Preparation method of light-color cold polymerized C9 petroleum resin

A polycarbon nine petroleum and resin technology, applied in the preparation of carbon nine petroleum resin, can solve the problems of inability to obtain high-quality performance resin products, resin hue, poor compatibility, and inability to meet the needs of high-end markets, and achieve post-processing The effect of simple process, good compatibility and easy production process

Active Publication Date: 2014-01-29
HENGHE MATERIALS & SCI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The thermal polymerization process of C9 petroleum resin has the advantages of simple process, high conversion rate and output, and stable product performance. Its main defect is that it is impossible to obtain high-quality resin products. High-end market demand, generally only used in alkyd paint and rubber mixing and other fields, the product added value is low

Method used

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  • Preparation method of light-color cold polymerized C9 petroleum resin
  • Preparation method of light-color cold polymerized C9 petroleum resin
  • Preparation method of light-color cold polymerized C9 petroleum resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～6

[0056] Embodiment 1~6 depolymerization technology influences on fraction B

[0057]

[0058] DCPD*: High temperature depolymerization is mainly based on α-DCPD depolymerization, and this depolymerization rate corresponds to α-DCPD.

[0059] Examples 7 to 9 all use fraction C with the same content as the raw material to prepare cold polycarbonate nine resins. The material preparation process is: ethylene cracking fraction C9 is subjected to vacuum rectification at a vacuum degree of -0.085MPa, and the cut-off boiling point is 140-190°C C9 fraction A, wherein, the C9 fraction content is 0.8wt% cyclopentadiene, 5.3wt% styrene, 13.5wt% methylstyrene, 17.9wt% α-dicyclopentadiene, 8.8wt% indene, CPD- MCPD dimer, methylcyclopentadiene dimer (DMCPD) 22.1wt%, naphthalene 2.6wt%, and the rest are C8-C12 hydrocarbons;

[0060] Fraction A contains 0.5wt% cyclopentadiene, 4.2wt% styrene, 15.6wt% methylstyrene, 25.8wt% α-dicyclopentadiene, 15.0wt% indene, CPD-MCPD dimer, methyl Cyclope...

Embodiment 7

[0064] The fraction C obtained from the prepolymerization was mixed with the solvent toluene at a mass ratio of 1:1, and then used as a polymerization raw material, and put into a stirred polymerization reactor, and at -5°C, 1.5wt% of the total material was slowly added dropwise. Boronium diethyl ether catalyst was added dropwise for 1 hour, and then polymerized at 25° C. for 1 hour to obtain a polymerization liquid. Add a calcium hydroxide / methanol mixture 2.5 times the catalyst amount of boron trifluoride ether into the polymerization solution, stir thoroughly for 30 minutes, and then filter to obtain a resin solution. Distill the resin liquid under reduced pressure at -0.085 MPa to 130° C., and remove the solvent to obtain C9 petroleum resin with a softening point of 113° C. and Gardner color number 4#.

Embodiment 8

[0066] The fraction C obtained from the prepolymerization was mixed with the solvent toluene at a mass ratio of 2:1, and then used as a polymerization raw material, and put into a stirred polymerization reactor, and slowly added dropwise at a temperature of 15°C, accounting for 1.0wt% of the total material. The boroether catalyst was added dropwise for 1 hour, and then polymerized at 25° C. for 1 hour to obtain a polymerization solution. Add a calcium hydroxide / methanol mixture 2.5 times the catalyst amount of boron trifluoride ether into the polymerization solution, stir thoroughly for 30 minutes, and then filter to obtain a resin solution. The resin liquid was distilled to 130° C. under reduced pressure at a vacuum degree of -0.09 MPa, and the C9 petroleum resin with a softening point of 122° C. and a Gardner color number of 5# was obtained after the solvent was removed.

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Abstract

The invention relates to a preparation method of light-color cold polymerized C9 petroleum resin. The preparation method comprises the steps of: carrying out ethylene cracking to obtain a side product C9 fraction, intercepting a fraction A with boiling point of 150 to 190 DEG C, depolymerizing in a depolymerizing reactor at normal pressure to remove most of DCPD, DMCPD and CPD-MCPD dipolymer, thus obtaining a fraction B; processing the fraction B in a prepolymerization way under the Friedel-Crafts catalyst at common temperature, so as to obtain a fraction C; mixing the fraction C and a solvent based on the mass ratio of (1 to 3): 1 to obtain the product serving as the raw material, dropwise adding a boron trifluoride diethyl ether catalyst, and polymerizing for 1 hour at 10 to 25 DEG C, and then removing the catalyst to obtain a resin solution, and finally releasing the pressure and distilling to reach the temperature of 230 DEG C to remove the solvent, thus obtaining the C9 petroleum resin. The preparation method is simple and convenient to carry out, has mild reaction condition, and is suitable for C9 fractions with different components, and can be applied to industrial production; and the prepared C9 petroleum resin has light color phase, and high compatibility, and is suitable for the fields of adhesive, and ink, etc.

Description

technical field [0001] The invention belongs to the field of preparation of C9 petroleum resin, in particular to a preparation method of light-coloured cold poly C9 petroleum resin. Background technique [0002] Petroleum resin is a solid or viscous liquid polymer with relatively low molecular weight, which is obtained by polymerizing the by-product C5 / C9 fraction 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] Aromatic petroleum resin, also known as C9 petroleum resin, is obtained by polymerizing the above-mentioned ethylene by-product C9 distillate as a raw material. The raw material for its production is mainly the cracked C9 distillate oil produced by the ethylene plant, accounting for about 10% to 20% of the ethylene production. The distillate has complex components and is rich in unsat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F240/00C08F6/08
Inventor 孙向东王斌陈碧芬徐迪静
Owner HENGHE MATERIALS & SCI TECH CO LTD
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