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Method for preparing colorless terpene resin

A technology of terpene resin and resin, applied in the field of preparation of colorless terpene resin, can solve the problems of no mention of removal, no mention of color of terpene resin, easy discoloration of terpene resin, etc. Heat resistance and easy handling

Inactive Publication Date: 2005-12-21
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation method of the terpene resin disclosed in the above-mentioned documents 1-2 is to propose a new process for preparing a light-colored terpene resin with a high softening point and a high yield. The resin is easy to change color after storage; Documents 3 and 4 mention the hydrogenation of terpene resins, but do not mention the color of terpene resins after preparation

Method used

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  • Method for preparing colorless terpene resin
  • Method for preparing colorless terpene resin
  • Method for preparing colorless terpene resin

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1) Preparation of terpene resin

[0036] By weight of the total amount of material, 5% of SbCl 3 Put it into a reaction kettle filled with 2L of toluene, cool down to -20°C, and then add 0.5 to 10% of anhydrous AlCl 3 Molecular sieve (anhydrous AlCl 3 Molecular sieve is anhydrous AlCl with a particle size of 10-30 mesh 3 Dissolve in absolute ethanol, then put 5A molecular sieve into it and soak for one day, then vacuum dry under nitrogen protection) or AlCl with a particle size of 20-30 mesh 3 Put it into the reaction kettle, stir, slowly add β-pinene dropwise, control the rate of addition, make the temperature rise in the reaction kettle at 2-10°C, keep warm for 1 hour after the pinene is added dropwise, warm up to room temperature, filter, and use the filtrate Stir with 0.5N dilute hydrochloric acid for 1 hour, let stand, and separate the oil layer, wash the oil layer with water for 3 to 4 times, and check that there is no Cl in the washing solution - Ions, Al 3-...

Embodiment 2

[0040] 1) Preparation of terpene resin

[0041] 10% SbCl 3 Put it into a reaction kettle filled with benzyl chloride, cool down to 0~-30℃, and then add 0.5~10% anhydrous AlCl 3 Molecular sieves or granules in 20-30 mesh AlCl 3 Put it into the reaction kettle, stir, slowly add α-pinene dropwise, control the rate of addition, make the temperature rise in the reaction kettle at 5-12°C, keep warm for 1 hour after the pinene is added dropwise, warm up to room temperature, filter, and use the filtrate Stir with 1N hydrochloric acid for 0.5 hours, let it stand, and separate the oil layer, wash the oil layer with water 3 to 4 times, and check that the washing liquid is free of Cl - Ions, Al 3+ Until the ions are removed, the washed reactant is vacuum distilled to obtain a terpene resin.

[0042] 2) Catalytic hydrogenation

[0043] Put 400g of the above-mentioned terpene resin and 0.5gPd / c (5.0% palladium content) into a 2L autoclave, add 400ml of n-hexane, and carry out catalytic...

Embodiment 3

[0045] 1) Preparation of terpene resin

[0046] By weight of the total amount of material, 2% of SbCl 3 Put it into a reaction kettle filled with 2L xylene, cool down to -20°C in a cold trap, and then add 0.5 to 10% of anhydrous AlCl 3 Molecular sieves or granules in 20-30 mesh AlCl 3 Put it into the reaction kettle, stir, slowly add dipentene dropwise, control the dropping speed, make the temperature rise in the reaction kettle at 2-8°C, keep warm for 1 hour after dipentene is added dropwise, raise the temperature to room temperature, filter, and use the filtrate Stir with 0.5N dilute hydrochloric acid for 1 hour, let stand, and separate the oil layer, wash the oil layer with water for 3 to 4 times, and check that there is no Cl in the washing solution - Ions, Al 3+ The washed reactants are vacuum distilled to obtain dipentene resin.

[0047] 2) Catalytic hydrogenation

[0048] Put 400g of dipentene resin and 0.2gPd / c (5.0% palladium content) into a 2L autoclave prepared...

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Abstract

This invention relates to the method of preparing shallow color terpene resin through positive ion polymerization, then preparing colorless terpene resin through catalytic hydrogenation. The preparation process is: makes the ª‡-pinene, beta-pinene or dipentene obtained from fat turpentine or rectified fat turpentine as raw material, and obtain shallow color terpene resin through positive ion polymerization with proper catalyst and temperature, then catalyzation hydrogenate the obtained terpene resin to get colorless terpene resin. The purpose of the invention is to control the polyreaction speed through controlling the activeness of the catalyst in tepene resin preparation by positive polymerization, finally obtain terpene resin of shallow color, high softening point and obtaining rate; use carbon as catalyst, hydrogenate terpene resin under mild condition to get colorless terpene resin.

Description

Technical field [0001] The present invention relates to a preparation method of terpene resin, in particular to a preparation method of colorless terpene resin. Background technique [0002] Using turpentine as raw material, pinene is first separated, and then the polymer obtained by cationic catalytic polymerization is commonly known as terpene resin, which is usually a low-molecular thermoplastic resin. Common ones include α-pinene resin, β-pinene resin, dipentene resin and polymers copolymerized with other monomers, such as terpene-styrene resin, terpene phenolic resin, etc. These resins are mainly used as tackifiers. The agent is used in pressure-sensitive adhesives, hot melt adhesives, rubber, paints, inks, textiles, and can also be used in the food industry and other fields. However, the terpene resin currently produced from turpentine as raw material has a darker color, especially α-pinene resin, whose Ghanaian color number is greater than 5. When the dark terpene re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/08
Inventor 熊德元刘雄民
Owner GUANGXI UNIV
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