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A kind of decolorization method of hydrocarbon-phenol type resin

A phenolic and resin technology, applied in the field of decolorization of hydrocarbon-phenolic resins, can solve the problems of poor marking, low operation efficiency, inability to guarantee product qualification, etc., and achieve the effect of reducing usage and reducing reaction time.

Active Publication Date: 2020-08-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If colored epoxy resin is used as the sealing material, marking is poor and work efficiency is low
Although it has been proposed that DCPD-phenol resin with good color tone can be directly synthesized, it cannot guarantee that all products are qualified, and there will still be some batches with significant coloring

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Dissolve 500g of DCPD-phenol resin with a Gardner color number of 18 or more in 750g of toluene, add 35g of dioxane, heat to 45°C in a nitrogen atmosphere, add 10g of 325 mesh zinc powder, react for 0.5 hours, and heat up to The decolorization reaction was carried out at 92° C. for 1.2 hours to obtain a solid-liquid mixture.

[0047] The above-mentioned solid-liquid mixture was filtered to obtain the filtrate and the zinc powder residue, and the zinc powder residue was dried to obtain 9.4 g of zinc powder.

[0048] The above filtrate was distilled under reduced pressure at -0.095MPa and 160°C to obtain decolorized DCPD-phenol resin.

[0049] After calculation, the decolorized DCPD-phenol resin is 493g. The decolorized DCPD-phenol resin has a Gardner color number of 12-13, light yellow, light coloring and good chroma.

Embodiment 2

[0051] Dissolve 500g of DCPD-phenol resin with a Gardner color number of 18 or more in 750g of toluene, add 35g of dioxane, heat to 45°C in a nitrogen atmosphere, add 10g of 325-mesh zinc powder (including the one recovered in Example 1) 9.4g of zinc powder), reacted for 0.5 hours, raised the temperature to 92°C for decolorization reaction for 1.2 hours, and obtained a solid-liquid mixture.

[0052] The above-mentioned solid-liquid mixture was filtered to obtain the filtrate and the zinc powder residue, and the zinc powder residue was dried to obtain 9.8 g of zinc powder.

[0053] The above filtrate was distilled under reduced pressure at -0.095MPa and 160°C to obtain decolorized DCPD-phenol resin.

[0054] After calculation, the decolorized DCPD-phenol resin is 493g. The decolorized DCPD-phenol resin has a Gardner color number of 12-13, light yellow, light coloring and good chroma.

Embodiment 3

[0056]Dissolve 500g of α-pinene-tert-butylphenol resin with a Gardner color number of 18 or more in 800g of methyl isobutyl ketone, add 37g of propylene glycol methyl ether, heat to 50°C in a nitrogen atmosphere, and add 100 mesh 11 g of aluminum powder was reacted for 0.5 hours, and the temperature was raised to 95° C. for decolorization reaction for 1.5 hours to obtain a solid-liquid mixture.

[0057] The above solid-liquid mixture was filtered to obtain the filtrate and the aluminum powder filter residue, and the aluminum powder filter residue was dried to obtain 10.3 g of aluminum powder.

[0058] The above filtrate was distilled under reduced pressure at -0.1MPa, 200°C to obtain the decolorized α-pinene-tert-butylphenol resin.

[0059] After calculation, the α-pinene-tert-butylphenol resin after decolorization is 490g, and the Gardner color number of the α-pinene-tert-butylphenol resin after decolorization is 13~14, light brown, light colored, color The degree is good. ...

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Abstract

The invention provides a decolorization method for hydrocarbon-phenol resin. The decolorization method comprises the following steps: dissolving the hydrocarbon-phenol resin in a solvent, adding a polar auxiliary agent, carrying out heating to 30 to 50 DEG C in a protective gas atmosphere, adding reductive metal, carrying out a reaction for 0.2 to 1 hour, carrying out heating to 65 DEG C or above,and carrying out a decolorization reaction for 1 to 3 hours so as to obtain a solid-liquid mixture; filtering the solid-liquid mixture so as to obtain a filtrate and reductive metal filter residues;and subjecting the filtrate to reduced pressure distillation under a pressure of minus 0.1 MPa to 0 MPa at 150 to 200 DEG C so as to obtain decolorized hydrocarbon-phenol resin. The decolorization method provided by the invention has the following advantages: significantly-colored hydrocarbon-phenol resin can be decolorized; the decolorized hydrocarbon-phenol resin has good hue; meanwhile, a decolorizing adsorbent is recyclable.

Description

technical field [0001] The invention relates to the field of resin synthesis, in particular to a method for decolorizing hydrocarbon-phenol resins. Background technique [0002] Dicyclopentadiene (DCPD) is a by-product C in the process of petroleum cracking 5 One of the main components of the distillate, it has extremely high reactivity. The structure of DCPD-phenol resin produced by the reaction of it with phenolic substances contains multiple functional groups such as phenolic hydroxyl group, benzene ring, five-membered ring, and six-membered ring, and has good electrical insulation, heat resistance and chemical reactivity. DCPD-phenol epoxy resin synthesized from DCPD-phenol resin is also a high-end product in the industry at present, and is widely used in electronic packaging, PCB ink and other fields. [0003] The synthesis method of DCPD-phenol resin is mainly: in the presence of BF3 complex (such as BF3-phenol, etc.) catalyst, DCPD is added dropwise to phenolic comp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G61/02C07D303/27C07D301/32
Inventor 杨鑫贺谷辉肖雄任六波潘卫章傅江福
Owner CHINA PETROLEUM & CHEM CORP