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Preparation method for Carbon 5/Carbon 9 hydrogenated petroleum resin

A technology of hydrogenated petroleum resin and C9 petroleum resin, which is applied in the field of preparation of C5/C9 hydrogenated petroleum resin, can solve the problems of difficult hydrogenation, harsh operating conditions, insufficient hydrogenation degree, etc., so as to improve the effective Catalytic area, reduce equipment investment cost, reduce the effect of fluid pressure drop

Inactive Publication Date: 2011-08-03
杭州腾王网络科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. patents US3442877, 3484421 and 3701760 have announced petroleum resin hydrogenation technology, which adopts a continuous fixed bed hydrogenation process. Because the hydrogenation of petroleum resin is quite difficult, the operating pressure of the two-stage method is high, and the second stage generally reaches 20- 35Mpa, great potential safety hazard, very high requirements for equipment, one-stage method due to insufficient hydrogenation degree, the quality cannot reach high quality, so the operating conditions of foreign petroleum resin hydrogenation process design are relatively harsh, the process type depends on the production scale and the target Product requirements vary
[0004] CN101628956A discloses the preparation technology of slurry-state still-type petroleum resin hydrogenation. Due to the characteristics of high temperature and high pressure, the design of special hydrogenation reaction equipment is quite difficult, so the industrialization of slurry-state still-type hydrogenation is not ideal
[0006] The catalysts currently used in commercial production are mostly nickel and platinum catalysts, and the carrier is aluminum oxide. Nickel catalysts are not ideal for hydrogenation of aromatic rings, while platinum catalysts are prone to poisoning.

Method used

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  • Preparation method for Carbon 5/Carbon 9 hydrogenated petroleum resin
  • Preparation method for Carbon 5/Carbon 9 hydrogenated petroleum resin
  • Preparation method for Carbon 5/Carbon 9 hydrogenated petroleum resin

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Preparation of Catalyst NiW / SiO 2 : The weight ratio of the catalyst components: the carrier silica is 79%, nickel 6%, tungsten trioxide 15%, and NiW / SiO is prepared by pore saturation co-impregnation method to load active metal components 2 , the specific surface area of ​​the carrier is measured by mercury porosimetry as 14m 2 / g, pore diameter 550nm, pore volume are 1.5cc / g; above-mentioned catalyzer is vulcanized 3-5 hour at 650-750K in hydrogen (90%) and hydrogen sulfide (10%) mixed gas, is cooled to room temperature after vulcanization, and uses Nitrogen was purged for 0.5 hours, and stored in a sealed bottle filled with argon for later use.

[0020] Preparation of Catalyst Ru / SiO 2 : silicon dioxide (mass ratio 99%) is impregnated in the solution that dissolves ruthenium trichloride (ruthenium mass ratio 1%), evaporate to dryness at 100 DEG C then, 200 DEG C dry 3h, hydrogen reduction 2h at 400 DEG C at last, Catalyst Ru / SiO 2 , the carrier and the first-stag...

Embodiment 2

[0025] Preparation of Catalyst NiW / SiO 2 : The weight ratio of the catalyst components: the carrier silica is 70%, nickel 10%, tungsten trioxide 20%, and NiW / SiO is prepared by pore saturation co-impregnation method to load active metal components 2 , the specific surface area of ​​the carrier is measured by mercury porosimetry as 13m 2 / g, average pore diameter 720nm, pore volume is 1.6cc / g; above-mentioned catalyst is vulcanized at 650-750K in the mixed gas of hydrogen (90%) and hydrogen sulfide (10%) for 3-5 hours, cool to room temperature after vulcanization, And purged with nitrogen for 0.5 hours, and stored in a sealed bottle filled with argon for later use.

[0026] Preparation of Catalyst Ru / SiO 2 : silicon dioxide (mass ratio 99%) is impregnated in the solution that dissolves ruthenium trichloride (ruthenium mass ratio 1%), evaporate to dryness at 100 DEG C then, 200 DEG C dry 3h, hydrogen reduction 2h at 400 DEG C at last, Catalyst Ru / SiO 2 , the specific surface...

Embodiment 3

[0032] Preparation of Catalyst NiW / SiO 2 : The weight ratio of the catalyst components: the carrier silica is 75%, nickel 8%, tungsten trioxide 15%, and the NiW / SiO is prepared by the pore saturation co-impregnation method to load the active metal component 2 , the specific surface area of ​​the carrier was measured by mercury intrusion porosimetry to an area of ​​9m 2 / g, average pore diameter 1200nm, pore volume is 1.8cc / g; above-mentioned catalyst is vulcanized at 650-750K for 3-5 hours in the mixed gas of hydrogen (90%) and hydrogen sulfide (10%), cool to room temperature after vulcanization, And purged with nitrogen for 0.5 hours, and stored in a sealed bottle filled with argon for later use.

[0033] Preparation of Catalyst Ru / SiO 2 : silicon dioxide (mass ratio 99%) is impregnated in the solution that dissolves ruthenium trichloride (ruthenium mass ratio 1%), evaporate to dryness at 100 DEG C then, 200 DEG C dry 3h, hydrogen reduction 2h at 400 DEG C at last, Catalys...

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Abstract

The invention discloses a preparation method for Carbon 5 / Carbon 9 hydrogenated petroleum resin. In the existing preparation methods, certain methods have extremely high requirements on devices and high cost, and catalysts used by certain methods are not ideal for aromatic ring hydrogenation effect or easily cause intoxication. The preparation method comprises the following steps: firstly dissolving Carbon 5 / Carbon 9 petroleum resin by a dissolvent, then carrying out centrifugal sedimentation on the carbon 5 / Carbon 9 petroleum resin so as to remove most insoluble gel and asphaltenes, filtering the carbon 5 / Carbon 9 petroleum resin in an absorption tower filled with fillers so as to remove remained insoluble gel, asphaltenes and heavy metals; carrying out medium pressure hydrogenation reaction on liquid obtained through filtration in a static bed filled with secondary hydrogenation catalyst; and finally, carrying out flash evaporation and steam stripping so as to remove solvent in the product. The preparation method adopts a macroporous catalyst carrier; fluids are not easily blocked in holes, thereby greatly reducing fluid pressure drop and increasing effective catalytic area; and secondary hydrogenation can be completed in medium pressure, thereby greatly reducing requirements on devices and investment cost of the devices and obtaining hydrogenated petroleum resin with high quality.

Description

technical field [0001] The invention relates to the processing field of petroleum resins, in particular to a preparation method of C5 / C9 hydrogenated petroleum resins. Background technique [0002] The 20~260℃ pyrolysis distillate produced in petroleum cracking, after thermal polymerization or in BF 3 or AlCl 3 Petroleum resins with different properties obtained by polymerization under the action of catalysts. Petroleum resins are widely used in the fields of coatings, inks, adhesives and rubbers. Polymer materials are blended to improve the performance of related products. However, petroleum resin has a deep color and the main reason for the color is that the polymer chain contains unsaturated double bonds, which has poor thermal and chemical stability, especially unstable to heat and oxygen, and will produce an unpleasant smell when heated. Long-term Disadvantages such as darkening the color under light seriously limit the scope of application. The fundamental method t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F240/00C08F8/04
Inventor 俞陆军严俊胡仙超刘秋平崔秀芳
Owner 杭州腾王网络科技有限公司
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