Uop Lcc

Alliedsignal Inc.

Other

Hermann A Zinnen

Thad S Franczyk

Anil Rajaram Oroskar

Stephen T Wilson

Stephen Frederic Yates

James A Johnson

James W Priegnitz

Chin-Hsiung Chang

James R Lansbarkis

Richard L Fergin

Steven P Johnson

Gary C Anderson

Kelly C Issa

Roberto E Prada

Methods have been found to prepare fused silica capillary gas chromatographic columns where the stationary phase is a molecular sieve affixed to the silica capillary wall without the aid of an organic binder by modifying the interior surface of the silica prior to contact with the molecular sieve. These totally inorganic columns greatly expand the application and range of gas chromatographic separations and allow the use of non-traditional carrier gases, even air, while not degrading the separation of components. The columns are films of small molecular sieve particles affixed to a silica surface modified by such treatments as hydrogen peroxide, alumina deposition, or silica deposition followed by fixation at 80.degree.-160.degree. C.

Zeolitic capillary columns for gas chromatography

A two-stage separation process for separating highly unsaturated triglycerides from an interesterification reaction product by sequential chromatographic separations wherein triglycerides are separated from saturated fatty acids in the first stage and unsaturated fatty acids are recovered in the second stage for recycle to the interesterification reaction zone. In a preferred embodiment using silica gel and silicalite in the two stages, respectively, and heptanone as desorbent in both stages, triglyceride product is removed as the first stage raffinate and the unsaturated fatty acid recycle product stream is removed as the raffinate in the second stage. In another embodiment, using silicalite adsorbent in both stages and 2-heptanone and acetone in the first and second stages, respectively, saturated fatty acids are removed as the extract in the first stage and triglycerides and unsaturated fatty acids are separated as raffinate product and extract product for recycle, respectively.

Process for separating fatty acids and triglycerides

In the process flow scheme for chromatographically separating para-xylene from C.sub.8 isomers containing substantial amounts of C.sub.9 aromatic hydrocarbon impurities with BaX or KY zeolite adsorbent and heavy desorbents, e.g., tetralin and diethyltoluene, a bottoms stream from the extract fractionation column containing desorbent is recycled to the separation unit and a sidecut stream, containing C.sub.9 aromatic hydrocarbon impurities and a minor amount of the desorbent from the raffinate stream, is directed to the raffinate fractionation column, thereby removing C.sub.9 aromatic hydrocarbons from the desorbent before recycling the desorbent to the separation unit, and preventing C.sub.9 aromatics from building up in the desorbent input. A fractionator for the extract column bottoms stream is eliminated, lowering capital costs, and energy requirements for the raffinate column are reduced.

Process for separating para-xylene from a C.sub.8 and C.sub.9 aromatic

A chromatographic process able to separate para-xylene from C.sub.8 isomers and C.sub.9 aromatics. In the process, the para-xylene-containing feed mixture is contacted with an X zeolite adsorbent having barium or barium and potassium ions, at exchangeable cationic sites. The para-xylene components are selectively adsorbed onto the adsorbent. The non-adsorbed feed is then removed from the adsorbent and the para-xylene recovered by desorption with indan or an alkyl derivative of indan. Any C.sub.9 aromatic hydrocarbons and the other xylene isomers in the raffinate can be separated from these heavy desorbents by fractionation of the raffinate and the desorbent can be recycled to the process.

Zeolitic para-xylene separation with indan and indan derivatives as

A process for the coextraction of para-cresol and meta-cresol from a feed mixture comprising p-cresol, o-cresol and m-cresol and one other alkyl phenol with an adsorbent comprising an X zeolite exchanged with barium ions or a mixture of barium and potassium ions at exchangeable sites to preferentially adsorb both para- and meta-cresol. The adsorbent must contain at least about 5 wt. % water (LOI method). The coextracted cresol isomers are thereafter removed from the adsorbent by contacting it with a desorbent material and recovering said coextracted cresols as a product stream. Para-cresol and meta-cresol can thereafter be recovered as purified individual isomers by a second state adsorptive separation using a second adsorbent selective for para-cresol, e.g., said first adsorbent dried to an LOI of less than about 4 wt. %, preferably about 2 wt. % water. In a preferred embodiment, the process uses a simulated moving-bed countercurrent flow system in both adsorption separation steps.

Separation of alkyl-substituted phenolic isomers with barium-potassium

A process for the separation of 2,4 DCP from a hydrocarbon feed mixture comprising 2,4 and 2,6 DCP which process employs an adsorbent comprising a type X or type L zeolite which has been cation exchanged at appropriate conditions with one or more cations selected from the group consisting of alkaline metals, alkaline earths and Group VIII elements of the Periodic Table. The adsorbed DCP isomer(s) thereafter is removed from the adsorbent by contacting it with a desorbent material and is recovered to an extract product stream, likewise the remainder of the feed material is recovered to a raffinate product stream. In a preferred embodiment the process uses a simulated moving-bed countercurrent flow system.

Separation of dichlorophenol isomers with zeolite adsorbents

A chromatographic process able to separate paraxylene from C.sub.8 isomers and C.sub.9 aromatics. In the process, the para-xylene-containing feed mixture is contacted with an X or Y zeolite adsorbent having Group IA or IIA cations, e.g., barium and/or potassium, at exchangeable cationic sites while maintaining the water content of the adsorbent at about 4.2-6% (LOI). The para-xylene components are selectively adsorbed onto the adsorbent. The non-adsorbed feed is then removed from the adsorbent and the para-xylene recovered by desorption with tetralin or alkyl derivatives of tetralin. The C.sub.9 's and the other xylene isomers in the raffinate, can be separated from this heavy desorbent by fractionation of the raffinate and the desorbent recycled to the process.

Zeolitic para-xylene separation with tetralin derivatives as heavy

The separation of free fatty acids from triglycerides and/or diglycerides is performed by an adsorptive chromatographic process in liquid phase with a crystalline aluminophosphate, e.g., AIPO.sub.4 -5, AIPO.sub.4 -11 or AIPO.sub.4 -54, as the adsorbent. A ketone, having from 3 to 8 carbon atoms, such as 2-heptanone, or a mixture thereof, alone or admixed with a normal alkane can be selected as the desorbent.

A chromatographic process able to separate para-xylene frpm C.sub.8 isomers and C.sub.9 aromatics. In the process, the para-xylene-containing feed mixture is contacted with an X or Y zeolite adsorbent having Group IA or IIA cations, e.g., barium and/or potassium, at exchangeable cationic sites. The para-xylene components are selectively adsorbed onto the adsorbent. The non-adsorbed feed is then removed from the adsorbent and the para-xylene recovered by desorption with tetralin or alkyl derivatives of tetralin. The C.sub.9 's and the other xylene isomers in the raffinate, can be separated from this heavy desorbent by fractionation of the raffinate and the desorbent recycled to the process.

This invention comprises a process for separating 3,5-diethyltoluene from a feed mixture comprising 3,5-diethyltoluene and at least one isomer thereof, which process comprises contacting the mixture at adsorption conditions with an adsorbent comprising an X zeolite cation exchange with a K cation, thereby selectively adsorbing the 3,5-diethyltoluene. The remainder of the feed mixture is removed by desorption at desorption conditions with a desorbent material comprising a monocyclic alkyl-substituted aromatic hydrocation, e.g., p- or m-diethylbenzene or p-cymene and optionally, a diluent, e.g., isooctane.

Extractive chromatographic separation process for recovering

A chromatographic process able to separate para-xylene from C.sub.8 isomers and C.sub.9 aromatics. In the process, the para-xylene-containing feed mixture is contacted with an X or Y zeolite adsorbent having Group IA or IIA cations, e.g., barium and/or potassium at exchangeable cationic sites. The para-xylene is selectively adsorbed onto the adsorbent. The feed is then removed from the adsorbent and the para-xylene recovered by desorption with diethyltoluene. The C.sub.9 's and the other xylene isomers in the raffinate, can be separated from this heavy desorbent by fractionation of the raffinate and the desorbent recycled to the process. The preferred desorbents are 2,3-diethyltoluene, 2,5-diethyltoluene and 2,6-diethyltoluene.

Zeolitic para-xylene separation with diethyltoluene heavy desorbent

The chromatographic adsorption separation of coumarone from indene-containing coal tar distillate feed mixtures with an alkali metal (Group IA) exchanged X-zeolite and polar materials, e.g., ketones, alcohols or esters as desorbents. Also disclosed is a process for separating a coumarone-indene coextract with sodium-exchanged Y zeolite and toluene as desorbent.

Separation of coumarone from indene

An adsorptive separation process useful in the purification of alpha naphthol-containing feed mixtures, said process comprising the employment of a type X, type Y or a de-aluminated type Y zeolite material and a desorbent material comprising a primary alcohol or an alkyl ester.

Purification of alpha naphthol-containing feedstock by adsorption

A chromatographic process able to separate para-ethyltoluene from feed mixtures of C.sub.8 and/or C.sub.9 aromatic hydrocarbons. In the process, the para-ethyltoluene-containing feed mixture is contacted with a Y zeolite adsorbent having potassium at exchangeable cationic sites. The para-ethyltoluene is selectively adsorbed onto the adsorbent. The non-adsorbed components of the feed are then removed from the adsorbent and the para-ethyltoluene recovered by desorption with tetralin or alkyl or dialkyl derivatives of tetralin or alkyl derivatives of naphthalene. The other C.sub.9 's and the xylene isomers in the raffinate and p-ethyltoluene in the extract can be separated from the heavy desorbent by fractionation of the raffinate or extract and the desorbent recycled to the process.

Zeolitic para-ethyltoluene separation with tetralin heavy desorbent

A process for separating 3,5-diethyltoluene (3,5-DET) and/or 2,6-diethyltoluene (2,6-DET) from a feed mixture comprising at least one isomer from the group 3,5- and 2,6-diethyltoluene and at least one other isomer thereof, which process comprises contacting the mixture at adsorption conditions with an adsorbent comprising an X zeolite, cation exchanged with a mixture of barium and potassium or sodium, lithium, barium or copper cations or mixtures thereof or a Y zeolite cation exchanged with barium, calcium, sodium, potassium or copper cations or mixtures thereof, thereby selectively adsorbing one or more of said isomers and removing one or more relatively non-adsorbed isomer(s) from contact with the adsorbent. 2,6-diethyltoluene is the most strongly adsorbed isomer with certain adsorbents and is recovered by desorption at desorption conditions with a desorbent material comprising a monocyclic alkyl-substituted aromatic hydrocarbon, e.g., p-diethylbenzene, m-diethylbenzene, p-xylene or p-toluene and optionally, a diluent, e.g., a straight chain or branched paraffin, e.g., n-heptane or iso-octane, an ether or a halogenated hydrocarbon. With certain adsorbents 3,5-DET is the least strongly adsorbed isomer and can be recovered in the raffinate. Certain of the adsorbent-cation combinations perform the dual function of strongly adsorbing 2,6-DET and least strongly adsorbing 3,5-DET.

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Evanston, IL, United States of America

Hermann A Zinnen