Method for directly preparing 1,3-dichloro-2-propanol by catalyzing glycerol with sulfur and zirconium

A sulfur-zirconium catalyzed glycerin, direct technology, applied in chemical instruments and methods, introduction of halogen preparation, physical/chemical process catalysts, etc., can solve the problems that the catalyst cannot be recycled and reused, does not conform to the development of green chemistry, and the post-processing of products is troublesome. , to achieve the effect of reducing the pre-reaction time, mild reaction conditions and low reaction temperature

Inactive Publication Date: 2009-12-30
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methods of patents CN1882522A and CN86102942A both use liquid acid as a catalyst, but the post-processing of the product is troublesome, ...

Method used

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  • Method for directly preparing 1,3-dichloro-2-propanol by catalyzing glycerol with sulfur and zirconium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 8.149 g of glycerin into the four-neck flask, add 0.256 g of catalyst sulfur zirconium under stirring, heat to reflux, and measure 9 ml of hydrochloric acid with a mass fraction of 36%. The temperature of the reaction system was raised to 100°C, and hydrochloric acid was added dropwise to the four-necked flask at a constant pressure. The dropwise addition was completed within 0.5 hours. When no water came out of the fractionating column, the reaction was stopped, the temperature was lowered, the catalyst was recovered, and the reaction product was distilled under reduced pressure to obtain 1,3-dichloro-2-propanol, the yield of 1,3-dichloro-2-propanol reaches 90.5%.

Embodiment 2

[0021] Add 24.447g of glycerin into the four-neck flask, add 1.222g of catalyst zirconium sulfur under stirring, heat to reflux, and measure 55ml of hydrochloric acid with a mass fraction of 30%. The temperature of the reaction system was raised to 100°C, and hydrochloric acid was added dropwise to the four-necked flask at a constant pressure. The dropwise addition was completed within 0.75 hours. When no water came out of the fractionating column, the reaction was stopped, the temperature was lowered, the catalyst was recovered, and the reaction product was distilled under reduced pressure to obtain 1,3-dichloro-2-propanol, the yield of 1,3-dichloro-2-propanol reaches 91.7%.

Embodiment 3

[0023] Add 48.160 g of glycerin into the four-neck flask, add 3.371 g of catalyst sulfur zirconium under stirring, heat to reflux, and measure 130 ml of hydrochloric acid with a mass fraction of 38%. The temperature of the reaction system was raised to 100°C, and hydrochloric acid was added dropwise to the four-necked flask at constant pressure. The dropwise addition was completed within 1 hour. When no water came out of the fractionating column, the reaction was stopped, the temperature was lowered, the catalyst was recovered, and the reaction product was distilled under reduced pressure to obtain 1,3-dichloro-2-propanol, the yield of 1,3-dichloro-2-propanol reaches 93.1%.

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Abstract

The invention relates to a method for directly preparing 1,3-dichloro-2-propanol by catalyzing glycerol with sulfur and zirconium, which comprises the following steps: using the glycerol and hydrochloric acid as raw materials according to a mol ratio of 1.0:1.0-5.0, and using the sulfur and the zirconium as catalysts; adding the glycerol and the catalysts into a reactor first; dropping the hydrochloric acid of which the mass percentage is between 20 and 38 percent into the reactor within 0.5 to 1.0 hour after starting chlorination reaction; and carrying off the water generated in the reaction process by a fractionating column of a filling glass ring to prepare the 1,3-dichloro-2-propanol, wherein the selections of the water division and the reaction condition in the reaction process are key factors for controlling the chlorination rate, and the temperature of the reaction system is adjusted and controlled by a temperature controller. By using the method for directly preparing the 1,3-dichloro-2-propanol by catalyzing the glycerol with the sulfur and the zirconium, the yield of the 1,3-dichloro-2-propanol can reach over 90 percent, the reaction condition is mild, and by using the hydrochloric acid to react with the glycerol, the post-treatment is simple and the catalysts can be recycled.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a chlorination method for directly preparing 1,3-dichloro-2-propanol from glycerin catalyzed by sulfur and zirconium. Background technique [0002] Biodiesel is a high-quality substitute for petrochemical diesel. Its superior performance, environmental friendliness and renewability have attracted attention from all over the world. Glycerol is the main by-product in the production process of biodiesel. The reuse of by-product glycerol has become a serious problem for the large-scale industrialization of biodiesel. In addition, the demand for synthetic chlorohydrin rubber in my country is also growing rapidly. 1,3-Di Chloro-2-propanol is an important chemical intermediate, and it is a raw material for the preparation of epoxy resin, pharmaceuticals, synthetic rubber, and papermaking. Therefore, it is of great practical significance to prepare 1,3-dichloro-2-propanol by usi...

Claims

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Application Information

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IPC IPC(8): C07C31/36C07C29/62B01J27/04
Inventor 肖国民刘群尚倩倩
Owner SOUTHEAST UNIV
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