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Solid super acid for catalytically synthesizing PMA (2-acetoxy-1-methoxypropane), and catalytic rectification technique and apparatus thereof

A technology of solid superacid and catalytic distillation, which is applied in the field of solid superacid for catalyzing the synthesis of PMA and its catalytic distillation process and equipment. Application and other issues, to achieve the effect of large-scale continuous production, improve the performance of repeated use, and improve the conversion rate of esterification reaction

Active Publication Date: 2015-04-29
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, solid superacids still have some shortcomings as emerging catalysts: most of the solid superacid catalysts developed at present are in powder form. Difficulty, unable to be industrialized and other problems
The preparation method of the zirconium-based solid superacid catalyst is introduced in detail in the patent application CN 101745420A, but for the molding process, only the mixing of bentonite and solid superacid catalyst powder is introduced for molding, and there is no detailed molding scheme; in the patent application CN 101890355A, the After zirconium hydroxide xerogel, binder pseudo-boehmite, peptizing acid and water are mixed evenly, they are respectively pressed into tablets by a tablet press and extruded by an extruder. The pressure is controlled to be 10- 50MPa, but no complete molding solution for titanium-based solid superacids has been found yet

Method used

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  • Solid super acid for catalytically synthesizing PMA (2-acetoxy-1-methoxypropane), and catalytic rectification technique and apparatus thereof
  • Solid super acid for catalytically synthesizing PMA (2-acetoxy-1-methoxypropane), and catalytic rectification technique and apparatus thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of solid superacid of catalytic synthesis PMA, its preparation method comprises the steps:

[0036] 1) Preparation of solid superacid TiO 2 / SO 4 2- Powder: Accurately weigh nano-sized TiO 2 Powder 20g in a watch glass, with 20g 2mol / L of H 2 SO 4 The solution was impregnated, and the two were fully stirred with a glass rod until it was a paste; then it was put into a vacuum drying oven at 0.1MPa and 120°C for 3 hours in vacuum; then the dried powder was transferred to a crucible and placed in a horse Roasting in the furnace, the calcination temperature is 500 ℃, and the calcination time is 2h, to obtain the solid super acid TiO 2 / SO 4 2- powder;

[0037] 2) Preparation of shaped solid superacid: the solid superacid TiO obtained in step 1) 2 / SO 4 2- Mix the powder with the binder pseudo-boehmite, the reinforcing agent glass fiber, and the pore-forming agent activated carbon evenly, then add the lubricant glycerin and deionized water, and knead for 30...

Embodiment 2

[0043] A kind of solid superacid of catalytic synthesis PMA, its preparation method comprises the steps:

[0044] 1) Preparation of solid superacid TiO 2 / SO 4 2- Powder: Accurately weigh nano-sized TiO 2 Powder 20g in a watch glass, with 30g 1mol / L of H 2 SO 4 The solution was impregnated, and the two were fully stirred with a glass rod until it was a paste; then it was placed in a vacuum drying oven at 0.1MPa and 90°C for 3 hours in vacuum; then the dried powder was transferred to a crucible and placed in a horse Roasting in a furnace, the calcination temperature is 350°C, and the calcination time is 5h, to obtain the solid super acid TiO 2 / SO 4 2- powder;

[0045] 2) Preparation of shaped solid superacid: the solid superacid TiO obtained in step 1) 2 / SO 4 2- The powder is evenly mixed with the binder fennel powder, the reinforcing agent glass fiber, and the pore-forming agent activated carbon, and then the lubricant glycerin and deionized water are added, and k...

Embodiment 3

[0051] A kind of solid superacid of catalytic synthesis PMA, its preparation method comprises the steps:

[0052] 1) Preparation of solid superacid TiO 2 / SO 4 2- Catalyst powder: accurately weigh nano-sized TiO 2 Powder 20g in a watch glass, with 50g 0.5mol / L of H 2 SO 4 The solution was impregnated, and the two were fully stirred with a glass rod until it was a paste; then it was placed in a vacuum drying oven at 0.1MPa and 110°C for 3 hours in vacuum; then the dried powder was transferred to a crucible and placed in a horse Roasting in a furnace, the calcination temperature is 400°C, and the calcination time is 3h, to obtain solid superacid TiO 2 / SO 4 2- catalyst powder;

[0053] 2) Preparation of shaped solid superacid: the solid superacid TiO obtained in step 1) 2 / SO 4 2- Catalyst powder, binder alumina, reinforcing agent glass fiber, and pore-forming agent activated carbon are evenly mixed, then lubricant glycerin and deionized water are added, and kneading ...

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Abstract

The invention discloses a solid super acid for catalytically synthesizing PMA (2-acetoxy-1-methoxypropane), and a catalytic rectification technique and apparatus thereof. The solid super acid is prepared by the following steps: reacting TiO2 powder with a H2SO4 solution to prepare solid super acid TiO2 / SO4<2-> powder, kneading with an adhesive, an enhancer, a pore forming agent, a lubricant and deionized water to obtain a formed precursor, carrying out extrusion forming, drying and roasting. The obtained solid super acid has the advantages of stable catalytic activity, low shedding loss tendency of the active component, and favorable repetitiveness, and can be easily separated from the reaction product. Propylene glycol monomethyl ether and acetic acid used as raw materials can be subjected to esterification reaction in a catalytic rectification tower under the catalytic action of the solid super acid to obtain the PMA. The method can implement the continuous catalytic rectification process, avoids the problems of recovery, equipment corrosion and the like in the liquid acid catalyst, and has the characteristics of low energy consumption, high reaction conversion rate, stable product quality and the like.

Description

technical field [0001] The invention specifically relates to a solid superacid that catalyzes the synthesis of propylene glycol monomethyl ether acetate (PMA) and its catalytic rectification process and equipment. Background technique [0002] Propylene glycol methyl ether acetate (PMA for short), with a melting point of 87°C and a boiling point of 149°C, is a non-pollution solvent with multiple functional groups. Its molecular formula includes ether bonds, alkyl groups and carbonyl groups, among which Ether bonds are lipophilic and can dissolve hydrophobic compounds; carbonyl groups are hydrophilic and can dissolve water-soluble compounds. Since there are both polar groups and non-polar groups in the molecular formula of PMA, the two functional groups are mutually exclusive and restrict each other, and at the same time can show their unique properties, so PMA can dissolve both polar substances and non-polar substances. Substances, and its dissolving power is much higher th...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07C69/16C07C67/08C07C67/54B01D3/14B01J8/02
CPCY02P20/10
Inventor 王红星薛学良卜祥伟叶长燊杨臣黄智贤邱挺李玲
Owner FUZHOU UNIVERSITY
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