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Preparation method of hydrogenated C9 petroleum resin

A technology of C9 petroleum resin and resin, which is applied in the field of preparation of hydrogenated C9 petroleum resin, can solve the problems of hydrogenated resin limitation, high impurity content of petroleum resin, etc., achieve low bromine index, high softening point, and good process stability Effect

Active Publication Date: 2012-07-25
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the current development of C9 petroleum resin polymerization technology, the output of crude C9 petroleum resin has increased significantly, and at the same time, it has brought about high impurity content, high sulfur and nitrogen content in petroleum resin, especially the increase of insoluble sol content, The disadvantage of the above patents is that due to the high impurity content of the raw materials, the amount of hydrogenated resin is largely limited by the throughput of the material and the life of the catalyst. The degradation of the resin occurs during the hydrogenation process, and the color of the product needs to be further improved. Improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The resin hydrogenation catalyst used in the examples was prepared as follows:

[0041] The hydrogenation catalyst is prepared by the coating method. The weight of the catalyst carrier alumina is 85 parts, of which Al 2 O 3 The content is 99.4% by weight, based on 100 parts of the carrier weight, taking 0.6 parts of palladium, 0.4 parts of platinum, and 2 parts of transition metal nickel. Firstly, prepare the alumina carrier whose particle size is Φ2~3mm spherical; then immerse 15 parts of the remaining alumina powder in the aqueous solution of palladium chloride, chloroplatinic acid and nickel nitrate, and spray it on the alumina as a thick slurry The hydrogenation catalyst of the present invention is obtained by drying at 120°C and calcining at 550°C on the spherical support, which is numbered H-1.

[0042] The weight of the catalyst carrier alumina is 85 parts, of which Al 2 O 3 The content is 99.4% by weight, based on 100 parts of the carrier weight, taking 0.4 parts of...

Embodiment 2

[0044] The carbon nine fraction (sulfur content 65.6μg / g, nitrogen content 58.1μg / g, bromine value 84gBr 2 / 100g oil) as the raw material, after selective hydrogenation treatment, the selective hydrogenation catalyst is a non-noble metal cobalt and molybdenum hydrogenation catalyst; the reaction temperature is 270℃, the pressure is 3.5MPa, the liquid volumetric space velocity is 3h -1 After selective hydrogenation, the sulfur content in the product is reduced to 5.2μg / g, the nitrogen content is reduced to 1.1μg / g, and the bromine value is 77gBr 2 / 100g oil. Carry out thermal polymerization in an autoclave, and then carry out rectification to remove unpolymerized C9 fractions to obtain crude C9 petroleum resin with a softening point of 110°C and Gardner hue of No. 12, and then use mineral oil The refined is dissolved in a ratio of 1:1.5 (resin: mineral spirit). The sulfur content in the dissolved resin solution is 2.4μg / g and the nitrogen content is 0.5μg / g. The crude carbon nine ...

Embodiment 3

[0050] The carbon nine fraction (sulfur content 67.1μg / g, nitrogen content 55.2μg / g, bromine value 108gBr 2 / 100g oil) as raw material, after selective hydrogenation treatment, the selective hydrogenation catalyst is a non-precious metal cobalt and molybdenum hydrogenation catalyst; the reaction temperature is 260℃, the pressure is 3.0MPa, and the liquid volumetric space velocity is 2.5h -1 After the selective hydrogenation, the sulfur content in the product is reduced to 6.2μg / g, the nitrogen content is reduced to 1.8μg / g, and the bromine value is 95gBr 2 / 100g oil. Carry out thermal polymerization reaction in an autoclave, and then carry out rectification to remove unpolymerized C9 fractions to obtain crude C9 petroleum resin with a softening point of 112℃ and Gardner hue of No. 13, and then reforming The raffinate is dissolved in a ratio of 1:2 (resin: reformed raffinate). The sulfur content in the dissolved resin solution is 3.5 μg / g and the nitrogen content is 0.8 μg / g. The ...

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Abstract

The invention relates to a preparation method of hydrogenated C9 petroleum resin, which is characterized by comprising the following steps of: (1) preparation of supported noble metal hydrogenated catalyst: preparing by using a coating method, selecting noble metal palladium and platinum and transition metal cobalt or nickel as metal active components, preparing a spherical alumina supporter, then coating the active components of palladium and platinum and transition metal on the alumina supporter, and activating to obtain a hydrogenated catalyst; (2) selective hydrogenation: desulfurizing and denitrifying; (3) high pressure hydrogenation reaction: controlling the weight ratio of resin to solvent to ensure that the concentration of resin is 20-40% by weight, taking chain-like or annular saturated hydrocarbon or aromatic hydrocarbon or hydrocarbon mixture as a solvent, and taking a supported noble metal hydrogenated catalyst as a catalyst, wherein the temperature of the high pressure hydrogenation reaction is 250-350 DEG C, the pressure is 8.0-20.0 MPa and the liquid volume space velocity is 0.5-2h<-1>. The properties of the final product hydrogenated C9 petroleum resin are as follows: Gardner is not more than 1, and the softening point is not smaller than 100 DEG C.

Description

Technical field [0001] The invention relates to the field of petrochemical technology. The invention relates to a preparation method of hydrogenated carbon nine petroleum resin, and particularly relates to a preparation method of hydrogenated carbon nine petroleum resin using cracked carbon nine fractions as a by-product of ethylene cracking. Background technique [0002] As we all know, adhesives play a very important role in human daily life. For example, they are used in packaging tapes, bandages, envelopes, note papers and many other daily-use items. The preparation of these adhesives requires the use of resin, and requires the resin to have good properties, such as light color, stability, and no peculiar smell. In industry, petroleum resin is an important source of resins for the above uses. [0003] Petroleum resin is a by-product of C5 or C9 fraction from cracking to produce ethylene. 3 Or BF 3 Complex catalytic polymerization or the product obtained after thermal polymeri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F240/00C08F8/04
Inventor 南军于海斌杨建国张景成刘新普耿姗石芳张玉婷曲晓龙
Owner CHINA NAT OFFSHORE OIL CORP
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