Synthesizing method of 2-methallyl alcohol

The technology of a kind of methallyl alcohol and synthetic method is applied in the synthetic field of 2-methallyl alcohol, can solve the problems such as raising production cost, high production cost, difficult DMF solvent, reaches the generation that avoids by-product ether, The effect of avoiding post-treatment process and improving reaction selectivity

Inactive Publication Date: 2010-06-30
宁波尖锋紫星生物科技有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] US2323781 uses electrolytic copper to assist the hydrolysis of potassium carbonate; the production cost of this method is relatively high, and the reaction process will produce difficult-to-treat copper-containing wastewater
[0005] US2313767 proposes to hydrolyze under the presence of surfactant pulling powder such as sodium naphthyl sulfonate. This production method needs to use relatively high price pulling powder such as sodium naphthyl sulfonate, which increases the production cost and the target product yield lower
[0006] JP2009107949 uses DMF to promote hydrolysis in order to avoid the use of heavy

Method used

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  • Synthesizing method of 2-methallyl alcohol

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Embodiment

[0031] The polyethylene glycol (PEG) used in the experiment of the embodiment adopts PEG-6000.

[0032] (1) Add 1000ml of water, 30g of sodium hydroxide (96% content), 240g of 2-methallyl chloride, and 0.5g of PEG-6000 to a 2L reaction flask in sequence; heat and reflux the reaction system obtained above, and prepare another 120g of sodium hydroxide dissolved in 200ml of aqueous hydroxide liquid solution in 200ml of water, within 5.5 hours, the above prepared sodium hydroxide aqueous solution was added dropwise to the reaction system heated to reflux; through GC detection, the 2-methylene in the reaction solution When the content of propyl chloride is less than 0.2%, the reaction is finished, the reaction time is 6.5h, and the volume of the reaction system is 1400ml;

[0033] (2) The reaction solution after the above-mentioned reaction is cooled, left to stand, layered, and the obtained organic layer is about 150g; the organic layer is dried and dehydrated with anhydrous sodiu...

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Abstract

The invention discloses a synthesizing method of 2-methallyl alcohol, comprising the following steps of: sequentially adding water, solid base, 2-methallyl chloride and polyethylene glycol to a reaction vessel, then refluxing by heating, and dripping an aqueous alkali solution with the concentration of 1-50 percent; (2) after reaction is completed, cooling, standing and demixing a reaction solution to obtain an organic layer and a water layer, drying and dewatering the organic layer, decoloring by activated carbon, filtering to obtain a target product, and circularly using filter liquor obtained by filtering and desalting the water layer as a new reaction solvent for preparing the 2-methallyl alcohol; and (3) adding the 2-methallyl chloride to the circularly used reaction solvent, and complementally adding the polyethylene glycol, the water and the base to perform new reaction for preparing the 2-methallyl alcohol, wherein the filter liquor obtained by filtering the water layer in each reaction is always circularly used as a next new reaction solvent. The synthesizing method of the 2-methallyl alcohol has the advantages of low production cost, high target product yield, low energyconsumption and little pollution.

Description

technical field [0001] The present invention relates to a kind of synthetic method of 2-methallyl alcohol. Background technique [0002] 2-methallyl alcohol (also known as 2-methallyl alcohol, isobutenol or methallyl alcohol) is an important intermediate, widely used in polymer monomers, surfactants and other fields. Generally adopt hydrolysis to prepare 2-methallyl alcohol, the earliest method appears in Sheshukov et al published, J Russ. Later, there are many improved methods on this basis, such as: [0003] US2072015 proposes hydrolysis at 120°C, under the catalysis of sodium hydroxide or sodium carbonate, at 5 atmospheres; this synthesis method needs to realize the reaction under high pressure conditions, and has high requirements for equipment. [0004] US2323781 uses electrolytic copper to assist the hydrolysis of potassium carbonate; the production cost of this method is relatively high, and the reaction process will produce difficult-to-treat copper-containing wast...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C29/09
Inventor 杨志杰余巍峰徐亚萍张华星骆成才陈金虎
Owner 宁波尖锋紫星生物科技有限公司
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