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Catalyst for selective hydrogenation reaction of phthalate and preparation method of catalyst

A phthalate ester and hydrogenation reaction technology, applied in the field of catalysis, can solve the problems of high loss rate and poor stability of precious metals in the catalyst, and achieve the effects of excellent stability, good activity and low loss rate

Active Publication Date: 2018-08-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Purpose of the invention: Aiming at the problems of poor stability of the existing phthalate hydrogenation reaction catalysts and high loss rate of precious metals in the catalyst, the present invention provides a method for the selective hydrogenation reaction of phthalates to produce rings. Catalyst for hexane 1,2-dicarboxylate, and a preparation method of the catalyst is provided

Method used

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  • Catalyst for selective hydrogenation reaction of phthalate and preparation method of catalyst

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Effect test

Embodiment 1

[0027] 1) Take 2g HY molecular sieve and 2g silicalite-1 molecular sieve, heat treatment at 120℃ for 1h; 2) Add 2g γ-alumina, 1g triethylhexyl phosphoric acid and 4g deionized water to the mixed molecular sieve after heat treatment , kneaded evenly; 3) Granulate the kneaded material into particles with a particle size of about 1.2 mm, and dry at 120 ° C for 3 hours; 4) Add 12 g of graphite to the dried particles and mix them evenly, and press them into Ф5× 5mm cylindrical particles; 5) The tablet is roasted at 700°C to obtain the carrier required for the preparation of the catalyst; 6) The carrier is immersed in a mixed solution containing ruthenium chloride, rubidium chloride, phosphoric acid, sodium chloride, and lanthanum nitrate for 0.5h , taken out and dried at 120°C, and then roasted at 200°C for 2h; the mass content of ruthenium element is 0.1%, the mass content of rubidium element is 0.1%, the mass content of phosphorus element is 0.1%, and the mass content of sodium el...

Embodiment 2

[0029] 1) Take 10g HY molecular sieve and 10g silicalite-1 molecular sieve, heat treatment at 700°C for 3h; 2) Add 10g aluminum stearate, 2g sodium lauryl sulfate and 30g sodium lauryl sulfate to the mixed molecular sieve after heat treatment Ionized water, kneaded evenly; 3) Granulate the uniformly kneaded material into particles with a particle diameter of about 1.2 mm, and dry at 120 ° C for 5 hours; 4) Add 12 g of graphite to the dried particles and mix them evenly, and press them into tablets by a tablet machine. Ф5×5mm cylindrical particles; 5) The tablet is calcined at 1200°C to obtain the carrier required for the preparation of the catalyst; 6) The carrier is immersed in the mixed solution of chloroplatinic acid, strontium chloride, magnesium chloride, cerium nitrate, and boric acid for 3 hours, and taken out Dry at 120°C, and then bake at 600°C for 4 hours; the mass content of platinum element is 5%, the mass content of strontium element is 2%, the mass content of boro...

Embodiment 3

[0031]1) Take 5g HY molecular sieve and 5g silicalite-1 molecular sieve, heat treatment at 500°C for 2h; 2) add 5g aluminum nitrate, 1.5g methyl amyl alcohol and 15g deionized water to the mixed molecular sieve after heat treatment, knead 3) Granulate the uniformly kneaded material into particles with a particle size of about 1.2mm, and dry at 120°C for 4 hours; 4) Add 12g of graphite to the dried particles and mix them evenly, and press them into Ф5×5mm particles by a tablet press Cylinder granules; 5) the tablet is roasted at 1100°C to obtain the carrier required for the preparation of the catalyst; 6) the carrier is immersed in the mixed solution of palladium chloride, potassium chloride, yttrium chloride, selenium nitrate and cerium nitrate for 2 hours, and taken out drying at 120°C, and then roasting at 550°C for 3 hours; the mass content of palladium element is 2.5%, the mass content of yttrium element is 1%, the mass content of selenium element is 1%, and the mass conten...

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Abstract

The invention discloses a catalyst for selective hydrogenation reaction of phthalate and a preparation method of the catalyst. The catalyst is prepared from a carrier, an active component and an auxiliary agent, wherein the carrier is a composite molecular sieve of an HY molecular sieve and a silicalite-1 molecular sieve; the active component is selected from at least one of ruthenium, platinum and palladium; the auxiliary agent comprises four types, wherein the first type auxiliary agent is selected from one of boron, phosphorus and selenium; the second type auxiliary agent is selected from one of sodium, magnesium and potassium; the third type auxiliary agent is selected from one of rubidium, strontium and yttrium; the fourth type auxiliary agent is selected from one of lanthanum and cerium. The preparation method of the catalyst comprises the following steps: taking the HY molecular sieve and the silicalite-1 molecular sieve and carrying out heat treatment to prepare the composite molecular sieve; after granulating and drying, adding graphite and carrying out tabletting and roasting to obtain a carrier; impregnating the carrier in soluble salt containing the active component andthe auxiliary agent; then taking out the carrier, drying and roasting to obtain the catalyst. The catalyst disclosed by the invention has relatively high activity and excellent stability; after the catalyst is operated for a long period, the loss rate of noble metal is low.

Description

technical field [0001] The invention relates to a catalyst for hydrogenation reaction, in particular to a catalyst for selective hydrogenation reaction of phthalate to prepare cyclohexane 1,2-dicarboxylate, which belongs to the technical field of catalysis. Background technique [0002] Phthalate esters (PAEs) are currently the most widely used plasticizers, but PAEs can enter the human body through many ways, and the toxicity research of its benzene ring structure has attracted extensive attention of scholars. With the deepening of environmental protection, green, and non-toxic concepts, PAEs are no longer suitable for the current development requirements, and the direct hydrogenation of benzene rings on PAEs to generate cyclohexane 1,2-dicarboxylate is a current research hotspot, which is expected to be It will replace PAEs plasticizer in the future. [0003] The patent US475064 describes the use of a Rh / C catalyst with a mass fraction of 5% to catalyze the synthesis of c...

Claims

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Application Information

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IPC IPC(8): B01J29/80B01J29/035B01J29/12B01J29/08B01J37/08B01J37/02C07C67/303C07C69/75
CPCB01J29/005B01J29/035B01J29/0354B01J29/084B01J29/088B01J29/126B01J37/0201B01J37/08B01J2229/18C07C67/303C07C2601/14C07C69/75
Inventor 黄先亮徐本刚吴学其张杰吴琳朱艳芳王金利蔡进
Owner CHINA PETROLEUM & CHEM CORP
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