A kind of preparation method of high softening point hydrogenated petroleum resin

A technology of hydrogenated petroleum resin and high softening point, which is applied in the field of petroleum resin and can solve the problems of limited use and poor compatibility of substrates

Active Publication Date: 2021-08-20
HENGHE MATERIALS & SCI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the preparation method of the above-mentioned alicyclic C5 petroleum resin, the process flow of C5 thermal polymerization → cationic catalytic polymerization is generally adopted, and the softening point of the obtained resin is usually 80-120 °C, and the Gardner color number is 7-12#, Further hydrogenation treatment is required; and the resin molecule is dominated by polycyclic ring structures similar to polydicyclopentadiene (PDCPD), which has poor compatibility with various substrates, and its use in high-end applications is limited

Method used

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  • A kind of preparation method of high softening point hydrogenated petroleum resin
  • A kind of preparation method of high softening point hydrogenated petroleum resin
  • A kind of preparation method of high softening point hydrogenated petroleum resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The composition of C5 thermal dimerization ingredients is: 10.0wt% of cyclopentadiene, 7.0wt% of cyclopentene, 3.0wt% of n-pentene, 1.5wt% of 2-pentene, and the rest is diluting solvent methylcyclohexane.

[0032] C5 thermal dimerization ingredients were reacted in a stirred high-pressure polymerization kettle at a temperature of 250°C for 10 hours, and the obtained polymerization liquid was flashed at a vacuum degree of -0.090MPa and a temperature of 95°C to obtain light components C5 and heavy components C 10 Mixed ingredients. replace the above C 10 The mixed material was reacted at a temperature of 125°C for 36 hours under the action of anhydrous aluminum trichloride catalyst to obtain a polymerization reaction liquid; after that, the catalyst was removed by washing with 15% alkali solution, and washed repeatedly until it was neutral, then entered the rectification tower, and then Vacuum degree -0.085MPa, temperature 240 ℃ for rectification, the solvent can be reco...

Embodiment 2~5

[0034] Using different C5 ingredients, under the same thermal dimerization reaction conditions and resin hydrogenation process, the obtained C 10 The composition and properties of hydrogenated petroleum resin are as follows:

[0035]

[0036] C5 thermal dimerization to C 10 The reaction conditions are: temperature 245°C, reaction time 10h; flash vacuum degree -0.085MPa, temperature 110°C;

[0037]The hydrogenation process conditions are: hydrogenation temperature 275°C, pressure 15MPa, LSHV 0.5h -1 .

[0038] It can be seen from the above table that when the ratio of monoolefin / diolefin (O / D value) in the ingredients is larger, the probability of side reactions is lower, and the C in the product 10 The higher the ratio, the C 15 The lower the ratio. The ratio of CPD to cyclopentene, n-pentene, etc. in the proportion will directly affect the softening point and molecular weight distribution (Mw / Mn) of hydrogenated petroleum resin.

Embodiment 6~8

[0040] Using the same dark petroleum resin liquid to be hydrogenated, mixed with refined mineral oil with a distillation range of 280-350°C and a dynamic viscosity of 6.6cP at a mass ratio of 1:5.5 to obtain hydrogenation raw materials, and investigated the effects of different hydrogenation processes on hydrogenated petroleum resin The performance impact is as follows:

[0041]

[0042]

[0043] It can be seen from the above table that the hydrogenation temperature has the greatest influence on the hydrogenation decomposition rate of the resin, that is, the final softening point, which is the biggest influencing factor for the breaking of the molecular bonds of the resin, followed by the liquid hourly space velocity, and the reaction pressure has little influence on it. Liquid hourly space velocity (LHSV) is the biggest factor affecting the depth of hydrogenation reaction, and the color number is the lightest; the second is hydrogenation temperature and hydrogenation pre...

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Abstract

The invention relates to a preparation method of hydrogenated petroleum resin with a high softening point, which uses C5 olefins as raw materials and obtains C through high-temperature thermal polymerization. 10 、C 15 Polymer, and then catalyzed polymerization to obtain dark-colored petroleum resin; under the action of hydrogenation catalyst and certain hydrogenation process conditions, a high softening point hydrogenated petroleum resin is prepared. The hydrogenated petroleum resin prepared by the present invention has very high softening point and relatively low molecular weight, has excellent compatibility with amorphous α-olefin copolymer (APAO), and is suitable for BOPP film, sealant, paper Laminating agent, high-grade asphalt modifier and other fields.

Description

technical field [0001] The invention belongs to the field of petroleum resins, in particular to a method for preparing hydrogenated petroleum resins with a high softening point. Background technique [0002] Petroleum resin is a solid or viscous liquid medium-low relative molecular weight polymer obtained by catalyzed polymerization or free radical polymerization with the by-product C5 and C9 fractions of the ethylene plant as the main raw material. According to the monomer and molecular structure of the resin, it can be roughly divided into aromatic petroleum resin, aliphatic petroleum resin and alicyclic petroleum resin. [0003] Aliphatic petroleum resins and alicyclic petroleum resins are obtained through different C5 raw materials and polymerization processes respectively. The structure of the former is mainly linear alkanes with branched chain structure, and most of them are directly obtained by catalytic polymerization through Friedel-Crafts alkylation; The latter st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/04C08F240/00
CPCC08F8/04C08F240/00
Inventor 王斌孙向东贾立朋
Owner HENGHE MATERIALS & SCI TECH CO LTD
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