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A method for metal hydrothermal reduction of glycerin to produce propylene glycol

A technology of propylene glycol and glycerin, which is applied in the field of environmental chemical industry to achieve the effects of convenient operation, fast reaction rate and mild reaction temperature conditions

Active Publication Date: 2016-04-06
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, under hydrothermal conditions, iron powder, copper powder, cobalt powder and other metals are used to replace the hydrogen source and nickel as a catalyst to reduce biodiesel by-product glycerol to propylene glycol has not been reported in literature and patents.

Method used

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  • A method for metal hydrothermal reduction of glycerin to produce propylene glycol
  • A method for metal hydrothermal reduction of glycerin to produce propylene glycol
  • A method for metal hydrothermal reduction of glycerin to produce propylene glycol

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 0.07g glycerol, 10mmol metal Ni, and a certain amount of Fe into the reactor, wherein Fe is determined by Fe / Ni molar ratio of 1 / 2, 3 / 4, 1 / 1, 4 / 3 and 2 / 1 respectively , under the conditions of reaction temperature of 280°C and reaction time of 150 min, hydrothermal reduction reaction occurs, and propylene glycol is obtained by separating the product. Then adjust the reaction temperature to 230°C, 250°C, 280°C and 300°C respectively, 0.07g of glycerin, 10mmol of Fe and Ni, and a reaction time of 120min to prepare propylene glycol; finally adjust the reaction time to 60min, 90min, 120min, and 150min and 180 min, 0.07 g of glycerin, 10 mmol of both Fe and Ni, and a reaction temperature of 250° C. to prepare propylene glycol. When the amount of glycerol added is 0.07g, the amount of Fe and Ni added is 10mmol, the reaction temperature is 250°C, and the reaction time is 120min, the yield of propylene glycol reaches 53.14%, and the conversion rate of glycerol reaches 79.25...

Embodiment 2

[0025] Under the joint action of Fe-Ni, the solid residue collected after the reaction in Example 1 was filtered and rinsed with deionized water, and dried in an oven at 70° C. for testing. D / MAX2550 type X-ray diffractometer is used for detection, the 2θ angle range of X-ray diffraction is 5-70°, and the rotation angle rate is 10° / min. The analysis results show that the attached figure 2 As shown, Fe reacts with Fe 2 o 3 Form exists, and Ni does not change, and in conjunction with embodiment 1, proves that in this reaction Fe is used as reducing agent, and Ni is used as catalyst, and this reaction does not need to provide the reason of external hydrogen source just.

Embodiment 3

[0027] Add 0.07g of glycerin, Cu and Ni into the reactor with the same dosage, the dosage is 1mmol, 3mmol, 5mmol, 10mmol and 15mmol in sequence, and the reaction temperature is 280℃, and the reaction time is 150min. Hydrothermal reduction reaction to obtain propylene glycol by isolating the product. Then adjust the reaction temperature to 230°C, 250°C, 280°C and 300°C respectively, 0.07g of glycerol, 10mmol of Cu and Ni, and 120min of reaction time to prepare propylene glycol; finally adjust the reaction time to 60min, 90min, 120min, and 150min respectively and 180 min, 0.07 g of glycerin, 10 mmol of both Cu and Ni, and a reaction temperature of 250° C. to prepare propylene glycol. When the addition amount of glycerol is 0.07g, the addition amount of Cu and Ni is 10mmol, the reaction temperature is 250℃, and the reaction time is 120min, the yield of propylene glycol reaches 46.61%.

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Abstract

The invention relates to a method for producing propylene glycol by hydrothermally reducing glycerol with metals. The method comprises the following specific steps: adding the glycerol, a reducing agent and a catalyst to a reactor in a certain proportion; carrying out hydrothermal reduction reaction under the condition that the reaction temperature is 200-400 DEG C and the reaction time is 60-180 minutes so as to convert the glycerol into the propylene glycol, wherein the reducing agent is any one of iron powder or copper powder or cobalt powder, and the catalyst is nickel powder. The method disclosed by the invention has the advantages of simple process, convenience for operation, no secondary pollution, waste recycling capability and certain economic and social benefits.

Description

technical field [0001] The invention relates to a process for producing propylene glycol from glycerol, in particular to a hydrothermal reduction method using cheap metals as reducing agents and catalysts, and belongs to the field of environmental chemical industry. Background technique [0002] At present, fossil fuels such as crude oil are becoming increasingly tense, and at the same time, more and more attention has been paid to the environmental problems caused by them. In view of biodiesel, as an environmentally friendly alternative energy, it has been paid more and more attention. It is estimated that at least 0.1 ton of glycerol will be produced per ton of biodiesel produced. It can be seen that the worldwide growth of biodiesel production will be accompanied by the production of a large amount of glycerol as a by-product. Although pure glycerol is widely used in food, medicine, etc., the purification cost of glycerol, which is a by-product of biodiesel, is too high....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/60C07C31/20
CPCC07C29/60C07C31/205
Inventor 沈峥张亚雷顾敏燕董文杰张敏桑文静周雪飞
Owner TONGJI UNIV
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