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Synthetic method for 2-methylallyl alcohol

A technology for the synthesis of methallyl alcohol and its synthesis method, which is applied in the field of synthesis of 2-methallyl alcohol and can solve the problem of low selectivity of 2-methallyl alcohol

Active Publication Date: 2014-02-19
SHANGHAI DUOLUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] What the present invention is to solve is the low selectivity problem of 2-methallyl alcohol existing in the prior art, and a kind of synthetic method of 2-methallyl alcohol is provided, and this method has 2-methallyl alcohol selectivity Advantages of high sex

Method used

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  • Synthetic method for 2-methylallyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1), preparation of catalyst

[0035] 850 grams of spherical γ-alumina with a diameter of 3 mm and 500 grams of nickel nitrate aqueous solution (calculated as NiO, containing 150 grams of NiO) were mixed, left to stand for 1 hour, dried at 80 ° C for 4 hours, and roasted at 500 ° C for 4 hours to obtain 1000g NiO / α-Al 2 o 3 Catalyst, the content of NiO in the catalyst is 15wt%.

[0036] (2), the synthesis of 2-methallyl alcohol

[0037] The fixed bed is loaded with the catalyst obtained by the above steps, the inert diluent is nitrogen, and the mol ratio of the inert diluent to 2-methyl-1,3-propanediol in the gas phase raw material is 3, and the gas phase raw material is 2-methyl-1,3 -Propylene glycol meter mass space velocity is 10 hours -1 , the reaction temperature is 320° C., the reaction pressure is 25 kPa, the reaction result is: the conversion rate of 2-methyl-1,3-propanediol is 95%, and the selectivity to 2-methallyl alcohol is 78.9%.

Embodiment 2

[0039] (1), preparation of catalyst

[0040] Mix 850 grams of spherical γ-alumina with a diameter of 3 mm and 500 grams of cobalt nitrate aqueous solution (calculated as CoO, including 150 grams of CoO), let it stand for 1 hour, dry at 80 ° C for 4 hours, and bake at 500 ° C in a nitrogen atmosphere 4 hours, get 1000 g CoO / α-Al 2 O3, CoO content in the catalyst is 15wt%.

[0041] (2), the synthesis of 2-methallyl alcohol

[0042] The fixed bed is filled with the catalyst obtained by the above steps, the inert diluent is nitrogen, and the mol ratio of the inert diluent to 2-methyl-1,3-propanediol in the gas phase raw material is 10, and the gas phase raw material is 2-methyl-1,3 -Propylene glycol meter mass space velocity is 10 hours -1 , the reaction temperature is 320° C., the reaction pressure is 25 kPa, the reaction result is: the conversion rate of 2-methyl-1,3-propanediol is 95%, and the selectivity to 2-methallyl alcohol is 80.0%.

Embodiment 3

[0044] (1), preparation of catalyst

[0045] Mix 950 g of spherical γ-alumina with a diameter of 3 mm with 500 g of NH 4 VO 3 Aqueous solution (in V 2 o 5 gauge, including V 2 o 5 A total of 50 grams) were mixed, left to stand for 1 hour, dried at 80°C for 4 hours, and roasted at 500°C for 4 hours to obtain 1000 grams of V 2 o 5 / α-Al 2 o 3 Catalyst, Catalyst V 2 o 5 The content is 5wt%.

[0046] (2), the synthesis of 2-methallyl alcohol

[0047] The fixed bed is filled with the catalyst obtained by the above steps, the inert diluent is nitrogen, and the mol ratio of the inert diluent to 2-methyl-1,3-propanediol in the gas phase raw material is 20, and the gas phase raw material is 2-methyl-1,3 -Propylene glycol meter mass space velocity is 10 hours -1 , the reaction temperature is 300° C., and the reaction pressure is 25 kPa. The reaction result is: the conversion rate of 2-methyl-1,3-propanediol is 95%, and the selectivity to 2-methylallyl alcohol is 80.0%.

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Abstract

The invention relates to a synthetic method for 2-methylallyl alcohol through a dehydration reaction of 2-methyl-1,3-propylene glycol. The synthetic method mainly overcomes the problem of low selectivity of 2-methylallyl alcohol in the prior art. According to the invention, a gas phase raw material containing 2-methyl-1,3-propylene glycol and an inertial diluent contacts with an alcohol dehydration catalyst in a fixed bed reactor and undergoes the dehydration reaction so as to produce a gas phase material containing 2-methylallyl alcohol; with such a technical scheme, the above-mentioned technical problem is overcome. The synthetic method provided by the invention is applicable to continuous industrial production of 2-methylallyl alcohol by using a fixed bed.

Description

technical field [0001] The invention relates to a synthesis method for preparing 2-methallyl alcohol by dehydrating 2-methyl-1,3-propanediol. Background technique [0002] 2-Methallyl alcohol is a very important organic intermediate, which itself can undergo self-polymerization and copolymerization reactions. Using 2-methallyl alcohol as the starting material, methacrylic acid and its esters can be prepared. In addition, 2-methallyl alcohol can also form allyl esters with other organic acids. Therefore, 2-methallyl alcohol is widely used in the fields of polymer monomers and surfactants. [0003] The earliest synthesis method of 2-methallyl alcohol is to prepare 2-methallyl chloride by hydrolysis under alkaline conditions. Subsequently, US2072015, US2323781, JP2009107949, etc. have improved and perfected this method. At present, the hydrolysis method is the most important method for producing 2-methallyl alcohol, and this method is the main method in industry. Although ...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C29/60
CPCC07C29/60C07C33/03
Inventor 陈建华林真意朱学文舒建生徐兴建李文贡
Owner SHANGHAI DUOLUN CHEM