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Method for synthesizing polyepichlorohydrin

A technology of polyepichlorohydrin and epichlorohydrin, which is applied in the field of synthesis of polyepichlorohydrin, and can solve cumbersome problems

Inactive Publication Date: 2015-03-25
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the large amount of impurities produced by the synthesis of polyepichlorohydrin in the prior art, reduce the complicated process and improve the quality of polycyclic compounds

Method used

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  • Method for synthesizing polyepichlorohydrin

Examples

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example 1

[0023] In the 100mL four-necked flask, drop into the chloropropane of 30g and the catalyst of 6.5g (phosphotungstopolyacid / TiO 2 ), then add 10mL of hydrogen peroxide and 5g of diamine hydrogen phosphate under stirring state, and react for 6 hours under reflux of chloropropane. After the reaction was completed, the system was separated into oil and water phase suspensions after standing for 1 hour; the oil layer was separated by distillation to obtain 23.36 mL of epichlorohydrin for future use. Then add 5g of diethylaluminum chloride and 50ml of anhydrous diethyl ether dried over molecular sieves to a three-necked flask equipped with a stirring bar, and stir for 10 minutes at room temperature, cool the stirred solution to 0°C with ice-salt water, and Add 10 mL of propylene oxide dropwise. By controlling the dropping rate to 1 drop / sec and maintaining the temperature at 5 °C. After reacting for 30 minutes, the volatile matter was extracted in time, and then 20 mL of pre-prepa...

example 2

[0025] Put 30g of chloropropane and 6.5g of catalyst (phosphotungstic heteropolyacid / Ti02) into a 100mL four-neck flask, then add 10mL of hydrogen peroxide and 5g of diamine hydrogen phosphate under stirring, and react under reflux of chloropropane for 6 hours. After the reaction was completed, the system was separated into oil and water phase suspensions after standing for 1.5 hours; the oil layer was separated by distillation to obtain 23.36 mL of epichlorohydrin for future use. Then add 5g of diethylaluminum chloride and 50ml of anhydrous diethyl ether dried by molecular sieves to the three-necked flask equipped with a stirrer, and stir at room temperature for 10 minutes, cool the stirred solution to 10°C with ice-salt water, Add 10 mL of propylene oxide dropwise. By controlling the dropping rate to 1 drop / sec and maintaining the temperature at 0 °C. After reacting for 30 minutes, the volatile matter was extracted in time, and then 20 mL of pre-prepared epichlorohydrin was...

example 3

[0027] In the 100mL four-necked flask, drop into the chloropropane of 30g and the catalyst of 6.5g (phosphotungstopolyacid / TiO 2 ), then add 10mL hydrogen peroxide and 5g diamine hydrogen phosphate under stirring state, and react for 6 hours under the reflux of chloropropane; after the reaction is completed, the system is divided into oil and water phase suspensions after standing for 1-2 hours; the oil layer is obtained by separating the essence 23.36mL of epichlorohydrin for use. Then add 5g of diethylaluminum chloride and 50ml of anhydrous diethyl ether dried over molecular sieves to a three-necked flask equipped with a stirring bar, and stir for 10 minutes at room temperature, cool the stirred solution to 0°C with ice-salt water, and Add 10 mL of propylene oxide dropwise. By controlling the dropping rate to 1 drop / sec and maintaining the temperature at 20 °C. After reacting for 30 minutes, the volatile matter was extracted in time, and then 20 mL of pre-prepared epichlor...

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Abstract

The invention discloses a method for synthesizing polyepichlorohydrin. The method comprises the following steps: catalyzing chloropropane by using a catalyst and additives, thereby obtaining epoxy chloropropane for later use; sequentially adding diethyl aluminum chloride and absolute ether into a three-opening flask with a stirrer, stirring for 10 minutes, cooling to be 0 DEG C, dropwise adding epoxypropane to react for 30-50 minutes, sucking out the volatile matters in time, further adding a methanol solution containing sodium hydroxide, stirring at normal temperature for 50 minutes, and stopping the reaction; moving the reaction mixture into a liquid separation funnel, washing, layering, and washing the obtained coarse product by using 5% hydrochloric acid, 5% sodium bicarbonate and distilled water till being neutral; and reducing the pressure by using a rotational evaporator, thereby obtaining 8.23g of polyepichlorohydrin. The polyepichlorohydrin yield is greater than 84.9%.

Description

technical field [0001] The invention belongs to the field of polymerization reaction and relates to a synthesis method of polyepichlorohydrin. Background technique [0002] Polyepichlorohydrin is light yellow to amber viscous liquid or solid. It is formed by the ring-opening polymerization of epichlorohydrin. Polyepichlorohydrin has the advantages of oil resistance, acid resistance, etc., and has outstanding resistance to gas penetration. Its shock absorption and high temperature resistance are also good, and it has good adhesion. The photoresist with excellent performance can be made by treating polyepichlorohydrin with cinnamic acid. Polyepichlorohydrin can be used to make sealing gaskets and oil-resistant hot melt adhesives, seawater-resistant, oil-resistant adhesives, etc., as well as flame-retardant, water-resistant, oil-resistant polyurethane adhesives and coatings. The ring-opening polymerization products of epoxy compounds are increasingly important as intermedia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
Inventor 陈兴权
Owner CHANGZHOU UNIV
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