# US 2014/0155672 A1 · Process and apparatus for simulated counter-current chromatographic separation for high-productivity production of paraxylene

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- Number: US 2014/0155672 A1
- Document ID: US20140155672A1
- Status: Published application
- Kind: A1
- Application number: 14/093,599
- Filed: 2013-12-02
- 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/US20140155672A1

## CPC

- 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 7/13: by molecular-sieve technique
- 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
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS

## Abstract

The present invention describes a process for the separation of xylenes in simulated counter-current utilising at least one adsorber with a limited cumulated total height (Hcu) of adsorbent and a superficial velocity (Vsl) of less than 2 cm/s.

## Claims

### Claim 1

A process for separation of paraxylene by simulated counter-current (SCC) chromatography from a charge F essentially comprising paraxylene and its aromatic C8 isomers, utilising a zeolitic adsorbent solid based on zeolite crystals X and a non-zeolitic phase, in which the zeolite crystals X have an average diameter by number of between 0.1 and 1.5 microns and preferably between 0.1 and 1.2 microns, said process using at least one adsorber divided into 4 chromatographic zones defined in the following fashion:
Zone 1: zone for desorption of the paraxylene, between injection of the desorbent D and withdrawal of the extract E.
Zone 2: zone for desorption of the isomers of the paraxylene, between the withdrawal of the extract E and injection of the charge F to be fractionated.
Zone 3: zone for adsorption of the paraxylene, between injection of the charge and withdrawal of the raffinate R.
Zone 4: zone between withdrawal of the raffinate R and injection of the desorbent D,
the number of adsorption beds being between 6 and 18 and preferably between 8 and 15 beds, the beds all being identical, and the height of each bed being between 0.7 m and 1.4 m, said process being characterised in that it has a cumulated height of adsorbent solid in relation to the different adsorber or adsorbers (Hcu) of between 6 m and 21 m and that the mean superficial velocity over each adsorber (Vsl) is between 1 cm/s and 2 cm/s, said superficial velocity being defined as the mean recycling flow rate by volume at the temperature of the process divided by the area of the section of the adsorber, and the cumulated height (Hcu) of adsorbent solid being distributed in the following fashion:
the cumulated height of adsorbent solid in zone 1 on average over a cycle is 21%±5% of (Hcu),
the cumulated height of adsorbent solid in zone 2 on average over a cycle is 37.5%±5% of (Hcu),
the cumulated height of adsorbent solid in zone 3 on average over a cycle is 29%±5% of (Hcu),
the cumulated height of adsorbent solid in zone 4 on average over a cycle is 12.5%±5% of (Hcu).

### Claim 2 (depends on 1)

A process for the separation of xylenes according to claim 1 wherein the atomic ratio Si/Al of the adsorbent is such that 1.05<Si/Al<1.55, preferably such that 1.10≦Si/Al<1.55 and still more preferably such that 1.10≦Si/Al<1.30.

### Claim 3 (depends on 1)

A process for the separation of xylenes according to claim 1 wherein the adsorbent solid comprises zeolite X having a content of barium oxide BaO ranging from 33% to 42% and advantageously from 35% to 38% by weight with respect to the total weight of the adsorbent.

### Claim 4 (depends on 1)

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

### Claim 5 (depends on 1)

A process for the separation of xylenes according to claim 1 wherein the number of adsorber used is 1.

### Claim 6 (depends on 1)

A process for the separation of xylenes according to claim 1 wherein the operating conditions of the adsorption step 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 in relation to the flow rate of charge of between 0.7 and 2.5,
recycling rate of 2.0 to 12, preferably 2.5 to 6 (the recycling rate being defined as the ratio between the mean flow rate flowing in the different beds of an adsorber in relation to the flow rate of injection of the charge into that adsorber), and
water content in liquid phase of between 70 and 140 ppm (by weight) and preferably between 80 and 120 ppm (by weight).

### Claim 7 (depends on 1)

A process for the separation of xylenes according to claim 1 wherein the adsorbent solid has a small proportion of amorphous phase, that is to say less than 5% by weight.

### Claim 8 (depends on 1)

A process according to claim 1 wherein the ignition loss of the adsorbent solid measured at 900° C. is between 4.0% and 7.7% by weight and preferably between 4.7% and 6.7% by weight.
