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Solid base catalyst, preparation of solid base catalyst as well as application of solid base catalyst to preparation of guaifenesin

A solid base catalyst and carrier technology, which is applied in the preparation of organic compounds, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of adverse effects on the environment and human body, high boiling point of solvent DMF, and many steps, and achieve low energy consumption , Easy to operate, environmentally friendly, and easy to regenerate

Active Publication Date: 2014-11-12
ZHEJIANG HAIZHOU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material p-toluenesulfonate mesityl glyceride used in this method comes from the reaction of mesityl glycerol and p-toluenesulfonyl chloride, the steps are numerous, and the boiling point of the solvent DMF is high, the energy consumption for removal is large, and a small amount of residue is harmful to the environment and adverse effects on the human body

Method used

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  • Solid base catalyst, preparation of solid base catalyst as well as application of solid base catalyst to preparation of guaifenesin
  • Solid base catalyst, preparation of solid base catalyst as well as application of solid base catalyst to preparation of guaifenesin

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Take 100g γ-Al 2 o 3 (Wenzhou Jingjing Alumina Co., Ltd.), add 2g aluminum sol (Jiangyin Xiagang Chemical Factory) as a binder, add 15g Mg(OAc) 2 , mix and grind for 1 hour, add 10g Ca(OH) 2 , add 1g NaOH, add 3g polyacrylamide (Henan Luoshan Zhongyuan Polymer Co., Ltd., molecular weight 8 million to 10 million) as an extrusion aid, continue mixing and grinding for 2 hours, add 20 g of water, and extrude with an extruder Into ? 1.6mm strip. Dry the product under infrared light for 5 hours, put it in an oven for 10 hours at 100°C, and finally put it in a muffle furnace and bake it at 500°C for 4 hours to obtain a composite solid alkali catalyst. After cooling, put it in a desiccator for use.

Embodiment 2

[0052] Take 100g γ-Al 2 o 3 As a carrier, add 3g glycerin as a binder, add 15g MgO, mix and grind for 1 hour, add 10g Ca(OH) 2 , add 1g KOH, add 5g polyacrylamide (Henan Luoshan Zhongyuan Polymer Co., Ltd., molecular weight 8 million to 10 million) as extrusion aid, continue mixing and grinding for 2 hours, add appropriate amount of water, and extrude into ? 1.6mm strip. Dry the product under an infrared lamp for 1 hour, put it in an oven for 8 hours at 120°C, and finally place it in a muffle furnace for calcination at 550°C for 4 hours to obtain the composite solid alkali catalyst. After cooling, place it in a desiccator for use.

Embodiment 3

[0054] Take 100g γ-Al 2 o 3 , add 3g starch as binder, add 10g Mg(CO 3 ) 2 , mix and grind for 0.5 hours, add 10g Ca(OH) 2 , add 0.5g Na 2 CO 3 , add 2g polyacrylamide (Henan Luoshan Zhongyuan Polymer Co., Ltd., molecular weight 8 million to 10 million) as extrusion aid, continue mixing and grinding for 2 hours, add appropriate amount of water, and extrude into ?1.6mm strips with extruder shape. The product was dried under an infrared lamp for 5 hours, placed in an oven for 6 hours at 100°C, and finally placed in a muffle furnace for 3 hours at 500°C to roast to obtain the compounded solid alkali catalyst, which was cooled and placed in a desiccator for later use.

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Abstract

The invention discloses a composite solid base catalyst which is mainly prepared from the following components in parts by mass: 100 parts of gamma-Al2O3 as a carrier, 0.5-5 parts of a binding agent as a loaded component, 1-25 parts of a magnesium-containing compound, 1-25 parts of a calcium-containing compound, 0.5-5 parts of polyacrylamide and 0.1-2 parts of inorganic base, wherein the binding agent is selected from one of glycerol, starch, methylcellulose, polypropylene glycol, alumina sol and sodium silicate; the magnesium-containing compound is selected from one of MgO, Mg(OH)2, Mg(CO3)2, Mg(OAc)2 and MgCl2; the calcium-containing compound is selected from one of CaO, Ca(OH)2, Ca(CO3)2 and CaCl2; the inorganic base is selected from one of NaOH, KOH, Na2CO3 and K2CO3. The catalyst is used for preparing guaifenesin, is simple and convenient to operate, environmentally friendly, low in energy consumption and high in yield.

Description

[0001] technical field [0002] The invention relates to a solid base catalyst and its preparation, and a method for preparing guaiacol glyceryl ether by using the solid base catalyst. Background technique [0003] Solid base catalysts have been paid more and more attention by scientific researchers because of their advantages such as mild reaction conditions, fast reaction rate, less side reactions, and recyclability. There are various types of solid bases and they are developing rapidly. Solid bases are classified into three types: organic solid bases, organic-inorganic composite solid bases, and inorganic solid bases. At present, many important reactions in industrial production are catalyzed by inorganic solid bases. Inorganic solid bases mainly include: metal oxide solid bases, hydrotalcite solid bases, and supported solid bases. Metal oxide solid bases mainly include alkali metal oxides, alkaline earth metal oxides, rare earth metal oxides and transition metal oxides...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C43/23C07C41/26
Inventor 陈昌略王必伟徐大国裴文
Owner ZHEJIANG HAIZHOU PHARMA CO LTD
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