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Method for preparing modified 1,3-pentadiene petroleum resin by using composite catalyst

A technology of composite catalyst and petroleum resin, which is applied in the field of petroleum resin, can solve the problems of limited application, poor thermal oxygen stability of unsaturated double bonds, and low softening point, and achieve multiple active sites, excellent thermal oxygen aging resistance, and softening point height effect

Pending Publication Date: 2021-01-29
遂川海州树脂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Piperylene petroleum resin has many advantages, but at the same time, it also has disadvantages such as low softening point, unsaturated double bonds in molecular structure and poor thermal oxygen stability, which limit its application in many fields.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of method utilizing composite catalyst to prepare modified piperylene petroleum resin, comprises the following steps:

[0025] S1. Mix aluminum nitrate and anhydrous methanol evenly, add water and expanded graphite, stir and impregnate for 60 minutes, add ammonia water dropwise and stir for 10 minutes, sonicate for 60 minutes, wash and filter after standing, activate at 156°C for 120 minutes, then add sodium carbonate Immerse in the aqueous solution for 5 hours, dry in vacuum, and roast for 4 hours at 500°C under the protection of argon to obtain material A;

[0026] S2. Under the protection of argon, mix anhydrous aluminum trichloride and xylene, add to material A, heat to reflux, stir and react for 8 hours, filter, wash and dry after the reaction to obtain material B;

[0027] S3, material B, phosphoric acid and SbCl 3 Mix according to the weight ratio of 80:4:9 to obtain composite catalyst;

[0028] S4. Add cyclohexane into the reaction device, feed nitrogen...

Embodiment 2

[0031] A kind of method utilizing composite catalyst to prepare modified piperylene petroleum resin, comprises the following steps:

[0032] S1. Mix aluminum nitrate and anhydrous methanol evenly, add water and expanded graphite with an expansion volume of 400mL / g, stir and impregnate for 40 minutes, add ammonia water dropwise and stir for 20 minutes, wherein aluminum nitrate, anhydrous methanol, water, expanded graphite, The weight ratio of ammonia water is 2:200:1000:8:300, the drip rate of ammonia water is 3.5g / min, ultrasonic for 30min, the power of the ultrasonic is 550W, wash and filter after standing for 3h, and activate at 165°C for 130min , then add a sodium carbonate aqueous solution with a concentration of 1.5mol / L for immersion for 2 hours, vacuum dry and roast for 2 hours at 600°C under the protection of argon to obtain material A;

[0033] S2. Under the protection of argon, mix anhydrous aluminum trichloride and xylene, and add to material A, wherein, the weight ...

Embodiment 3

[0038] A kind of method utilizing composite catalyst to prepare modified piperylene petroleum resin, comprises the following steps:

[0039] S1. Mix aluminum nitrate and anhydrous methanol evenly, add water and expanded graphite with an expansion volume of 300mL / g, stir and impregnate for 46 minutes, add ammonia water dropwise and stir for 18 minutes, wherein aluminum nitrate, anhydrous methanol, water, expanded graphite, The weight ratio of ammonia water is 1.2:100:800:4:500, the drip rate of ammonia water is 5g / min, and the ultrasonic power is 500W for 38min. After standing for 5h, it is washed and filtered, and activated at 150°C for 180min. Then add a sodium carbonate aqueous solution with a concentration of 2mol / L for immersion for 4 hours, and after vacuum drying, roast for 3.3 hours at 520°C under the protection of argon to obtain material A;

[0040] S2. Under the protection of argon, mix anhydrous aluminum trichloride and xylene, and add to material A, wherein, the weig...

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PUM

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Abstract

The invention discloses a method for preparing modified m-pentadiene petroleum resin by using a composite catalyst. The method comprises the following steps: uniformly mixing aluminum nitrate and absolute methanol, adding water and expanded graphite for dipping, dropwise adding ammonia water, stirring, carrying out ultrasonic treatment, standing, washing, filtering, activating, adding into a sodium carbonate aqueous solution for dipping, drying and roasting to obtain a material A; under the protection of argon, mixing anhydrous aluminum trichloride and xylene, adding the mixture into the material A, heating to reflux, stirring, filtering, washing, drying, and mixing with phosphoric acid and SbCl3 to obtain a composite catalyst; and taking cyclohexane as a solvent, the composite catalyst asa catalyst, 1,3-pentadiene and styrene as raw materials, 2-methyl-1-butene and myrcene as monomers, carrying out polymerization reaction, carrying out after-treatment, mixing the obtained product with an antioxidant 1520, a light stabilizer Tinuvin 622LD, an antioxidant DTDTP, expandable graphite, molybdenum trioxide and N-phenyl-alpha naphthylamine, stirring at 160-180 DEG C, and cooling.

Description

technical field [0001] The invention relates to the technical field of petroleum resins, in particular to a method for preparing modified piperylene petroleum resins with a composite catalyst. Background technique [0002] Piperylene petroleum resin is a kind of C5 aliphatic petroleum resin. Because it has good compatibility with oils, greases and synthetic resins, it can be dissolved in many solvents. After mixing with other substances, it has good water resistance, Good acid resistance, low melting point, good adhesion, has been widely used in adhesives, coatings, rubber tires, paper and other industries. Piperylene petroleum resin has many advantages, but at the same time, it also has disadvantages such as low softening point and poor thermo-oxidative stability containing unsaturated double bonds in the molecular structure, which limits its application in many fields. Contents of the invention [0003] Based on the technical problems existing in the background technolo...

Claims

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Application Information

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IPC IPC(8): C08F236/10C08F212/08C08F210/14C08F236/22C08F4/02C08F4/20C08F4/14C08F4/08C08L47/00C08L67/02C08K13/04C08K7/24C08K3/22C08K5/18C08K5/372C08K5/375
CPCC08F236/10C08L47/00C08L2201/08C08K2003/2255C08F212/08C08F210/14C08F236/22C08L67/02C08K13/04C08K7/24C08K3/22C08K5/18C08K5/372C08K5/375C08F4/02C08F4/20C08F4/14C08F4/08
Inventor 肖奕萱
Owner 遂川海州树脂有限公司