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Catalyst for preparing monohydric alcohol and dihydric alcohol by hydrogenation of dimethyl substituted 1,3-dioxane, and application

A technology of dioxane and dimethyl, applied in metal/metal oxide/metal hydroxide catalysts, molecular sieve catalysts, reduction preparation of oxygen-containing functional groups, etc., can solve problems such as side reactions

Inactive Publication Date: 2013-07-03
武汉椿岭科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for 1,3-dioxane compounds, due to the structural characteristics of the six-ring ring, its chemical properties are stable, especially when there is a methyl group on the carbon connected to the oxygen atom, it is easy to occur in an acid-catalyzed environment. side effects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1 : select the composition as Ni / active SiO 2 / Al 2 o 3 catalyst, the mass ratio of each component is 20 / 20 / 60, 8ml of the catalyst is placed in a quartz reduction tube, under normal pressure, the hydrogen flow rate is 40ml / min, the temperature is raised to 400°C at a heating rate of 2°C / min, and at 400°C Reduction for 6 hours; keep the hydrogen flow at 40ml / min and cool down to normal temperature, and under the protection of hydrogen, transfer the catalyst to the reaction substrate 4,4-dimethyl-1,3-dioxane through degassing In methanol 50% solution, the reaction substrate is 24ml, at hydrogen pressure 4mPa, temperature 140 ℃, reaction time 12 hours, its conversion rate of substrate is 95%, the selectivity of isoamyl alcohol is 92%.

Embodiment 2

[0012] Example 2 : select the composition as Ni / active SiO 2 / Al 2 o 3 catalyst, the mass ratio of each component is 20 / 20 / 60, 8ml of the catalyst is placed in a quartz reduction tube, under normal pressure, the hydrogen flow rate is 40ml / min, the temperature is raised to 400°C at a heating rate of 2°C / min, and at 400°C Reduction for 6 hours; keep the hydrogen flow at 40ml / min and cool down to normal temperature, and under the protection of hydrogen, transfer the catalyst to the deaerated reaction substrate as 4,5-dimethyl-1,3-dioxane In methanol 50% solution, the reaction substrate is 24ml, at hydrogen pressure 4mPa, temperature 140 ℃, reaction time 12 hours, its substrate conversion rate is 85%, the selectivity of isoprene glycol is 85%.

Embodiment 3

[0013] Example 3: The selected composition is Ni / Hβ molecular sieve / Al 2 o 3 catalyst, the mass ratio of each component is 20 / 20 / 60, 8ml of the catalyst is placed in a quartz reduction tube, under normal pressure, the hydrogen flow rate is 40ml / min, the temperature is raised to 400°C at a heating rate of 2°C / min, and at 400°C Reduction for 6 hours; keep the hydrogen flow at 40ml / min and cool down to normal temperature, and under the protection of hydrogen, transfer the catalyst to the reaction substrate 4,4-dimethyl-1,3-dioxane through degassing In methanol 50% solution, the reaction substrate is 24ml, under hydrogen pressure 4mPa, temperature 110 ℃, reaction time 12 hours, its substrate conversion rate is about 100%, the selectivity of isoamyl alcohol is 89%.

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PUM

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Abstract

The invention relates to a catalyst for preparing monohydric alcohol and dihydric alcohol by hydrogenation of dimethyl substituted 1,3-dioxane. The catalyst is characterized by consisting of an active metal, a solid acid and an adhesive Al2O3, wherein the mass percentage of the active metal is 8-20%; the mass percentage of the solid acid is 20% and the balancing being the adhesive Al2O3. High conversion rate and high selectivity of a reaction substrate are realized by using the solid hydrogenation catalyst with double active sites of the solid metal and acid and by using a hydrogenation reaction.

Description

technical field [0001] The invention relates to a catalyst for preparing monohydric alcohol and dihydric alcohol through hydrogenation of dimethyl-substituted 1,3-dioxane and its application. Background technique [0002] Acetal is a conventional method for the chemical protection of hydroxyl groups. There are many ways to obtain the target hydroxyl compound by deprotection, and the most common method is reverse reaction under acid catalysis. However, for 1,3-dioxane compounds, due to the structural characteristics of the six-ring ring, its chemical properties are stable, especially when there is a methyl group on the carbon connected to the oxygen atom, it is easy to occur in an acid-catalyzed environment. side effects. Contents of the invention [0003] The object of the present invention is to provide a kind of 1,3-dioxane substituted by dimethyl to prepare the catalyst and application of monohydric alcohol and dihydric alcohol, utilize the solid hydrogenation catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J29/76B01J23/75B01J23/46B01J29/74C07C29/132C07C31/125C07C31/20
Inventor 刘新泰司君华黄胜飘徐德超宋琪
Owner 武汉椿岭科技有限公司
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