Solution, extraction catalyst from aqueous

Xylose is obtained from sulfite Hquors, particularly from hardwoods, such as birch, by methanol extraction of concentrates or dried sulfite lyes, ultrafiltration (qv) and reverse osmosis (qv), ion exchange, ion exclusion, or combinations of these treatments (201). Hydrogenation of xylose is carried out in aqueous solution, usually at basic pH. The Raney nickel catalyst has a loading of 2% at 125°C and 3.5 MPa (515 psi) (202,203). 

The mixture is filtered off from the catalyst, made acidic with dilute hydrochloric acid, and the methanol is removed under vacuum. The remaining aqueous solution is made alkaline with solution of sodium hydroxide and extracted with ether. After drying and concentrating the ether extract, there is obtained 1 7 g 1 -isoprOpylamino-4,4boiling point164°Cto 165°C/0.05 mm. The hydrochloride melts at 230°C. 

Kawasaki et /. (1996) have used a supported membrane catalyst for extraction of erythromycin from its dilute, slightly alkaline aqueous solutions. 1-Decanol was used as an intermediate fluid membrane phase and a buffered acidic aqueous solution was used to strip the organic membrane. 

Smaller aldehydes form cyclic acetal-type oligomers readily in aqueous conditions.60 Diols and polyols also form cyclic acetals with various aldehydes readily in water, which has been applied in the extraction of polyhydroxy compounds from dilute aqueous solutions.61 E in water was found to be an efficient catalyst for chemoselective protection of aliphatic and aromatic aldehydes with HSCH2CH2OH to give 1,3-oxathiolane acetals under mild conditions (Eq. 5.7).62... 

InTox A process for destroying toxic wastes in aqueous solution by oxidation with oxygen at high temperatures and pressures in a pipe reactor. No catalyst is required. The reactions take place at approximately 300°C and 120 atm. Developed by InTox Corporation, UK, based on a process for extracting aluminum from bauxite developed by Lurgi in the 1960s. See also Zimpro. 

It is possible to extract the nanocolloids from aqueous solution into an organic phase or to support them onto inorganic supports by what is called the precursor method (described in Section 3.5) to generate heterogeneous catalysts. Such catalysts find application in chemical catalysis, e.g., in selective hydrogenation of fatty acids. 

In most ammonia plants, there are facilities to remove CO from the feed because CO will poison the catalyst. Generally, the technique used is to react the CO with water to produce CO2 and H2. The CO2 is removed by solvent extraction, and the H2 is recycled. (In case you were wondering, typical solvents used to remove CO2 are ethanolamine or an aqueous solution of potassium carbonate.)... 

The TPA process. The technology involves the oxidation of p-xylene, as shown already in Figure 18—2. The reaction takes place in the liquid phase in an acetic acid solvent at 400°F and 200 psi, with a cobalt acetate/ manganese acetate catalyst and sodium bromide promoter. Excess air is present to ensure the p-xylene is fully oxidized and to minimize by-products. The reaction time is about one hour. Yields are 90—95% based on the amount of p-xylene that ends up as TPA. Solid TPA has only limited solubility in acetic acid, so happily the TPA crystals drop out of solution as they form. They are continuously removed by filtration of a slipstream from the bottom of the reactor. The crude TPA is purified by aqueous methanol extraction that gives 99 % pure flakes. 

In the classical oxo process the catalyst cohalt carbonyl is formed in situ by introducing divalent cobalt into the reactor. High temperature is required for this catalyst formation that gives a mixture of aldehydes and alcohols containing only 60-70% of linear product. A new BASF process using cobalt carbonyl hydride shows improved selectivity and efficient catalyst recovery. The catalyst is prepared by passing an aqueous solution of cobalt salt over a promoter and extracting the catalyst from the water phase with olefin. 

A number of simple and inexpensive materials catalytically promote the cobalt-carbonylation (Reaction 2) in aqueous solution. These include ion-exchange resins, zeolites, or special types of activated carbon. Formation of the active catalyst in a separate reactor is thus economically feasible. The mechanism of this catalysis has not yet been elucidated and seems to differ for each promoter mentioned. After an induction period during which the cobalt fed to the reactor is partially retained by the promoter, fully active materials have absorbed cobalt carbonyl anion Co(CO)4 (ion exchange resins), Co2+ cation (zeolites), or a mixture of Co2+, cobalt carbonyl hydride, and cluster-type cobalt carbonyls (activated carbon). This can be shown by analytical studies (extraction, titration, and IR studies) of active material withdrawn from the reactor. 

Step 2 Extraction of the Catalyst from the Aqueous Solution. It is not feasible technically to charge the aqueous solution of cobalt carbonyl hydride directly into the hydroformylation reactor because two phases may form, especially with the long chain olefins. The most direct and most efficient way to eliminate water while permitting full use of the carbonyl catalyst is to extract it from the water phase with the olefin intended for hydroformylation. The extraction is carried out between... 

Most reactions in two-phase systems occur in a liquid phase following the transfer of a reactant across an interface these are commonly known as extractive reactions. If the transfer is facilitated by a catalyst, it is known as phase-transfer catalysis [2]. Unusually, reactions may actually occur at an interface (interfacial reactions) examples include solvolysis and nucleophilic substitution reactions of aliphatic acid chlorides [3 ] and the extraction of cupric ion from aqueous solution using oxime ligands insoluble in water [4], see Section 5.2.1.3(ii). 

Kuntz subsequently showed that the RhCl (tppts) 3 catalyzed the hydroformylation of propylene in an aqueous biphasic system [29]. These results were further developed, in collaboration with Ruhrchemie, to become what is known as the Ruhrchemie/Rhone-Poulenc two-phase process for the hydroformylation of propylene to n-butanal [18, 19, 22, 30]. Ruhrchemie developed a method for the large scale production of tppts by sulfonation of triphenylphosphine with 30% oleum at 20 °C for 24 h. The product is obtained in 95% purity by dilution with water, extraction with a water insoluble amine, such as tri(isooctylamine), and pH-controlled re-extraction of the sodium salt of tppts into water with a 5% aqueous solution of NaOH. The first commercial plant came on stream in 1984, with a capacity of 100000 tons per annum of butanal. Today the capacity is ca. 400000 tpa and a cumulative production of millions of tons. Typical reaction conditions are T=120°C, P=50bar, CO/H2 = 1.01, tppts/Rh = 50-100, [Rh] = 10-1000 ppm. The RhH(CO) (tppts)3 catalyst is prepared in situ from e.g. rhodium 2-ethylhexanoate and tppts in water. 

Cbncezning the cause of the detitanaiton it can be noted that it involves the breakage of Si-O Ti bonds, and like the dissolution, it requires the breakage of Si-O-Si bonds. Thus, the basicity of the reaction medium must be involved in the extraction of Ti from the framework. In fact an appropriate treatment of the fresh catalyst with an aqueous solution of ammonia causes detitanation as well as the reaction environment (Fig. 2). 

A mixture consisting of 254 parts of 2-nitro-l-phenyl-1-propanol. 600 parts of methanol, 90 parts of acetic acid, and 7 parts of Raney nickel catalyst, was reduced with molecular hydrogen under conditions similar to those set forth in Example 1. At the conclusion of the reduction, the charge was removed from the hydrogenation apparatus, and filtered. The filtrate was then distilled at atmospheric pressure up to a temperature of 80° C. to remove the methanol present. The still residue was next extracted with a 100-part portion of a 50-50 mixture of benzene butanol, in order to remove non-basic impurities from the crude reduction product. After considerable agitation, the resulting mixture was allowed, to settle, and the upper benzene-butanol layer discarded. To the aqueous solution of the phenyl amino propanol acetate (salt) was added 60 parts of sodium hydroxide in the form of a 50 percent solution. This treatment resulted in the formation of two separate layers. The upper layer, containing principally free phenyl amino propanol, was separated and distilled under reduced pressure (60-70 mm.) up to a temperature of 100° C. At this point the pressure was further reduced (1-2 mm), and substantially pure phenyl amino propanol was collected at 125° C. 

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