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Preparation method of low-hydrolysable chloride itaconic acid epoxy resin

A technology of chloritaconic acid epoxy resin and itaconic acid, which is applied in the direction of organic chemistry, can solve the problems of difficult control of one-time addition of alkali, high temperature of closed-loop reaction of alkali addition, and high hydrolyzed chlorine, so as to achieve narrow molecular weight distribution and reduce Side reaction, low viscosity effect

Active Publication Date: 2015-01-28
JINAN SHENGQUAN GROUP SHARE HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the high alkali-adding closed-loop reaction temperature existing in the above-mentioned prior art, the one-time alkali-adding reaction is difficult to control, and the shortcomings such as the high hydrolysis chlorine of the obtained itaconic acid epoxy resin, propose a kind of low hydrolysis chloroitaconic acid epoxy resin Preparation

Method used

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  • Preparation method of low-hydrolysable chloride itaconic acid epoxy resin
  • Preparation method of low-hydrolysable chloride itaconic acid epoxy resin

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 100g itaconic acid (Qingdao Langyatai product, content ≥99.6%), 1986g epichlorohydrin (Shandong Haili product, content ≥99.8%), and 0.05g tetraethylammonium chloride into a 2L reaction bottle, and stir at room temperature Dissolve for 30min. Then turn on the vacuum pump, use high-purity nitrogen to break the vacuum, discharge the material and the air in the reaction bottle, and replace the air twice. Introduce high-purity nitrogen gas, raise the temperature to 90°C under normal pressure, and react at constant temperature for 2 hours. Turn on the vacuum pump, depressurize and reflux, the vacuum degree is 130Torr, cool down to 60°C, add 64.5g of 50% NaOH solution dropwise within 6h, remove the water in the system by decompression and reflux during the dropwise addition, and heat up after the dropwise addition To 88 ° C, continue to react for 3 hours, remove part of the excess epichlorohydrin. Remove the remaining epichlorohydrin by rotary evaporation, add 429g o...

Embodiment 2

[0036] Add 100g itaconic acid (Qingdao Langyatai product, content ≥99.6%), 2065g epichlorohydrin (Shandong Haili product, content ≥99.8%), and 0.03g tetrabutylammonium bromide into a 2L reaction bottle, and stir at room temperature Dissolve for 30min. Then turn on the vacuum pump, use high-purity nitrogen to break the vacuum, discharge the material and the air in the reaction bottle, and replace the air twice. Introduce high-purity nitrogen, raise the temperature to 80°C under normal pressure, and react at constant temperature for 5 hours. Turn on the vacuum pump, depressurize and reflux, the vacuum degree is 115Torr, cool down to 55°C, add 68.9g of 50% KOH solution dropwise within 4h, remove the water in the system by decompression and reflux during the dropwise addition, and heat up after the dropwise addition At 90°C, continue the reaction for 3 hours to remove part of the excess epichlorohydrin. The remaining epichlorohydrin was removed by rotary evaporation, 463 g of me...

Embodiment 3

[0038] Add 100g itaconic acid (Qingdao Langyatai product, content ≥99.6%), 2120g epichlorohydrin (Shandong Haili product, content ≥99.8%), 0.04g benzyltrimethylammonium chloride into a 2L reaction bottle, Stir at room temperature to dissolve for 30 minutes. Then turn on the vacuum pump, use high-purity nitrogen to break the vacuum, discharge the material and the air in the reaction bottle, and replace the air twice. Introduce high-purity nitrogen, raise the temperature to 85°C under normal pressure, and react at constant temperature for 4 hours. Turn on the vacuum pump, depressurize and reflux, the vacuum degree is 110Torr, cool down to 53°C, add 72.3g of 50% KOH solution dropwise within 3h, remove the water in the system by decompression and reflux during the dropwise addition, and raise the temperature after the dropwise addition is completed At 80°C, continue the reaction for 3 hours to remove part of the excess epichlorohydrin. The remaining epichlorohydrin was removed b...

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Abstract

The invention discloses a preparation method of low-hydrolysable chloride itaconic acid epoxy resin. The method comprises the following steps: carrying out addition ring opening on raw materials comprising itaconic acid and epoxy chloropropane under the action of a catalyst under the protection of nitrogen to obtain a chlorohydrin ester structure intermediate, carrying out an alkali addition ring closing reaction to form an epoxy structure, and post-processing to obtain the low-hydrolysable chloride itaconic acid epoxy resin; and the alkali addition ring closing reaction is realized through carrying out reduced pressure refluxing under a vacuum degree of 100-150Torr, cooling to 40-60DEG C, adding an aqueous solution of an alkaline compound in a dropwise manner for 2-6h, carrying out reduced pressure refluxing in the dropwise addition process in order to remove water in a system, heating after the dropwise addition, and continuously carrying out a reduced pressure refluxing reaction for 1-3 to remove parts of excess epoxy chloropropane. The itaconic acid epoxy resin prepared through the method has the advantages of low hydrolysable chloride, narrow molecular weight distribution, low viscosity, high purity and the like, can be used as an epoxy resin diluent.

Description

technical field [0001] The invention belongs to the field of epoxy resin preparation, and in particular relates to a preparation method of low hydrolysis chloroitaconic acid epoxy resin. Background technique [0002] Bio-based polymer materials use renewable resources as the main raw material. While reducing the consumption of petrochemical products in the plastics industry, it also reduces the environmental pollution in the production process of petroleum-based raw materials. It is an important development direction of current polymer materials. It is also one of the important means to realize "energy saving and emission reduction" and develop "low-carbon economy", which has important practical value and broad development space. At present, the research on bio-based plastics is mainly limited to some natural polymers or thermoplastic materials such as starch plastics, cellulose-based materials, PLA, PHBV, etc. There are relatively few studies on bio-based thermosetting resi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/30C07D303/16C08G59/20
CPCC07D301/30C07D303/16C08G59/12
Inventor 江成真葛成利朱红军刘萌
Owner JINAN SHENGQUAN GROUP SHARE HLDG
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