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A method for purification and enhanced stability of alkynol compounds

A compound and stability technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of unqualified appearance, low added value, and low purity of alkynyl alcohol compounds

Inactive Publication Date: 2012-10-03
河北百灵威超精细材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to provide a method for purifying and enhancing the stability of the acetylenic alcohol compound with the following general formula, which solves the problems of low purity, unqualified appearance and low added value of the acetylenic alcohol compound produced by the existing technology

Method used

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  • A method for purification and enhanced stability of alkynol compounds
  • A method for purification and enhanced stability of alkynol compounds
  • A method for purification and enhanced stability of alkynol compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: Preparation of 1-ethynyl-1-cyclohexanol

[0026] Add 150L tetrahydrofuran to the reaction kettle, add 22.4Kg of potassium tert-butoxide under stirring, cool to 0°C, pass acetylene gas, control the temperature below 5°C, and ventilate for 4 hours, add cyclohexanone 19.8Kg dropwise while passing acetylene gas , After the addition, the reaction was stirred for 2 hours, and the temperature was controlled below 0°C. The reaction solution was poured into ice water, the aqueous layer was extracted with dichloromethane, the organic layers were combined, dried over anhydrous sodium sulfate, concentrated, and distilled under reduced pressure to collect fractions at 52-54°C / 2mm. 21.7Kg of light yellow liquid was obtained, the yield was 87.5%, and the purity was 95% (detected by GC method).

Embodiment 2

[0027] Example 2: Purification of 1-ethynyl-1-cyclohexanol

[0028] Crude product input and yield

[0029]

[0030] Add water to the reaction bottle, then add sodium bisulfite, and after it is completely dissolved, add crude 1-ethynyl-1-cyclohexanol to the reaction solution.

[0031] Heat and stir for 1 hour to stop the reaction. Static separation, the organic layer was collected, the aqueous layer was extracted with ethyl acetate, the organic layers were combined, concentrated, and distilled to obtain a qualified product.

Embodiment 3

[0032] Example 3: Enhancement of the stability of 1-ethynyl-1-cyclohexanol

[0033] Qualified 1-ethynyl-1-cyclohexanol was examined under the following conditions respectively.

[0034]

[0035]

[0036] Results: The stability of 1-ethynyl-1-cyclohexanol can be greatly enhanced and the quality can be improved by adding polymerization inhibitor.

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Abstract

The invention relates to a method for purification and enhanced stability of alkynol compounds. The invention is characterized by including the following steps successively: adding potassium tert-butoxide to tetrahydrofuran, feeding acetylene gas after cooling to obtain potassium acetylide, adding ketone dropwise, pouring the reaction solution into water and getting the alkynol by hydrolyzing, removing the unreacted ketone in the crude alkynol with sodium bisulfite, distilling to obtain a product with purity over 99%, and adding a polymerization inhibitor to the qualified alkynol product to enhance the stability. The method help to solve the problems that the alkynol products produced in the prior art are low in purity, unqualified in appearance, and low in additional value.

Description

technical field [0001] The invention relates to a method for purifying and enhancing stability of acetylenic alcohol compounds. Background technique [0002] The acetylenic alcohol compounds with the following structure are a series of important fine chemical products widely used in the fields of medicine, synthetic materials, petrochemical industry and so on. Its main uses are: (1) used as an intermediate for the synthesis of medicines, pesticides, and terpene spices (2) used as a stabilizer for the storage and production of addition-type silicone rubber, and as an inhibitor of hydrosilylation reactions; (3) used as Used as drier for ink, paint and coating; (4) used as glazing agent for nickel plating or copper; (5) used as acid corrosion inhibitor, viscosity stabilizer, viscosity reducer, etc. [0003] [0004] Alkynyl alcohol compounds usually have the following several synthetic methods: [0005] (1) Potassium acetylene is prepared by passing acetylene gas into a te...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/042C07C35/06C07C35/17C07C29/80C07C29/94
Inventor 邢靓邓雄飞张东峰毕志强柯伟伦
Owner 河北百灵威超精细材料有限公司
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