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A kind of preparation method of c5/c10 copolymer resin

A technology of copolymer resin and distillate, which is applied in the field of preparation of C5/C10 copolymer resin, can solve the problems of indene resin preparation process and low intrinsic viscosity not introduced in detail, achieve excellent adhesive performance and compatibility, simple process, wide Promoting the effect of app prospects

Active Publication Date: 2018-10-19
HENGHE MATERIALS & SCI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN94110604.7 provides a kind of using liquid composite aluminum trichloride double cation complex (LAL) as catalyst, with C9 fraction rich in styrene and indene as raw material to prepare 11# color, which can be used for benzene in rubber tire industry The method of ethylene-indene resin; Lu Jingfeng et al. mentioned the use of petroleum cracking by-product C9 to produce styrene-indene resin with a softening point of 97°C and a color number of 12#; US4113931 provided a continuous production process for the preparation of indene resin by catalytic polymerization; Patent US2285416 provides a preparation method of coumarone-indene copolymer resin suitable for the field of adhesives; US4603186 provides a low intrinsic viscosity acrylonitrile-methyl methacrylate-methylstyrene / styrene-indene tetra The preparation method of meta-copolymer; JP2014237620A mentions the preparation of high-purity indene and indene resin, but does not introduce the preparation process of indene resin in detail

Method used

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  • A kind of preparation method of c5/c10 copolymer resin
  • A kind of preparation method of c5/c10 copolymer resin
  • A kind of preparation method of c5/c10 copolymer resin

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Experimental program
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Effect test

Embodiment 1-6

[0042] Effects of different raw material ratios on the properties of copolymer resin

[0043]

[0044] The default C10 raw material has been rectified by step (1) to cut off components with a boiling point of 140-210°C.

[0045] The reaction conditions are as follows: add 55wt% n-hexane solvent in advance to the reaction kettle, slowly add 0.5wt% boron trifluoride diethyl ether catalyst dropwise, and at the same time slowly add the above mixed polymerization raw materials. Then react at 10° C. for 2.5 hours to obtain a reddish-brown polymerization solution. The above polymerization liquid is washed with 5wt% NaOH aqueous solution at a temperature of 70°C to remove the catalyst, and then washed with water to neutrality to obtain a light yellow resin liquid; The solvent and oligomers are removed by distillation to obtain the copolymer resin.

Embodiment 7

[0047] 70wt% of C10 fraction A, 20wt% of C5 raw material 1 and 10wt% of C5 raw material 2 were mixed to obtain polymerization raw material B. Add toluene solvent accounting for 60wt% of the total material in advance in the high-pressure reactor with stirring, then slowly add the polymerization raw material B, and simultaneously add gaseous boron trifluoride catalyst accounting for 0.3wt% of the total material mass, and react at 10°C for 3 hours , to obtain a reddish-brown polymer solution. The above polymerization liquid is washed with 5wt% NaOH aqueous solution at a temperature of 70°C to remove the catalyst, and then washed with water to neutrality to obtain a light yellow resin liquid; The solvent and oligomers were removed by distillation to obtain a C5 / C10 copolymerized petroleum resin with a softening point of 105°C and a Gardner color number of 3.5#.

Embodiment 8

[0049]30wt% of C10 fraction A, 40wt% of C5 raw material 1 and 30wt% of C5 raw material 4 were mixed to obtain polymerization raw material B. In the autoclave with agitation, add in advance the n-pentane solvent accounting for 50wt% of the total material, then slowly add the polymerization raw material B, and add the anhydrous aluminum chloride catalyst accounting for 1.0wt% of the total material mass at the same time, at 50 ° C After reacting for 2.5 hours, a reddish-brown polymer solution was obtained. The above polymerization liquid is washed with 5wt% NaOH aqueous solution at a temperature of 90°C to remove the catalyst, and then washed to neutrality with water to obtain a light yellow resin liquid; The solvent and oligomers were removed by distillation to obtain a C5 / C10 copolymerized petroleum resin with a softening point of 101° C. and a Gardner color number of 5#.

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Abstract

The invention relates to a preparation method of C5 / C10 copolymer resin. The preparation method comprises the following steps: decompressing and rectifying an ethylene byproduct C10 fraction to intercept a C10 fraction A with a boiling point of 140 DEG C to 210 DEG C; then mixing the fraction A and a C5 fraction with the boiling point of 30 DEG C to 60 DEG C to obtain a polymerization raw material B; adding the polymerization raw material B into a solvent; then adding a Friedel-Crafts catalyst; reacting at -10 DEG C to 80 DEG C for 2.5h to 5h to obtain a polymerization liquid; and carrying out post-treatment to obtain the C5 / C10 copolymer resin. The C5 / C10 copolymer resin prepared by the preparation method has the advantages of good compatibility, shallow color and luster and adjustable softening point. The method is simple and convenient in process and is suitable for a plurality of types of C5 and C10 raw materials; and the preparation method has high operability and has wide popularization and application prospects.

Description

technical field [0001] The invention belongs to the field of petroleum resin preparation, in particular to a preparation method of C5 / C10 copolymer resin. 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] The by-product C5 fraction of ethylene has been widely used in resin synthesis, among which piperylene (PD) and cyclopentadiene (CPD) are the main monomers in petroleum resin synthesis. Ethylene by-product C10 fraction, that is, C10 raffinate oil, is obtained by cracking naphthalene fraction and extracting naphthalene, which contains indene, methyl-indene, methyl-styre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F240/00
CPCC08F240/00
Inventor 王斌孙向东贾立朋
Owner HENGHE MATERIALS & SCI TECH CO LTD