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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 high impurity content of petroleum resin, limitation of hydrogenated resin, etc., and achieve high softening point, low bromine index and process stability Good results

Active Publication Date: 2011-04-06
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 embodiment is prepared as follows:

[0041] The hydrogenation catalyst was prepared by coating method. Catalyst carrier alumina weight is 85 parts, wherein Al 2 o 3 The content is 99.4% by weight. Based on 100 parts by weight of the carrier, 0.6 parts of palladium, 0.4 parts of platinum and 2 parts of transition metal nickel are taken. First 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 in the form of thick slurry Dry at 120°C and activate by calcination at 550°C on a spherical carrier to obtain the hydrogenation catalyst of the present invention, coded as H-1.

[0042] Catalyst carrier alumina weight is 85 parts, wherein Al 2 o 3 The content is 99.4% by weight. Based on 100 parts by weight of the carrier, 0.4 parts of palladium, 0...

Embodiment 2

[0044] C9 fraction (sulfur content 65.6μg / g, nitrogen content 58.1μg / g, bromine value 84gBr) 2 / 100g oil) as raw material, after selective hydrogenation treatment, the selective hydrogenation catalyst is a non-precious metal cobalt-molybdenum hydrogenation catalyst; the reaction temperature is 270°C, the pressure is 3.5MPa, and the liquid volume space velocity is 3h -1 , the sulfur content in the product after selective hydrogenation 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 reaction in a high-pressure reactor, and then carry out rectification to remove unpolymerized C9 fractions to obtain crude C9 petroleum resin with a softening point of 110°C and a Gardner hue of No. 12, and then use mineral oil Essence is dissolved in the ratio of 1: 1.5 (resin: mineral spirits), sulfur content is 2.4 μ g / g, nitrogen content is 0.5 μ g / g in the resin liquid after dissolving, and crude car...

Embodiment 3

[0050] C9 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 molybdenum hydrogenation catalyst; the reaction temperature is 260 °C, the pressure is 3.0MPa, and the liquid volume space velocity is 2.5h -1 , the sulfur content in the product after selective hydrogenation 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 a high-pressure reactor, and then carry out rectification to remove unpolymerized C9 fractions to obtain crude C9 petroleum resin with a softening point of 112°C and a Gardner hue of No. 13, and then use reforming The raffinate is dissolved in a ratio of 1: 2 (resin: reforming raffinate), and the sulfur content in the dissolved resin liquid is 3.5 μg / g, and the nitrogen content is 0.8 μg / g,...

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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. It is a preparation method of hydrogenated C9 petroleum resin, in particular, it relates to a preparation method of hydrogenated C9 petroleum resin by using cracked C9 distillate as a by-product of ethylene cracking as a raw material. Background technique [0002] Adhesives are known to play a very important role in the daily life of human beings, for example they are used in packing tape, bandages, envelopes, note papers and many other items of daily use. The preparation of these adhesives requires the use of resins, and the resins are required to have good properties, such as light color, stability, and no peculiar smell. In industry, petroleum resin is an important source of resin for the above-mentioned purposes. [0003] Petroleum resin is the by-product of carbon five or carbon nine fractions produced during cracking to produce ethylene 3 or BF 3 Complex catalytic polymerization ...

Claims

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Application Information

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Patent Type & Authority Applications(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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