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Method for preparing terpene resin

A technology of terpene resin and pinene, which is applied in the field of preparation of terpene resin, can solve the problems of hydrogenation catalyst poisoning, difficult industrial production, and high cost of hydrogenation, and achieve the effect of easy product, easy preparation, and no corrosion

Active Publication Date: 2009-10-14
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome in existing terpene resin preparation, with AlCl 3 and SbCl 3 When Lewis acid is used as a catalyst, it is easy to be wrapped by resin and difficult to clean, and the remaining catalyst will poison the hydrogenation catalyst and corrode the equipment, so that the cost of catalytic hydrogenation is too high and it is difficult to industrialize the technical deficiency of colorless terpene resin production. A new method for preparing terpene resin with heteropolyacid (salt) as catalyst

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0055] Add 0.30g of activated phosphotungstic acid to a dry three-necked flask, control the bath temperature between -17°C and -15°C, then add 5ml of toluene, and then take 5mL of β-pinene into a dry dropping funnel , Slowly drop into the reaction flask, about 1h drop. After mechanical stirring for 9 hours, methanol terminated the reaction. Filter the reaction mixture to recover the catalyst, wash a small amount of residual catalyst with an appropriate amount of ethanol, recover the solvent, unreacted monomer raw materials and oligomers by distillation, and vacuum-dry the residue at 50-80°C to obtain terpene as a colorless solid Vinyl resin. Resin yield: 34.56%.

Embodiment 2

[0057] Add 0.30g of activated phosphotungstic acid to a dry three-necked flask, control the bath temperature between -12°C and -10°C, then add 5ml of 1,2-dichloroethane, and then take 5mL of β-pinene In a dry dropping funnel, slowly drop it into the reaction flask, and drop it in about 1 hour. After mechanically stirring the reaction for 18 hours, the reaction was terminated with methanol. Filter the reaction mixture to recover the catalyst, wash a small amount of residual catalyst with an appropriate amount of ethanol, recover the solvent, unreacted monomer raw materials and oligomers by distillation, and vacuum-dry the residue at 50-80°C to obtain terpene as a colorless solid Vinyl resin. Resin yield: 60.85%

Embodiment 3

[0059] Add 0.30g of activated phosphotungstic acid to a dry three-necked flask, control the bath temperature between 10°C and 12°C, then add 5ml of dichloromethane, and then take 5mL of α-pinene into a dry dropping funnel , Slowly drop into the reaction flask, about 1h drop. After mechanical stirring for 9 hours, methanol terminated the reaction. Filter the reaction mixture to recover the catalyst, wash a small amount of residual catalyst with an appropriate amount of water, distill and recover the solvent, unreacted monomer raw materials and oligomers, and dry the residue under vacuum at 50-80°C to obtain terpene as a colorless solid Vinyl resin. Resin yield: 69.97%

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Abstract

The invention relates to a method for preparing terpene resin, which obtains the terpene resin by cation homo-polymerization or co-polymerization and taking Alpha-pinene, Beta-pinene, dipentene or pinene and the mixture of dipentene and styrene as raw materials and heteropoly acids or salts thereof as a catalyst. The Alpha-terpene resin and Beta-terpene resin prepared by the method both have the yield higher than 60 percent and the relative average molecular weight is around 800. Compared with the existing industrial production method, in which the catalyst is a metal halide, the method has the greatest advantages that: the product has light color; the traces of the residual catalyst in the terpene resin prepared do not cause catalyst poisoning in subsequent hydrogenation reaction, therebyhaving no or low erosion to equipment and low hydrogenation cost; the catalyst is easily to be separated and can be recycled for reusing, which lowers polymerization cost; the treatment after product ion is simple and does not generate a large amount of environment-polluting wastewater; the catalyst is easily to be prepared and is a fine-performance polymerization catalyst producing colorless terpene resin with low cost; and the prospect of industrial application is broad.

Description

technical field [0001] The invention relates to a method for preparing terpene resin, more specifically, the invention is a new method for preparing terpene resin by using heteropolyacid (salt) as a catalyst to catalyze the homopolymerization of pinene or copolymerization with other monomers. Background technique [0002] Terpene resin is a general term for polymers obtained by cationic catalytic polymerization of pinene as raw material. The common ones are α-pinene resin, β-pinene resin, dipentene resin, and polymers obtained by copolymerization of terpene and other monomers, such as terpene-styrene resin, terpene phenolic resin, etc. Terpene resin has excellent physical properties such as non-toxic, hydrophobic, non-crystallization, electrical insulation, strong adhesion, etc. and chemical properties such as acid and alkali resistance, anti-aging, etc. It is easily soluble in aromatic hydrocarbons and vegetable oils, and is an excellent tackifier. It is widely used in rub...

Claims

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Application Information

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IPC IPC(8): C08F32/04C08F2/06C08F4/22
CPCY02P20/584
Inventor 刘祖广朱华龙雷福厚
Owner GUANGXI UNIV FOR NATITIES
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