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Method for efficiently preparing alkynol

An alkynol, high-efficiency technology, applied in the field of chemical intermediates and chemical preparation, can solve problems such as low conversion rate, and achieve the effects of high conversion rate, good product purity, and safe operation

Active Publication Date: 2018-11-23
PANJIN GELIN KAIMO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction has a low conversion rate due to the reaction with water

Method used

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  • Method for efficiently preparing alkynol
  • Method for efficiently preparing alkynol
  • Method for efficiently preparing alkynol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1, preparation methyl butynyl alcohol

[0037] In a 10L three-necked flask, 6L of anhydrous methanol was added, protected by nitrogen, and 550g of sodium metal (small pieces) was slowly added under ice-water cooling. After the sodium metal is completely dissolved, add 1.5 L of acetone, stir evenly, and cool to below 0°C. Slowly feed acetylene, and control the flow of acetylene so that the reaction temperature is preferably at 0-5°C. When the reaction is no longer exothermic, it is the end of the reaction. Then feed a small amount of acetylene, and react for 0.5 hours under airtight micro-positive pressure (the nitrogen balloon does not become larger).

[0038] In another 20L three-necked flask, add 2.5 kg of ammonium chloride and 3L of methanol. Under ice water cooling, the reaction solution was poured into the ammonium chloride system for neutralization reaction. Control the neutralization reaction temperature to less than 20°C. After neutralization, fi...

Embodiment 2

[0039] Embodiment 2, preparation methyl butynol

[0040] In a 500L stainless steel reaction kettle, 300L of anhydrous methanol was added under nitrogen protection. Under jacket frozen brine cooling, slowly add metal sodium block 20kg. After the metallic sodium is completely dissolved, add 55 L of acetone, stir evenly, and cool to below 0°C. Slowly feed acetylene, and control the flow of acetylene so that the reaction temperature is preferably at 0-5°C. When the reaction is no longer exothermic, it is the end of the reaction. Then a small amount of acetylene was passed through, and the airtight micro positive pressure was reacted for 1 hour. In another 1000L glass-lined reactor, add 150 kg of ammonium chloride and 300L of methanol. Under the cooling of frozen brine, the reaction liquid is pumped into the ammonium chloride system for neutralization reaction. Control the neutralization reaction temperature to less than 20°C. After neutralization, filter. The filtrate was f...

Embodiment 3

[0041] Embodiment 3, preparation methyl butynol

[0042] In a 500L stainless steel reaction kettle, 300L of anhydrous tert-butanol was added under nitrogen protection. Under jacket frozen brine cooling, slowly add metal potassium block 20kg. After the potassium metal is completely dissolved, add 33 L of acetone, stir evenly, and cool to below 0°C. Slowly feed acetylene, and control the flow of acetylene so that the reaction temperature is preferably at 0-5°C. When the reaction is no longer exothermic, it is the end of the reaction. Then a small amount of acetylene was passed through, and the airtight micro positive pressure was reacted for 1 hour. In another 1000L glass-lined reactor, add 100 kg of ammonium chloride and 200L of methanol. Under the cooling of frozen brine, the reaction liquid is pumped into the ammonium chloride system for neutralization reaction. Control the neutralization reaction temperature to less than 20°C. After neutralization, filter. The filtrat...

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Abstract

The invention relates to a method for efficiently preparing alkynol, belongs to the field of preparation of chemical intermediates and chemicals, and particularly relates to a preparation method of alkynol. The preparation method comprises the following steps that 1, alkali metal is added into an anhydrous alcohols solvent; an alcohol-alkali metal solution is prepared; 2, a compound I is added into the alcohol-alkali metal solution; uniform stirring is performed; cooling is performed to be 0 DEG C or below; 3, acetylene is introduced through being metered at normal pressure; alkynol is obtained; 4, the alkynol solution after reaction is neutralized by ammonium chloride and a same alcohol mixed suspension system; 5, the neutralized mixed suspension system is filtered; after alcohols are recovered from filter liquid, reduced pressure distillation is performed to obtain an alkynol product. The method overcomes the defect that under the existing harsh reaction conditions of high pressure,liquid ammonia and the like, the solid potassium hydroxide feeding difficulty is avoided; under the ordinary pressure condition, the ketone compounds are converted into alkynol at high conversion rate. The method has the advantages of high conversion rate, simple process and good product purity.

Description

technical field [0001] The invention belongs to the field of chemical intermediates and chemical preparation, and in particular relates to a preparation method of acetylenic alcohol. Background technique [0002] The existing mature production method of acetylenic alcohols is to react with aldehydes and ketones to obtain acetylenic alcohols in a high-pressure pressure vessel using an ammonia-acetylene system as a catalyzer. This method has a high conversion rate, but dangerous high-pressure reaction conditions are used, and there is a problem of difficult addition of solid potassium hydroxide. [0003] DSM's patent CN1558888A uses a tubular reactor for high-pressure reaction. Under the condition of immobilizing the basic resin system in the tubular reactor, ammonia-acetylene is used to drive the aldehyde or ketone to react under pressure in the tubular reactor to obtain the acetylenic alcohol. This method must be carried out under high pressure conditions. [0004] DSM pa...

Claims

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Application Information

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IPC IPC(8): C07C29/44C07C33/042C07C33/28C07C33/048C07C35/17C07C33/30
CPCC07C29/44C07C33/042C07C33/28C07C33/048C07C35/17C07C33/30
Inventor 宫宁瑞
Owner PANJIN GELIN KAIMO TECH CO LTD
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