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Synthesis of o-cresol formaldehyde epoxy resin

A novolac epoxy resin and a synthesis method technology, which is applied in the field of synthesis of o-cresol novolac epoxy resin, can solve the problem of no inert gas being injected into the recovered epichlorohydrin, and achieve a stable synthesis method, high epoxy value, The effect of low saponification chlorine

Inactive Publication Date: 2008-07-16
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The method for preparing o-cresol novolac epoxy resin at present mainly is to adopt two sections to add alkali to synthesize, do not use catalyzer, do not see and adopt negative pressure condition when epichlorohydrin dissolves o-cresol novolac resin (OCN), reclaim epichlorohydrin is not See report on inert gas bubbling

Method used

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  • Synthesis of o-cresol formaldehyde epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 100g of OCN and 400g of epichlorohydrin into a 5000ml four-neck flask, dissolve at 40°C for 3h at a vacuum of 0.1Mpa; add 0.1g of triethylamine, and etherify at 40°C and at a vacuum of 0.02MPa for 3h; At 40°C and a vacuum of 0.02MPa, 120g of 50% sodium hydroxide solution was added dropwise, and the addition was completed in 3 hours. The refluxed epichlorohydrin flowed back to the reactor in time to maintain the closed-loop reaction for 2 hours; the epoxychlorohydrin was recovered by heating to At 120°C, feed inert gas, adjust the flow rate of the inert gas according to the vacuum degree, keep the vacuum degree at 0.06Mpa, pass the inert gas for 1 hour, turn off the inert gas, and continue to recover until the final temperature is 130°C, and the vacuum degree is greater than 0.09Mpa; the recovery is completed Add 500g of toluene to dissolve for 0.5h, add 100g of 10% sodium hydroxide solution to refine and react for 5h at 75°C under normal pressure; add 300g of toluene...

Embodiment 2

[0037] Change the sodium hydroxide solution concentration of refining reaction into 30% in example 1, other conditions are constant, obtain EOCN139g.

[0038] It is determined that the softening point of the EOCN obtained in this example is 87° C., the epoxy equivalent is 195 g / eq, and the easily saponifiable chlorine is 455 ppm.

Embodiment 3

[0040] Add 100g of OCN and 600g of epichlorohydrin into a 5000ml four-neck flask, dissolve at 100°C for 0.5h at a vacuum of 0.05MPa; add 0.1g of benzyltriethylammonium chloride and 8g of 50% sodium hydroxide solution , Etherification at 75°C and a vacuum of 0.05MPa for 0.5h; dropwise adding 90g of 48% potassium hydroxide solution at 75°C and a vacuum of 0.05MPa for 3h, and maintain the ring closure reaction for 2h; heat to recover epichlorohydrin When the temperature reaches 125°C, feed the inert gas, adjust the flow rate of the inert gas according to the vacuum degree, keep the vacuum degree at 0.8Mpa, pass the inert gas for 2 hours, turn off the inert gas, and continue to recover until the final temperature is 200°C, and the vacuum degree is greater than 0.09Mpa; After the recovery, add 200g of butanol to dissolve for 1.5h, add 40g of 25% potassium hydroxide solution to undergo a refining reaction at 80°C and normal pressure for 3h; add 900g of xylene, then add 200g of deioni...

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Abstract

The invention provides a synthesis method of o-cresol formaldehyde epoxy resin, which comprises steps that: at 0.01-0.1Mpa vacuum degree, the o-cresol formaldehyde epoxy resin is dissolved by epichlorohydrin and a catalyzer is added for circumfluence and etherification reaction; at the 0.02-0.1Mpa vacuum degree, alkali is added for catalyzing cyclization reaction; the epichlorohydrin is recycled and processed after refining reaction. The o-cresol formaldehyde epoxy resin obtained by the synthesis method of the invention can reach a scheduled softening point and has high epoxy value and low content of easily saponifiable chlorine.

Description

technical field [0001] The present invention relates to a kind of synthetic method of organic polymer compound, relate in particular to a kind of synthetic method of o-cresol novolac epoxy resin (EOCN). Background technique [0002] Epoxy resins generally refer to organic polymer compounds containing two or more epoxy groups in the molecule. The molecular structure of epoxy resin is characterized by active epoxy groups in the molecular chain, and the epoxy groups can be located at the end, middle or ring structure of the molecular chain. Due to the active epoxy groups in the molecular structure, they can undergo cross-linking reactions with various types of curing agents to form insoluble, infusible high polymers with a three-dimensional network structure. [0003] EOCN belongs to novolac polyepoxy resin, which is a multifunctional epoxy resin and is in solid form at room temperature. Compared with bisphenol A epoxy resin, which belongs to glycidyl ether epoxy resin, the pr...

Claims

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Application Information

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IPC IPC(8): C08G59/08
Inventor 刘守贵蒲建光谭周琴张杰王平宋尚林
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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