Alkyne-rich C4 fraction selective hydrogenation method

A technology for selective hydrogenation of alkyne-rich carbon four fractions, which is applied in the fields of hydrocarbons, chemical instruments and methods, hydrogenation to hydrocarbons, etc., and can solve the problems of catalyst activity decline, cost increase, selectivity decline, etc.

Pending Publication Date: 2022-04-12
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reduction temperature of Ni often reaches about 500 ° C. At this temperature, the reduced Pd atoms are easy to aggregate, which greatly reduces the activity of the catalyst. It is necessary to increase the content of active components to compensate for the loss of activity, but it will also increase the cost. selectivity decline

Method used

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  • Alkyne-rich C4 fraction selective hydrogenation method
  • Alkyne-rich C4 fraction selective hydrogenation method
  • Alkyne-rich C4 fraction selective hydrogenation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Catalyst carrier prepared: 3 mm of commercially available bispacles, 3 mm diameter, after 1,100 ° C for 4 h, is 20 ~ 45 nm and 90 ~ 400 nm, respectively, the specific surface area is 43m 2 / g, weigh 100g of the carrier.

[0038] Catalyst preparation:

[0039] (1) Palladium chloride is formed into an active component impregnation liquid, and the pH is 1.7, and then the carrier is added to the salt solution of the PD, and after impregnation adsorption 2 h, 100 ° C drying for 4 h, 550 ° C, calcination 2h, and produce semi-finished catalyst C1-a.

[0040] (2) Nitrate is completely dissolved into a dipping liquid, an equal volume impregnation, and the semi-finished catalyst C1-a is immersed in the prepared solution, uniform shaking, 0.5 h, drying at 100 ° C for 2 h, 400 ° C for 6 h, Semi-finished catalyst C1-B.

[0041] (3) Nickel nickel nitrate, copper nitrate is dissolved in 70 g of water, and 35 g of n-hexane, 17 g of polyethylene glycol octylphenyl ether (Tritonx-100), 17 g...

Embodiment 2

[0055] Catalyst carrier prepared: 3 mm of commercially available bispy pores, a diameter of 3 mm, after 1050 ° C for 4 h, is 14 to 45 nm and 85 to 350 nm, respectively, the specific surface area is 60m 2 / g, weigh 100g of the carrier.

[0056] Catalyst preparation:

[0057] (1) Nickel nickel nitrate, copper nitrate is dissolved in 80 g of water, add 40 g of n-pentane, 20 g of hexadalkyltrimethyla bromide, 20 g n-pentanol thorns to form a microemulsion, and add the carrier to the prepserned microemulsion After 0.5 h in 0.5 h, the residue was filtered, washed with deionized water to neutral. It was dried at 60 ° C for 6 h, baked at 590 ° C for 2 h, and semi-finished catalyst C2-a was obtained.

[0058] (2) Palladium chloride is dissolved in 80 g of water, 40 g n-pentane, 20 g of hexadalkyltrimethylammonium bromide, 20 g n-pentanol thoroughly stirring to form a microemulsion. The semi-finished C2-A prepared by step (1) was immersed in the prepared microemulsion to be immersed in 0.5...

Embodiment 3

[0073] Catalyst carrier prepared: 3 to 4 mm in a commercially available bifurcous hole, a diameter of 3 to 4 mm, after 10 ° C for 4 h, is 30 ~ 45 nm and 100 ~ 500 nm, respectively, the specific surface area is 25m 2 / g, weigh 100g of the carrier.

[0074] Catalyst preparation:

[0075] (1) Nickel nickel nitrate, copper nitrate is dissolved in 75 g of water, add 34 g of n-heptane, 17 g of sorbitol monohydrate polyoxyethylene ether (Tween 80), 16 g n-pentanol thorns to form a microemulsion, add the carrier to After impregnation with a microemulsion for 2 h, the residue was filtered, washed with deionized water to neutral. It was dried at 80 ° C for 3 h at 500 ° C to prepare the semi-finished catalyst C3-a.

[0076] (2) Palladium chloride is prepared into an active component impregnation liquid, and the pH is 2.5, and the semi-finished catalyst C3-a prepared by step (1) is added to the salt solution of the PD, and the adsorption of the adsorption 2 h then dried at 110 ° C for 3 h, 4...

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Abstract

The invention relates to an alkyne-rich C4 fraction selective hydrogenation method, which comprises the following steps: by taking alkyne-rich C4 fraction after butadiene extraction as a raw material, under the action of a catalyst, carrying out selective hydrogenation on alkyne and alkadiene to obtain butene by adopting an adiabatic fixed bed reactor, and under the adopted process operation conditions, the molar ratio of hydrogen at the inlet of the reactor to the sum of the content of total alkyne and alkadiene is 1.5-2.5; the reaction inlet temperature is 30-80 DEG C, the reaction pressure is 1.0-3.0 MPa, and the liquid volume space velocity is 10-25 h <-1 >. The catalyst at least contains four components of Pd, Bi, Ni and Cu, and Ni, Cu and a small amount of Pd are loaded by adopting a microemulsion method and are distributed in macropores of the carrier. Bi and most Pd are loaded by adopting a traditional solution impregnation method and are distributed in small holes of the carrier. By adopting the method disclosed by the invention, the C4 fraction rich in alkyne after butadiene extraction can be effectively utilized, the resource waste is reduced, and meanwhile, the hydrogenation method disclosed by the invention has the characteristics of high anti-coking performance and good operation stability.

Description

Technical field [0001] The present invention relates to a method of selecting hydrogenated hydrogenated hydrogenated butene after elongation of butadiene extracted after extension of the deproduction cycle. Background technique [0002] 1,3-butadiene is an important monomer of synthetic rubber. Industrial mainly based on hydrocarbon cleavage ethylene, the cleavage carbon 4 is used as a raw material, and the method of solvent extraction is carried out. In addition to 40 to 60% by weight of 1,3-butadiene, lysis carbon 4, typically contains 1 to 2% by weight of alkyne (mainly vinylcerase), in order to obtain polymerization grade 1,3-butadiene ( The purity of butadiene is ≥99.5%, the alkyne content is <100 ppm, which is usually extracted with two-stage normal distillation in the second stage of ordinary distillation. As the impurities, the carbon tetralene hydrocarbon is discharged mainly in the second extraction rectification tower, with a set of 800,000 tons / year of the ethyle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C5/09C07C11/167B01J23/89C07C7/167
Inventor 谢元常晓昕展学成胡晓丽马好文王斌孙利民吕龙刚谢培思柏介军杨卓陈智
Owner PETROCHINA CO LTD
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