and aluminum to total zinc is 9%-12%. The solid base catalyst is used for catalytically preparing the propylene glycol ether, the conversion rate of PO (Propylene oxide) is above 95%, the selectivity is above 95:5, and the yield is above 85%.

Description

technical field [0001] The invention relates to the field of catalysts and organic synthesis, in particular to a solid base catalyst-magnesium-zinc-aluminum composite oxide used for catalyzing the preparation of propylene glycol ether compounds. Background technique [0002] Propylene glycol ether compounds are a class of fine chemical products with very good properties, and are one of the important derivatives of epoxy compounds. They are widely used in coatings, inks, electronic chemicals, leather, cleaning agents, antifreeze and other industries. Because it has two strongly soluble groups—ether bond and hydroxyl group, the stronger one is lipophilic and can dissolve hydrophobic compounds; the latter is hydrophilic and can dissolve hydrophilic compounds, and is known as "universal solvent". [0003] Although the properties of propylene glycol ether and glycol ether are basically the same, the toxicity of propylene glycol ether is far lower than that of glycol ether. Since...

Claims

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Application Information

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IPC IPC(8): B01J27/138C07C41/03C07C43/13
Inventor 谢应波张庆张华罗桂云
Owner 上海泰坦科技股份有限公司
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