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Preparation of hydrogenation catalyst and use thereof

A hydrogenation catalyst and catalyst technology, applied in the direction of catalyst activation/preparation, catalyst carrier, physical/chemical process catalyst, etc., can solve problems such as catalyst poisoning, affecting performance, and excessive reduction in softening point of hydrogenated petroleum resin

Active Publication Date: 2010-05-05
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Early U.S. Patent US2824860 just carried out the report that hydrotreating petroleum resin, as US4328090, US4629766 adopts Al 2 o 3 Support presulfurized Ni, W or Ni, Mo as catalysts to produce light-colored petroleum resins. In addition, the US Patent No. 4540480 uses noble metal-supported catalysts, and the active components are mainly selected from Pd, Rh, Ru, Re, Pt, etc. These catalysts With high activity, there are also insufficient applications, as in the early literature Catalysis, Berkuan, Morrell and Egloff Reinhold, 1940P 400 It is reported in that the residual halogen in the resin will cause the deactivation of the catalyst, and even a small amount of halogen Cl in the reaction system can lead to catalyst poisoning. These factors will inevitably reduce the service life of the catalyst and also cause a decline in economic benefits.
[0007] Currently used sulfided Ni, W, Mo or noble metal supported catalysts have their own deficiencies. The industrially used presulfided Ni, W, Mo catalysts belong to hydrodesulfurization catalysts, such as used in patents CN1199742A and US6433104B1 Presulfurized Ni, W / Al 2 o 3 As a resin hydrogenation catalyst, although this catalyst has high hydrogenation catalytic activity, it can cause too much degradation reaction of petroleum resin during the reaction process, resulting in too much decrease in the softening point of hydrogenated petroleum resin, which affects the performance
For noble metal supported catalysts, active components can be selected from Pd, Pt, Ni, Ru, Rh, Re, etc., as reported in CN101157029A, CN1084521A, CN1189493C, US4952639, US4276396, the initial activity of noble metal supported catalysts in resin hydrogenation reaction High, it has an inhibitory effect on the degradation side reaction, but the residual halogen Cl in the raw resin can be adsorbed by the surface of the catalyst during the hydrogenation reaction, which will gradually increase the surface acidity of the catalyst, and eventually lead to the occurrence of hydrogenation cracking of the resin, causing the softening point of the hydrogenated resin At the same time, noble metal grains sintered during use, resulting in a reduction in hydrogenation active sites, reducing the yield of hydrogenated resin, and shortening the service life of the catalyst

Method used

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  • Preparation of hydrogenation catalyst and use thereof
  • Preparation of hydrogenation catalyst and use thereof
  • Preparation of hydrogenation catalyst and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The preparation of embodiment 1 catalyst carrier

[0048] Weigh 500g of pseudo-boehmite, 200g of aluminum hydroxide, 300g of diatomaceous earth and 100g of polyethylene glycol powder, mix well, add 276g of 6% dilute nitric acid aqueous solution for kneading, aging at room temperature for 30 minutes, and shape it on an extruder It is in the form of φ3 strips, dried at 120°C for 24 hours, and then fired at 800°C for 2 hours.

[0049] Cut the strip carrier into φ3×3 particle size and set aside.

[0050] Carriers 2, 3, 4, and 5 were prepared according to the above-mentioned preparation methods with different raw powder ratios. The composition and characterization of the carriers are shown in the following table:

[0051] Table 1 Carrier Raw Material Ratio and Carrier Characterization

[0052]

Embodiment 2

[0053] The loading of embodiment 2 active components

[0054] Weigh 100g of carriers 1 to 5 in Example 1, add 100ml (0.012g Sr / ml) of strontium nitrate aqueous solution to immerse for 24 hours, dry at 120°C for 12 hours, and then roast at 600°C for 4 hours to obtain a composite modified oxide Aluminum support, Sr content 1.2%.

[0055] Take 100g of the above-mentioned carriers 1, 2, 3, 4, and 5 respectively, put them into 120ml of a mixed aqueous solution containing palladium chloride and ruthenium chloride, wherein the palladium content is 0.00125g / ml, and the ruthenium content is 0.00083g / ml, and soak for 24 hours After drying at 120°C for 6 hours, the above operation was repeated 4 times to obtain a catalyst loaded with 0.6% Pd and 0.4% Ru. After drying, it was calcined at 400°C for 4 hours to obtain the corresponding C-1, C-2, C-3, C- 4. C-5 catalyst.

Embodiment 3

[0056] Embodiment 3 catalyst activity evaluation

[0057] Dissolve commercially available mixed C5 petroleum resin in cyclohexane solvent to form a raw material solution with a concentration of 20% (wt), wherein the chlorine content is 945ppm.

[0058] The physical properties of raw material mixed C5 petroleum resin are as follows:

[0059] Table 2 Raw material resin properties

[0060]

Color value (Gardner)

Chlorine content (ppm)

Bromine value (gBr / 100g)

Softening point (℃)

Hybrid carbon five petroleum resin

7.82

4728

70.47

106

[0061] The catalyst prepared in Example 2 was loaded into a single-tube fixed-bed reactor, and reduced at 300° C. for 4 hours in a hydrogen atmosphere under normal pressure to activate the catalyst, followed by hydrogenation reaction. The reaction conditions are as follows: temperature 270°C, pressure 8.0Mpa, liquid space velocity 4.0h -1 , hydrogen air velocity 200h -1 , the reaction mix...

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Abstract

The invention provides a preparation method of a hydrogenation catalyst suitable for the hydrogenation reaction of C5 petroleum resin. The method comprises the steps of: taking aluminium hydroxide, kieselguhr, pore-expanding agent and rare earth element-modified aluminium oxide as a carrier; loading bi-component noble metal on the carrier; and adjusting the catalytic activity with the rare earth element to obtain the hydrogenation catalyst with high activity and long service life. The catalyst is particularly suitable for the hydrogenation of the perchloride-containing C5 petroleum resin, thereby being capable of preparing hydrogenated petroleum resin with light hue and high softening point.

Description

technical field [0001] The present invention belongs to the preparation method and use of petroleum resin hydrogenation catalyst, and particularly relates to the preparation and application of a hydrogenation catalyst for C5 petroleum resin. The raw material C5 petroleum resin is the cracking by-product C5 Fractions include piperylene, isoprene, pentene, and a small amount of cyclopentadiene and dicyclopentadiene. The mixed carbon five fractions are catalyzed and polymerized to obtain mixed carbon five petroleum resins. The catalyst prepared in the invention is especially suitable for the hydrogenation process of the mixed C5 petroleum resin with high halogen content. The catalyst has high activity and long-term resistance to halogen stability, and can be used to produce high-quality hydrogenated C5 petroleum resin. Background technique [0002] In the industrial production process of ethylene, a large number of cracked C5 fractions will be produced. Usually, the C5 fraction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63B01J23/58B01J32/00B01J35/10B01J37/00C08F240/00C08F8/04
Inventor 王开林司晓郡齐彦伟张磊
Owner CHINA PETROLEUM & CHEM CORP
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