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Preparation process of 1,2-cyclohexanediol diglycidyl ether

A technology of diglycidyl ether and cyclohexanediol, applied in organic chemistry and other directions, can solve the problem of high energy consumption and achieve the effects of low chromaticity, environmental protection comprehensive cost and low viscosity

Inactive Publication Date: 2011-10-19
武汉森茂精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing 1,2-cyclohexanediol diglycidyl ether process system uses 1,2-cyclohexanediol as raw material, first dissolves refined 1,2-cyclohexanediol in toluene, xylene, benzene, ethyl acetate Add appropriate amount of boron trifluoride diethyl ether complex as a catalyst in solvents such as esters, add a certain proportion of epichlorohydrin dropwise at an appropriate temperature, and after a certain period of reaction, remove excess epichlorohydrin under high temperature vacuum, drop 30 -40% by weight sodium hydroxide aqueous solution, carry out ring-closing reaction, after reacting for a certain period of time, divide the lye in the system, wash to neutrality, add an appropriate amount of solvent for extraction, obtain the target product after the upper layer extract is distilled to remove the solvent, and The main disadvantage is high energy consumption

Method used

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  • Preparation process of 1,2-cyclohexanediol diglycidyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Add 540 kg of water into the reaction kettle, add 10 kg of sulfuric acid as a catalyst, add 980 kg of epoxycyclohexane dropwise at 50°C, complete the dropwise addition within 1 hour, and hydrolyze for 2 hours to obtain cyclohexanediol The aqueous solution was transferred to the etherification tank by siphon, and 720 kg of solvent toluene was added, and azeotropic dehydration was carried out at 95°C for 6 hours. Hexylene glycol / toluene solution, boron trifluoride etherate complex was added thereto, 190 kg of epichlorohydrin was added dropwise at 55°C, the addition was completed within 2 hours, and the obtained intermediate solution was transferred to Wash the kettle with water, add 280 kg of sodium hydroxide solution with a mass percentage concentration of 30% dropwise, drop it at 50°C for 2 hours, react for 2 hours, let it stand to remove the lower layer of saline solution, add 200 kg of water, mix it well and then let it stand to remove The lower aqueous solution was r...

Embodiment 2

[0020] Add 540 kg of water into the reaction kettle, add 10 kg of sulfuric acid as a catalyst, add 980 kg of epoxycyclohexane dropwise at 55°C, complete the dropwise addition within 1.5 hours, and hydrolyze for 2 hours to obtain cyclohexanediol The aqueous solution was transferred to the etherification kettle by siphon, and 720 kg of solvent benzene was added, and azeotropic dehydration was carried out at 76°C for 7 hours. Hexylene glycol / benzene solution, adding boron trifluoride etherate complex therein, dripping 190 kilograms of epichlorohydrin at 60 ℃, adding dropwise within 1.5 hours, and transferring the intermediate solution obtained after reacting for 4 hours to Wash the kettle with water, add 280 kg of sodium hydroxide solution with a mass percentage concentration of 30% dropwise, drop it at 50°C for 2 hours, react for 2 hours, let it stand to remove the lower layer of saline solution, add 200 kg of water, mix it well and then let it stand to remove The lower aqueous ...

Embodiment 3

[0022] Add 540 kg of water into the reaction kettle, add 10 kg of sulfonic acid-based polystyrene gel-type acidic ion exchange resin as a catalyst, add 980 kg of epoxycyclohexane dropwise at 50°C, and complete the dropwise addition within 1 hour , hydrolysis reaction for 2 hours, the prepared cyclohexanediol aqueous solution was transferred to the etherification kettle by siphon, 720 kg of solvent xylene was added, and azeotropic dehydration was carried out at 120°C for 4 hours, the condensate was separated from the water by the oil-water separator, and the solvent was refluxed to the etherification kettle until no water is taken out to obtain a cyclohexanediol / xylene solution, to which boron trifluoride etherate complex is added, and 190 kg of epichlorohydrin is added dropwise at 50°C, within 1 hour After the addition is completed, the obtained intermediate solution is transferred to a washing kettle after 4 hours of reaction, and 280 kilograms of potassium hydroxide solution ...

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Abstract

The invention relates to a preparation process of 1,2-cyclohexanediol diglycidyl ether by epoxy cyclohexane, which comprises the following steps of: adding water into a reactor, adding an acid catalyst, dropwise adding the epoxy cyclohexane, and carrying out hydrolysis reaction to obtain an aqueous cyclohexanediol solution; transferring the aqueous cyclohexanediol solution to an etherification reactor, adding a solvent, carrying out azeotropic dehydration, and leading the solvent to flow back to the etherification reactor, thus obtaining a cyclohexanediol solution; adding a lewis acid catalyst, dropwise adding epichlorohydrin, reacting for 2-4 hours, and then transferring the intermediate solution to a rinsing kettle; and dropwise adding an alkaline solution, reacting, adding water, carrying out full mixing, standing for separating out a lower-layer aqueous solution, and transferring residual materials to a solvent removing kettle for removing the solvent, thus obtaining a target product, namely, the 1,2-cyclohexanediol diglycidyl ether. The target product has the advantages of high epoxide value, low viscosity, low chromaticity and low volatile matters, as well as the advantages of environment friendliness and low comprehensive cost as the process takes three industrial wastes as raw materials.

Description

technical field [0001] The invention relates to a process for preparing 1,2-cyclohexanediol diglycidyl ether from epoxycyclohexane. Background technique [0002] Existing 1,2-cyclohexanediol diglycidyl ether process is based on 1,2-cyclohexanediol as raw material, firstly the refined 1,2-cyclohexanediol is dissolved in toluene, xylene, benzene, ethyl acetate Add appropriate amount of boron trifluoride diethyl ether complex as a catalyst in solvents such as esters, add a certain proportion of epichlorohydrin dropwise at an appropriate temperature, and after a certain period of reaction, remove excess epichlorohydrin under high temperature and vacuum, and add dropwise 30 -40% by weight sodium hydroxide aqueous solution, carry out ring-closing reaction, after reacting for a certain period of time, divide the lye in the system, wash to neutrality, add an appropriate amount of solvent for extraction, obtain the target product after the upper layer extract is distilled to remove t...

Claims

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Application Information

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IPC IPC(8): C07D303/27C07D301/26
Inventor 黄茂喜吕佩田忠艳孙波
Owner 武汉森茂精细化工有限公司
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