# US 2014/0155673 A1 · Process and device for simulated-countercurrent chromatographic separation for the production of metaxylene with high yield

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- Number: US 2014/0155673 A1
- Document ID: US20140155673A1
- Status: Published application
- Kind: A1
- Application number: 14/095,404
- Filed: 2013-12-03
- Published: 2014-06-05
- Earliest claimed: 2012-12-03
- Assignees: Ifp Energies Nouvelles
- Applicants: IFP Energies nouvelles
- Inventors: Pascal ETIENNE; Philibert LEFLAIVE; Damien LEINEKUGEL LE COCQ; Catherine LAROCHE
- Web page: https://patentgrep.com/patent/US20140155673A1

## CPC

- C07C 7/13: by molecular-sieve technique
- B01D 15/1828: {characterised by process features}
- B01D 15/1842: {characterised by apparatus features}
- B01J 20/186: {Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity}
- B01J 20/28011: {Other properties, e.g. density, crush strength}
- B01J 20/2803: {Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products}
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

This invention describes a process for separation of xylenes for the purpose of the production of high-purity metaxylene, a simulated countercurrent process using at least one adsorber with a limited cumulative total level (Hcu) of adsorbent at a surface velocity (Vsl) that is less than 2 cm/s.

## Claims

### Claim 1

Process for separation of metaxylene by simulated countercurrent chromatography (CCS) starting from a feedstock F that essentially comprises metaxylene and its C8 aromatic isomers, using a zeolitic adsorbent solid based on Y zeolite crystals and a non-zeolitic phase, in which the Y zeolite crystals have a mean diameter of a number that is less than or equal to 1.7 μm, preferably less than or equal to 1.5 μm, and preferably also less than or equal to 1.2 μm, a process that uses at least one adsorber that is divided into 4 chromatographic zones that are defined in the following manner:
Zone 1: Zone for desorption of metaxylene, encompassed between the injection of the desorbent D and the sampling of the extract E,
Zone 2: Zone for desorption of isomers of metaxylene, encompassed between the sampling of the extract E and the injection of the feedstock that is to be fractionated F,
Zone 3: Zone for adsorption of metaxylene, encompassed between the injection of the feedstock and the draw-off of the raffinate R,
Zone 4: Zone located between the draw-off of raffinate R and the injection of the desorbent D,
with the number of beds of each adsorber being between 6 and 18 beds, and preferably between 8 and 15 beds, with the beds all being identical, and the height of each bed being between 0.7 m and 1.40 m, said process being characterized in that it has a cumulative level (Hcu) of adsorbent solid on the different adsorber(s) of between 6 m and 21 m, and in that the mean surface velocity over each adsorber (Vsl) is between 0.9 cm/s and 1.8 cm/s, with said surface velocity being defined as the volumetric flow rate of mean recycling at the temperature of the process that is divided by the area of the cross-section of the adsorber and the cumulative height (Hcu) of adsorbent solid being distributed in the following manner:
The cumulative level of adsorbent solid in zone 1, on average over a cycle, is 17%±5% of (Hcu),
The cumulative level of adsorbent solid in zone 2, on average over a cycle, is 41.5%±5% of (Hcu),
The cumulative level of adsorbent solid in zone 3, on average over a cycle, is 25%±5% of (Hcu),
The cumulative level of adsorbent solid in zone 4, on average over a cycle, is 16.5%±5% of (Hcu).

### Claim 2 (depends on 1)

Process for separation of xylenes according to claim 1, wherein the Si/Al atomic ratio of the adsorbent is preferably such that 2.0<Si/Al<3.0, and preferably such that 2.5≦Si/Al<2.85.

### Claim 3 (depends on 1)

Process for separation of xylenes according to claim 1, wherein the adsorbent solid that is used is a zeolitic adsorbent based on NaY or NaLiY crystals with crystals whose mean diameter in numbers is between 0.1 and 1.0 micron, and preferably between 0.1 and 0.8 micron.

### Claim 4 (depends on 1)

Process for separation of xylenes according to claim 1, wherein the inside diameter of each adsorber is between 4 m and 10 m.

### Claim 5 (depends on 1)

Process for separation of xylenes according to claim 1, wherein the adsorber number that is used is 1.

### Claim 6 (depends on 1)

Process for separation of xylenes according to claim 1, wherein the operating conditions of the adsorption stage are as follows:
Temperature 100° C. to 250° C., preferably 120° C. to 180° C.,
Pressure between the bubble pressure of the xylenes at the temperature of the process and 30×105 Pa,
Ratio of the flow rate of desorbent to the flow rate of feedstock of between 0.7 and 6.5,
Recycling rate of 3.5 to 14, preferably 4.5 to 12 (with the recycling rate being defined as the ratio between the mean flow rate flowing into the different beds of an adsorber to the feedstock injection flow rate in this adsorber),
Water content in the liquid phase of between 0 and 140 ppm (by weight) and in a preferred manner between 5 and 120 ppm (by weight).

### Claim 7 (depends on 1)

Process according to claim 1, wherein the fire loss of the adsorbent solid that is measured at 900° C. is between 0% and 4.0% by weight, and preferably between 0% and 3.0% by weight.
