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Method for preparing dicyclopentadiene hydrogenated petroleum resin

A technology for hydrogenating petroleum resin and dicyclopentadiene is applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, catalyst carriers, etc. The problem of high hydrogenation temperature and pressure can achieve the effect of omitting the secondary hydrogenation process, reducing the unsaturated bond of the resin, and reducing the hydrogenation temperature and hydrogenation pressure.

Active Publication Date: 2012-07-11
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After using existing catalysts for hydrogenation, hydrogenated resins with ideal hue cannot be obtained, and the hydrogenation temperature and pressure are relatively high, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of catalyst

[0031] (1) Preparation of carrier

[0032] Weigh water 2000ml, 26% water glass 342g, 25% HNO 3 Add 145ml into the three-necked bottle, control the pH value to 8.0-8.4, raise the temperature to 45-55°C, and add 15% AlCl dropwise 3 Solution 3000ml and 11% NH 3 ·H 2 O solution 2150ml, control pH value 8.5~8.7, control AlCl 3 The flow rate is 90ml / min, the dropwise addition is completed, aged at 60°C for 30min, and filtered; put the filter cake into an autoclave, and add 87% NH 4 HCO 3 175g of the solution was heated to 130°C for 3 hours to crystallize, and then cooled to 60°C for aging for 30 minutes. Add 5000ml of water to the filter cake, stir at 60°C for 30 minutes, and filter; dry the filter cake at 150°C for 10 hours, and pulverize to obtain 342g of silicon-alumina macroporous oxide.

[0033] Take 300g of silicon aluminum oxide, Al 2 o 3200g, add 3% HNO 3 , 0.5% urotropine, 2.5% citric acid mixed solution 500ml, put into the kn...

Embodiment 2

[0039] The preparation of the carrier was the same as in Example 1. Take 0.82gPdCl 2 , add 60ml of 0.25% HCl, heat and boil for 30min, dissolve and cool to obtain PdCl 2 solution; take 70g carrier and put it into the dipping tank, pour the above PdCl 2 solution, soaked at 50°C for 60min; added 100ml of 5% hydrazine hydrate, and reduced at 50°C for 1h; then washed twice with 200ml of water, and the filter cake was dried at 120-150°C for 8-10 hours; calcined at 500-550°C for 6 hour, the finished catalyst is obtained, and the weight content of palladium in the catalyst is 0.7%.

[0040] In the 2L autoclave with stirring, add catalyst, through nitrogen replacement, hydrogen reduction, then add the dicyclopentadiene petroleum resin that dissolves with cyclohexane, solvent: resin: the weight ratio of catalyst is 200: 100: 5, with Hydrogen fully replaces the air in the kettle, then fills the hydrogen pressure to 3.5MPa, starts to heat up, and starts stirring. Control the reaction...

Embodiment 3

[0042] The preparation of the carrier was the same as in Example 1. Take 0.35gPdCl 2 , add 60ml of 0.25% HCl, heat and boil for 30min, dissolve and cool to obtain PdCl 2 solution; take 70g carrier and put it into the dipping tank, pour the above PdCl 2 solution, soaked at 50°C for 60min; added 100ml of 5% hydrazine hydrate, and reduced at 50°C for 1h; then washed twice with 200ml of water, and the filter cake was dried at 120-150°C for 8-10 hours; calcined at 500-550°C for 6 hour, the finished catalyst is obtained, and the weight content of palladium in the catalyst is 0.3%.

[0043] Add catalyst in the 2L autoclave with stirring, through nitrogen replacement, hydrogen reduction, then add the dicyclopentadiene petroleum resin that dissolves with cyclohexane, solvent: resin: the weight ratio of catalyst is 200: 100: 6, with Hydrogen fully replaces the air in the kettle, then fills the hydrogen pressure to 5.5MPa, starts to heat up, and starts stirring. Control the reaction ...

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Abstract

The invention relates to a method for preparing dicyclopentadiene hydrogenated petroleum resin. Dicyclopentadiene petroleum resin is used as a raw material and hydrogenated under the action of a catalyst to prepare the dicyclopentadiene hydrogenated petroleum resin, wherein the weight ratio of the dicyclopentadiene petroleum resin to the catalyst is 100: (3-6), the hydrogenating temperature is 170 to 215 DEG C, the pressure of the reaction hydrogen is 3.0 to 5.5MPa, and the reaction time is 4 to 8 hours; a silicon-aluminum composite oxide is used as a carrier in the catalyst, the active ingredient of the catalyst is Pd, the weight of the Pd is 0.1 to 1.0 percent of the weight of the catalyst, the specific surface of the catalyst is 350 to 420 m<2> / g, and the pore volume is 0.6 to 0.7ml / g;and according to the dicyclopentadiene hydrogenated petroleum resin product prepared by the method, the bromine number is less than or equal to 2.0gBr / 100g, the chromaticity (Gardner) is less than orequal to 1, and the softening point is 110 to 120 DEG C.

Description

technical field [0001] The invention relates to a method for preparing dicyclopentadiene hydrogenated petroleum resin by hydrogenating dicyclopentadiene petroleum resin. Background technique [0002] Dicyclopentadiene petroleum resin is obtained by thermal polymerization of dicyclopentadiene, which is a by-product of petroleum cracking to ethylene. It is a thermoplastic hydrocarbon resin with a relatively low number-average molecular weight. This type of resin has a deep hue. , high unsaturated hydrocarbon bond content, low thermal stability and oxidation stability, poor adhesion and other defects, it is not well compatible with many resin matrices, the effect of using it as a tackifier is poor, and it is not used directly. It needs to be modified to prepare high-grade petroleum resin. [0003] The simplest modification is resin hydrogenation. After hydrogenation, the unsaturation of petroleum resin is greatly reduced, the hue is light, and there is no special smell. It is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F240/00C08F8/04B01J23/44B01J32/00B01J21/12B01J35/10
Inventor 李正姜丹蕾付学红周亚婷周遵石王芳田艳明宋尚德刘绍岩刘玲
Owner PETROCHINA CO LTD
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