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Hydrogenation catalyst based on dicyclopentadiene (DCPD) resin undergoing heat polymerization by dicyclopentadiene in ethylene pyrolysis C9 and preparation method thereof and application

A technology for dicyclopentadiene and hydrogenation catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the cumbersome activation process, serious resin degradation, inability to To meet the needs of hydrogenation and other issues, to achieve the effect of simple activation process and improved sulfur resistance performance

Active Publication Date: 2017-01-04
CHINA PETROLEUM & CHEM CORP
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AI Technical Summary

Problems solved by technology

Supported sulfided nickel-tungsten or nickel-molybdenum sulfide resin hydrogenation catalysts have high activity, but they need to be activated by sulfidation before use. The activation process is cumbersome, the resin degradation is serious, and the product yield is only about 80%. Softening point dropped from 120°C to 9O°C
[0012] CN1237117A discloses a method for hydrogenation of unsaturated hydrocarbons, catalytic hydrogenation of hydrocarbon molecules with a number average molecular weight greater than 180, the active components are 7 (wt)% NiO and 15-25.0 (wt)% WO 3 , and adding 0.25 to 10 (wt)% of the alkali metal accelerator to improve halogen resistance, alkali metals include 1-3 groups, and lanthanides, actinides metals, typically lanthanum, potassium, magnesium, rubidium, cesium, Rubidium, zinc and calcium, but the resin degradation is serious when the nickel-based catalyst hydrogenates the resin, and the softening point decreases more
For C-based 9 The dicyclopentadiene thermally polymerized DCPD resin obtained by distillate separation has a sulfur content as high as 400-500 μg / g, so the above-mentioned Pd-based noble metal catalyst cannot meet its hydrogenation requirements

Method used

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  • Hydrogenation catalyst based on dicyclopentadiene (DCPD) resin undergoing heat polymerization by dicyclopentadiene in ethylene pyrolysis C9 and preparation method thereof and application
  • Hydrogenation catalyst based on dicyclopentadiene (DCPD) resin undergoing heat polymerization by dicyclopentadiene in ethylene pyrolysis C9 and preparation method thereof and application
  • Hydrogenation catalyst based on dicyclopentadiene (DCPD) resin undergoing heat polymerization by dicyclopentadiene in ethylene pyrolysis C9 and preparation method thereof and application

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0035] The preparation of catalyst: the preparation and evaluation data of table 3 catalyst:

[0036] Weigh a certain amount of formed γ-alumina carrier, use soluble salts of molybdenum and manganese to make a loading solution equal to the volume of the carrier, soak the carrier in the loading solution for a certain period of time at room temperature, and pour out the remaining The soaking solution is dried, roasted and cooled, then soaked in an equal volume of palladium soluble salt solution for a certain period of time, and then dried and roasted to obtain the required catalyst.

[0037] The catalyst is reduced in a hydrogen atmosphere, first raised to 120°C at 3-5°C / min, and kept at a constant temperature for 2h to 3h, then raised to 300°C at a rate of 3-5°C / min, kept at a constant temperature for 4h to 6h, and then put the bed in a hydrogen atmosphere. The temperature of the layer was lowered to 260°C for the hydrogenation reaction.

[0038] Catalyst hydrogenation reactio...

Embodiment 1-8

[0046] Examples 1-8 are catalyst preparation and evaluation experiments.

[0047] Weigh 30 g of strip-shaped γ-alumina carrier after molding, and carry the required Mo content on the catalyst according to Table 3. 2 o 3 , MnO weight percent content Weigh required ammonium molybdate tetrahydrate and 50% manganese nitrate to prepare 45ml solution. Soak the carrier in the solution for 12 hours at room temperature, and pour off the remaining soaking solution. After drying at 118-120°C, calcining at 500-600°C for 6 hours, loaded with high content of molybdenum and manganese, the catalyst has the performance of anti-sulfur poisoning and hydrogenation performance of sulfide. The gamma-alumina carrier after loading molybdenum and manganese is soaked with an equal volume of palladium chloride solution for 12 hours (weighing the amount converted into palladium chloride according to the palladium content required for loading), and then dried, The catalyst is prepared by roasting, and ...

Embodiment 9-20

[0053] Embodiment 9-20 is based on ethylene cracking C 9 The reaction condition experiment of the DCPD petroleum resin of medium dicyclopentadiene thermopolymerization, catalyzer is the catalyzer among the embodiment 5.

[0054] Catalyst evaluation was carried out in a 10 ml fixed bed reactor.

[0055] The prepared catalyst is reduced in a hydrogen atmosphere in a 10ml fixed-bed reactor, first raised to 120°C at 3-5°C / min, and kept at a constant temperature for 2h-3h, then raised to 300°C at a rate of 3-5°C / min, and kept at a constant temperature for 4h- 6h, and then lower the bed temperature to 260°C in a hydrogen atmosphere for hydrogenation reaction.

[0056]The experimental process of catalyst hydrogenation reaction conditions is as follows: use one of n-heptane, methylcyclohexane or n-octane to make DCPD resin into a solution with a concentration of 10-20%, preheat to 250-260°C and enter the fixed bed Reactor, control the reactor temperature at 260-280°C, the reaction p...

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Abstract

The invention relates to a hydrogenation catalyst based on dicyclopentadiene (DCPD) resin undergoing heat polymerization by dicyclopentadiene in ethylene pyrolysis C9 and a preparation method thereof and application. The catalyst takes gamma-aluminium oxide as a carrier, and catalyst active ingredients are palladium, molybdenum and manganese; based on 100% of the total weight of the catalyst, the catalyst comprises 0.5-1.2% of Pd, 10.0-15.0% of Mo2O3, 5.0-10.0% of Mn, and the balance gamma-aluminium oxide. The catalyst is in a strip shape, a clover shape or a sphere shape with a size of phi 3*3-5 mm, and the specific surface area is 100-150 m2 / g. The ingredients are loaded on the carrier in a substep mode and are reduced in hydrogen atmosphere, and the activation process is simple and convenient; a fixed bed hydrogenation process is adopted, the resin does not undergo desulfuration pretreatment, and desulfuration and saturation are performed in one step. Hydrogenation reaction is performed in a heat insulation or row tube fixed bed reactor, and DCPD resin solution concentration, feeding temperature, reaction temperature, pressure, volume liquid hourly space velocity and hydrogen / oil ratio conditions are optimized.

Description

technical field [0001] The present invention relates to a kind of based on ethylene cracking C 9 A hydrogenation catalyst for DCPD (dicyclopentadiene) resin thermally polymerized in medium dicyclopentadiene, especially a hydrogenation catalyst for DCPD resin with high sulfur content, and a preparation and application method. Background technique [0002] When the ethylene unit uses raw materials such as light hydrocarbons, naphtha, diesel oil, and hydrogenated tail oil to crack to produce ethylene and propylene, the by-product cracking C 9 , accounting for about 10-20% of ethylene production, cracking C 9 The composition of C varies with the cracking raw material, cracking process, and cracking depth, and the cracking C of different manufacturers 9 There are also significant differences in composition. However, from the perspective of synthesis, it can be divided into two categories: one is active components, such as styrene and its derivatives, indene and its derivatives...

Claims

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Application Information

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IPC IPC(8): B01J21/04B01J23/656C08F240/00C08F8/04
Inventor 李明玉司晓郡吴俊华马颖涛宁小娟赵耀
Owner CHINA PETROLEUM & CHEM CORP
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