WO2012174486A1 - Versatile pressure apparatus for conducting chemical reactions with compressed gasses - Google Patents

Abstract

Disclosed is a chemical reactor assembly which bridges the chasm between academics and industry by way of its flexibility. Chemical reactor kits allow users to design and quickly implement their own reaction systems. By applying, various types of quick -release/connects couplings and control valves, researchers can plan and construct required configurations.

Description

VERSATILE PRESSURE APPARATUS FOR CONDUCTING CHEMICAL

REACTIONS WITH COMPRESSED GASSES

CROSS-REFERENCE TO A RELATED APPLICATION

The present application claims priority to U.S. provisional application Serial No.

61/497,121, filed June 15, 2011, entitled "Versatile pressure apparatus for conducting chemical reactions with compressed gases". The entire content of the aforementioned provisional application is incorporated herein by reference.

BACKGROUND

Organic syntheses include many steps, like preparations and introductions of substrates, solvents, other reagents, as well as catalysts. Many chemical reactions are also conducted under specific conditions that require an inert atmosphere. Some of them require different temperatures, different types of gases (air, argon, nitrogen, CO, C0₂, H₂, D₂, ethylene, butane and others) and variable pressure settings. Reactions like the formation of carbon-carbon, carbon-nitrogen, or carbon-sulfur bonds frequently require an inert atmosphere and atmospheric pressure. Hydrogenation reactions, particularly with heterogeneous and homogenous catalysts, require hydrogen gas, under low pressure (0-60 psig) or medium pressure (60-150 psig). Similarly, carbonylation reactions require soluble catalysts and carbon monoxide gas under medium or high pressure. Pressure dependent chemical reactions are mostly performed in metal designed reactors or in thick-walled glass vessels that require tools to assemble them. To contain gasses in a reaction vessel is usually a complex and inconvenient procedure.

The most known commercially available hydrogenation apparatus, used in chemical laboratories, is the Parr shaker-type apparatus, designed in 1921 year, published in 1923, and offered commercially by Parr in about 1926. The broad usefulness of this apparatus is best illustrated by the numerous examples, in chemical literature, published during the past eighty years. However, the apparatus is expensive, difficult to clean and uses a single reaction vessel, limiting the number of experiments running at the same time. Finally, the Parr apparatus is solely dedicated to hydrogenation and cannot be used for other type of reactions such as carbonylation.

Over the years a number of different hydrogenation apparatuses have been developed and reviewed. They were designed to accommodate variety of temperatures and pressure. A low pressure hydrogenation apparatus, for example a type of Schlenk-tube, was employed for asymmetric hydro genations. In general, it first requires a reaction mixture to be prepared in a Schlenk-tube, degassed by freeze-thaw cycles, and then transferred, for hydrogenation, into a glass autoclave equipped with: (i) a gas inlet tube; (ii) a septa covered stop valve; (iii) and a pressure gauge. In other words, the hydrogenation process required two steps: the preparation of a reaction mixture, in one vessel, and then performing a chemical reaction in a second vessel. A schematic representation of a modified Schlenk-tube, for hydrogenation, is also described by Warad where, the first step e.g., degassing and hydrogenation processes had been performed in a glass vessel. The usefulness of such systems tends to be limited to scientific teaching institutions, and although published, it has never been commercialized.

Another, set of apparatus, Pressure Reaction Vessels, Lab-Crest®, have been produced and commercialized by Andrews Glass Co. The apparatus consists of borosilicate glass, female/male coupling components, a PTFE insert, a PTFE O-Ring, a stainless steel plug, and valves: a needle valve and a pressure release valve. The application of Lab-Crest®, to catalytic carbonylation reactions, was recently described by Denmark and Hoover. A totally different type of hydrogenation apparatus, H-Cube®, using the continuous flow of a high-pressure reactor system has been developed by ThalesNano Inc. In this system a continuous flow of substrate is combined with hydrogen generated in-situ from electrolysis of water. Although, H-Cube® seems to be very attractive for chemists, the apparatus is very expensive ($50k - $60k), limited to certain catalyst e.g., Pd/C, Rh/C, Pt0₂ as well as limited to batch scale (0.1 -100 g). In addition, it is only adapted to one type of the reaction.

Reviews of other commercially available options (atmospheric/balloon hydrogenation, pressure bottles, autoclaves, and shakers) are mostly applied to the hydrogenation reactions and are cumbersome and represent lack of versatility.

Recently, industrial and academic laboratories have turned to combinatorial methodology and high-throughput screening techniques in pressure dependent reactions. These typically involve an arrangement of many parallel chemical reactors. This paralleled assembly, in general, comprises of a plurality of reactor vessels and plurality of valves configured to allow a gas flow into the reactor vessels. Usually the gas is supplied to reactors at higher pressure than pressure within reactor vessels. Very often the equipment is very expensive. In order to reduce cost, some laboratories construct in-house less expensive systems. For example, Bradleys et al. described a low/medium-pressure hydrogenation manifold for catalyst evaluation. Their four- port manifold is connected with reaction glass vessels via thick-walled plastic tubing screwed directly into a Teflon® adapter. This system is good for small volumes of a reaction mixture, however, is unsuitable for large volumes of solutions, since it requires screwing/unscrewing the whole bottle with its content possibly causing spillage.

Another gas manifold, for olefin polymerization, is described by Constable at al. Reaction vessels with their coupling assemblies are attached to a seven-port manifold via adaptors, self-sealing quick connects or on/off ball valves, and flexible stainless steel tubing. The withdrawback of this, in-house, constructed system, is that each size of reaction vessel (70 mL to 300 mL) requires a specially designed and manufactured coupling assembly.

As is apparent from the foregoing review, standard laboratory reactors for chemical reactions, running under pressure not exceeding 150 psig, are generally heavy devices made of thick-walled glass or metal parts requiring more or less intricate assembly with simple or specialized tools. There is a need, therefore, for a versatile easy-to-assemble and disassemble reactor, easily adaptable for conducting a variety of chemical reactions under pressure in a general laboratory setting, or in any other setting where portability and adaptability are desired.

SUMMARY

The present invention via embodiments disclosed hereinafter and many other embodiments within the scope of the claims of this patent overcome the problems as set forth above and/or afford other related advantages. The current disclosure describes various embodiments allowing for an easy assembly and disassembly of a variety of chemical reactors. It is an aim of the disclosed embodiments and many other embodiments within the scope of the present teachings to provide for a reactor that can be rapidly and safely assembled prior to running any chemical reaction. The disclosure provides for chemical reactors that do not require any tools to assemble and then to dissemble. Chemists are able to choose the most suitable configuration of a reactor for their experiment, to assemble the reactor rapidly, as well as to connect it easily to compressed gas sources. Moreover, the suitably configured reactor can be utilized as a portable unit, and easily transported between laboratories. Toward these goals, modular components are disclosed herein that include glass vessels variable sizes, pressure gauges, and durable metal parts, such as control valves, quick-connects/disconnects couplings, with different types of fittings, as well as other parts described.

In general, following the present teachings a chemical reactor can be assembled and applied for conducting any type of reactions that are to proceed in air or inert atmosphere, as well as under atmospheric-, low-, or medium-pressure, and/or under catalytic conditions. In one aspect, a reactor is disclosed that is very useful for catalytic hydrogenation processes under medium pressure.

A chemical rector prepared according to the present teachings can be employed in industrial or academic chemical laboratories, in classroom demonstrations and exercises, for educational outreach to high school students, and in independent activities.

BRIEF DESCRIPTION OF THE DRAWINGS

The present invention, including device, apparatus and method aspects, is illustratively shown and described in reference to the accompanying drawings.

Figure 1 is an illustration of an embodiment of an apparatus of the current invention, which consists of three panels a, b, and c. Panel a illustrates an assembled embodiment of the Snap-Reactor that consists of two coupled portions, e.g. Snap-Vessel 100 and Snap-Manifold 200. Panel c illustrates a single decoupled Snap-Vessel 100. Panel b illustrates a single decoupled Snap-Manifold 200.

Figure 2 illustrates apparatus Model-A, comprising decoupled portions 100 and 200, and shows descriptions and numbering of removable parts. Model-A illustrates Snap-Reactor with a DESO quick-connects type, 6 and 8, while permanently connected to a gas line via plastic tubing 15.

Figure 3 illustrates apparatus Model-A 1, comprising decoupled portions 101 and 200, and shows descriptions and numbering of removable parts. Model-Al illustrates the Snap- Reactor with a SESO quick-connects, 5 and 8, while permanently connected to a gas line via plastic tubing 15.

Figure 4 illustrates apparatus Model-B, comprising decoupled portions 100 and 201, and shows descriptions and numbering of removable parts. Model-B illustrates the Snap-Reactor with a DESO quick-connects, 6 and 8, and with the possibility to adjust the gas flow by a valve 13, when it is connected to a gas source in a remote distance. Figure 5 illustrates apparatus Model-Bl, comprising decoupled portions 101 and 201, and shows description and numbering of removable parts. Model-Bl illustrates the Snap-Reactor with a SESO quick-connects, 5 and 8, and with the possibility to adjust the gas flow by a valve 13, when it is connected to a gas source in a remote distance.

Figure 6 illustrates apparatus Model C, comprising decoupled portions 102 and 202, and shows descriptions and numbering of removable parts. Model-C illustrates the Snap-Reactor equipped with a FF quick-connects 7 and 9, gas flow regulating valve 13, injection port 18 or 24, and ball valve 131. This assembly is employed for delivering air-sensitive reagents, without decoupling the quick-connects (7 and 9). Snap-Manifold 202 is attached permanently to a gas line and a vacuum system, via tubing 15 and via needle valve 16, respectively.

Figure 7 illustrates apparatus Model-D, comprising decoupled portions 100 and 203, and shows descriptions and numbering of removable parts. Model-D illustrates the Snap-Reactor with additional DESO quick-connects, 61 and 81. This assembly allows for disconnecting the Snap-Reactor from a gas source and then re-loading with the reacting gas. Model-D also represents a portable unit after disconnecting form the vacuum system.

Figure 8 illustrates apparatus Model-E, comprising decoupled portions 101 and 203, and shows descriptions and numbering of removable parts. Model-E illustrates the Snap-Reactor with additional DESO quick-connects 61 and 81. This assembly allows for disconnecting the Snap-Reactor from a gas line and then reloading with the reacting gas. Model-E also represents a portable unit.

Figure 9 illustrates apparatus Model-F, comprising decoupled portions 102 and 204, and shows descriptions and numbering of removable parts. Model-F illustrates the Snap-Reactor equipped with injection port 18 or 24 and ball valve 131, and additional DESO quick-connects 61 and 81. This model requires at least a mono-port manifold 206. It is also employed for connecting to n-port-manifolds.

Figure 10 illustrates apparatus Model-G, comprising decoupled portions 100 and 205, and shows descriptions and numbering of removable parts. Model-G illustrates the Snap- Reactor with additional quick-connects 61 and 81 (DESO) in the Snap-Manifold. This model is used for connecting to n-port-manifolds. It also represents a portable unit.

Figure 11 illustrates apparatus Model-G, comprising coupled embodiments 100 and 205 and a mono-port manifold 206, and shows descriptions and numbering of removable parts. Panel d illustrates mono-port manifold 206 that serves as a purging system. Model-G illustrates a portable unit of the Snap-Reactor. After purging and decoupling from the mono-port manifold 206, the Snap-Reactor can be transported to a different place in the laboratory.

Figure 12 illustrates a 2-port-manifold 207 together with two disconnected embodiments of the Snap-Reactors Model-G (as shown in Figure 10). The 2-port manifold 207 serves as: (i) a purging system 208/209; (ii) a safety system with a pressure regulated relief valve 22; (iii) an individual pressure regulating systems 29 and 13; and (iv) a vacuum regulating system 16. Removable parts of the 2-port manifold are described and numbered.

Figure 13 illustrates a 3 -port manifold 210 with disconnected embodiments of two Model-G units and one Model F unit. The 3 -port manifold 210 serves as: (i) a purging system 208/209; (ii) a safety system 22; and (iii) pressure/vacuum regulating systems 29/13/16. Removable parts of the 3 -port-manifold 210 are described and numbered.

Figure 14 illustrates apparatus Model-H, representing a simplified Snap-Reactor. Model- H comprises disconnected Snap Vessel 100 and unit 211 which consists of a pressure gauge 12 and female body 8 (DESO) connected by a hex reducing coupling 40. Pressure gauge 12 is directly connected to female body 8 that, in turn can, be coupled to male stem 6 (DESO). Model- H can be used for monitoring the progress of chemical reactions where any gas is evolved (increased pressure) or the reacting gas is consumed (decreased pressure).

Figure 15 illustrates apparatus Model- AR (R designating 'relief), comprising disconnected portions 103 and 212 of decoupled Snap-Reactor. Model-AR, by analogy to Model A, utilizes Snap-Manifold 212 with an additional pressure relief valve 34. Snap-Vessel 103 is an example of a glass vessel comprising a round bottom flask. Removable parts are described and numbered.

Figure 16 illustrates the use of tube fitting connections in a DESO Snap-Reactor model. Figure 17 illustrates a round shaped Snap-Reactor protective cover.

Figure 18 illustrates a rectangular shaped Snap-Reactor protective cover. DETAILED DESCRIPTION

Following is a list of various elements that can be used to assemble a reactor of the present teachings.

Glass reaction vessel or a glass vessel 1 is a bottle or a tube fabricated of heavy-wall borosilicate glass. The neck of the vessel is internally threaded and includes a groove for a seal (O-ring). The vessel is adopted to operate in low- and medium pressure systems. The thickness of the glass wall depends on the internal pressure applied, and is between 5 and 9 mm. All glass vessels are pressure tested up to 2.5x working pressure. The glass vessels are available in different sizes (100 mL to 4,000 mL): a bottom part of the 3-4 liters glass vessel 103 may have a rounded shape as illustrated in Figure 15.

Magnetic stir-bar 2 is a PTFE coated stir-bar. The size of the magnetic stir-bar used is determined by the size of the reaction vessel. The solution is agitated either by a PTFE coated magnetic stir-bar or a suspended magnetic stirrer on a freely rotating shaft.

O-ring seal 3 may be made of a synthetic polymer like fluoroelastomers, e.g., Viton® or

Karlez® or Simriz ®, or PTFE, e.g. Teflon®, as well as of any other suitable material that is resistant to chemicals. The properties of the seal can be selected to account for different sealing pressures and temperatures.

Adapter 4 is made of synthetic polymer, e.g. Nylon® or Teflon®. Adapter 4 is externally threaded to match the internally threaded neck of glass reaction vessel 1. The front of adapter 4 has a groove to accept an O-ring seal. Moreover, it has a 1/8" centrally threaded inner hole to accept a male stem of quick-release connects (DESO, SESO or FF). Adapter 4 comes in the standard 25/25 size, as well as other sizes.

Quick connect-disconnect fittings (or quick-release connects or quick-connects) comprise two parts: a male stem (5, 6, and 7) and a female body (8 or 81 and 9). It is a mechanical device which rapidly joins or separates the gas system components without the use of tools. The quick- connects couplings are designed to be used in positive pressure and vacuum systems: they come standard in brass or stainless steel. Different types of quick-connects couplings can be used, for example: single-end shut-off (SESO) (5 with 8 or 81), double-end shut-off (DESO) (6 with 8 or 81) and full-flow model (FF) (7 with 9). SESO quick-connects offer a shutoff valve in the female body 8 or 81 with no shut-off in the male stem 5. When the male stem 5 is removed from the female body 8 or 81, pressure is automatically shut off only at one end, e.g. at the female body 8 or 81. The male stem 5 of SESO has no valve and offers unrestricted flow.

DESO quick-connects are the same as SESO, but there is a small poppet valve in the male stem 6 or 61. Thus, when the male stem, 6 or 61, is removed from the female body 8 or 81, pressure is shut off automatically at both ends and consequently the flow is restricted.

FF quick-connects, both the male stem 7 and the female body 9, have no valves and offer straight-thorough flow with no restrictions whether connected or disconnected.

Union cross 10 is a 1/8" female modular part to which other modular parts such as quick- release connects, a pressure gauge, and valves are attached. The union cross 10 comes in the standard brass or stainless steel.

Reducing adapter 11 or 111 is a 1/2" threaded metal part with the 1/8" extension that connects two apertures having different diameters. It is made of brass or stainless steel.

Pressure gauge 12 is calibrated in psig, monitors an internal pressure in the reaction vessel. It is equipped with a ½ in. threaded extension to attach to a gas line.

Ball/needle valves 13 or only a ball valve 131 are used for isolation. They provide a highly reliable seal. A quarter turn of the handle of the valve quickly opens or closes the valve.

Tube fittings, either male tube fitting 14 or female tube fitting 141. They are made of brass or stainless steel.

Plastic tubing 15 made of polytetrafluoroethylene (PTFE), e.g. Teflon®, or any plastic material that is enough flexible and resistant to withstand low/medium pressures applied.

Needle valve 16 is a threaded valve that by manual actuation allows the valve to be opened or closed gradually: manual actuation is accomplished by rotary action with a screw thread stem.

Female hose connector 17 (HC) is made of brass or stainless steel. It has a specially designed serrated shank which properly stretches the tube for optimum sealing.

Rubber septum 18 is used for isolating and delivering reagents and/or solvents, as well as sampling.

Stainless steel tubes 19 are cylinders used to assemble multi-port manifolds. Female elbows 20 are threaded metal parts made of brass or stainless steel to accommodate other parts.

Female branch tee 21 (tee joint) is a threaded metal part made of brass or stainless steel to accommodate the stainless steel tubes and/or other metal parts.

Pressure relief valve 22 is a single-threaded valve that protects the reaction system from excessive pressure (overpressurizing). The valve is held closely by a spring as the system operates at its normal pressure. When the pressure increases to the set point of the valve, it opens automatically and remains open until the system pressure decreases to the release point. It is standard in brass or stainless steel.

Tape pipe threaded sealant 23 is a ¼ in. wide PTFE tape to wrap around the male thread.

The tape is used for to maintaining leak-free connections.

Septa 24 is made of PTFE face and perfluoroelasomer, e.g. Simriz® of silicone backing. The PTFE, e.g. Teflon®, liner has excellent chemical resistance while the silicon backing has reseal ability.

Hex reducing nipple coupling 25 is a ¼" threaded metal with a male NPT and a 1/8" threaded male NPT.

Pipe fitting hex nipple 26 is a threaded metal part with a male 1/8" NPT at both ends.

To complete the assembly the following elements may also be required: tube fitting reducing union 27; tube fitting female branch tee 28; pressure regulator 29; tube fitting female elbow 30 is a threaded metal part; hose 31 for connecting to a vacuum system; tube hose connector 33; and a three-threaded pressure relief valve 34.

The uses of the foregoing elements for assembling various embodiments of the reactors of the present teachings are illustrated in Figures 1-15. The various embodiments are illustrated as follows: (i) a coupled unit is illustrated in Figure 1, panel a; (ii) various decoupled units are illustrated in Figures 1-10; (iii) the uses as a part of mono- and multi-port manifolds are illustrated in Figures 11-13; (iv) the uses of a pressure relief valve 34 is illustrated in Figure 15.

Reactor Assembly

An embodiment Model A, of the reactor of the present teachings, termed hereinafter Snap-Reactor, is presented in Figures 1 and 2. Figure 1 shows the coupled Snap-Vessel 100 with Snap-Manifold 200 as a complete set (Figure 1, panel a), as well as a decoupled Snap-Manifold (1, panel b) from the Snap-Vessel (Figure 1, panel c) as two independent parts.

In general, a whole unit of the Snap-Reactor consists of two main sections: the Snap- Vessel 100 and the Snap-Manifold 200. The heart of the Snap-Reactor is the quick-connects- disconnects fittings (DESO, SESO or FF) with their associated utilities.

Snap- Vessel 100 is the part in which a chemical reaction takes place (Figure 2). It comprises (i) a glass vessel 1 comprising a 1/8" internally threaded neck with a groove for an O- ring, (ii) an externally and internally threaded adapter 4, and (iii) a male stem of quick-connects couplings (DESO) 6.

Snap-Manifold 200 is a part of a purging system while coupled with the Snap-Vessel

100. It serves not only as a purging system, but also serves as delivering system. It delivers reacting gasses to the glass vessel 1 as well as, in some configurations, it is employed to add adequate reagents (see Figures 6 and 9). An example of Snap-Manifold 200 is described in Figure 2. It comprises: (i) a female body 8; (ii) a union cross 10; (iii) reducing adapter 11; (iv) a pressure gauge 12; (v) a tube fitting 14; (vi) plastic tubing 15; (vii) a needle valve 16; (viii) a male hose connector 17; and (ix) a hose 31. Other examples of Snap-Manifold are illustrated in Figures 3-10.

Snap-Vessel and Snap-Manifold are coupled via selected quick-connect/release fittings in order to assembly the Snap-Reactor (Figure 1, panel a). The quick-connects/release set is the heart of Snap-Reactor. The quick-connects set consists of two parts, a male stem 5, 6 or 7 and a female body 8 or 9. Three different types of quick-connects/release fittings can be applied in designing and constructing Snap-Reactor: a double-end shut-off (DESO) 6 or 8 (Figure 2), single-end shut-off (SESO) 5 or 8 (Figure 3), and full-flow (FF) 7 or 9 (Figure 6).

The female bodies of the quick-connects of the DESO and SESO, 8, are constructed in the same way. They both offer a shut-off valve in the female body when decoupled. It means that when the quick-connects of SESO (5 with 8) or DESO (6 with 8) is decoupled, the flow of a gas from a gas source is disconnected, but not shut-off.

The female body of the FF quick-connects differs from the female body of DESO. When two parts of the quick-connects fittings of FF, 7 and 9, are both coupled or decoupled the female body allows unrestricted flow. On the other hand, the male stem of the three quick-connects fittings, SESO 5 or DESO 6, or FF 7, are constructed differently. Of the three male stems of quick-connects couplings (SESO, DESO, and FF), only DESO 6 has a small poppet valve which permanently restricts flow of gas when decoupled. The remaining two male stems of the quick-connects, SESO 5 and FF 7, allow unrestricted flow when decoupled. These properties of the male stems are utilized to design and construct different models of Snap-Reactor, Models A-G (see Figures 2-10). The properties of the male stem 6 of the DESO quick-connects are employed for designing: (i) a portable reactor; (ii) loading very sensitive reagents in a glow box; (iii) for attaching Snap- Reactor to external mono-port and multi-port manifolds (Figures 11, 12, and 13). On the other hand, a FF male stem is used for designing Snap-Reactor with a special mode of delivery of reagents: via a septum or septa (Figure 9). Its function is not only important for delivering reagents to a reaction mixture, into a reaction vessel, but also for taking a sample for analyses (sampling) for monitoring progress of a chemical reaction.

To assemble Snap-Reactor units, Snap-Vessel and Snap-Manifold (Figure 1) are rapidly connected together with quick-release connects, e.g., a male stem (5 or 6 or 7) with a female body (8 or 9). Subsequently, a male stem 6 is inserted into female body 8 (Figures 2, 4, and 7) or a male stem 5 is inserted into a female body 8 (Figures 3, 5, and 8) or a male stem 7 is inserted into a female body 9 (Figures 6 and 9) by pressing a snap ring located around the female body (Figures 2-11). The locking mechanism then locks the component halves together.

To disassemble Snap-Reactor, Snap-Vessel and Snap-Manifold are rapidly disconnected via the same quick-release connects by pulling down a snap ring (body sleeve) 8 or 9 around the female body.

The simplest model of Snap-Reactor, Model A, is illustrated in Figure 2. Its Snap- Vessel, the lower section of the chemical apparatus, is comprised of four parts: (i) a glass reaction vessel 1; (ii) a PTFE e.g., Teflon® encapsulated magnetic stir-bar 2; (iii) a PTFE e.g., Teflon® adapter 4 with an O-ring 3; (iv) a male stem (DESO 6). The glass reaction vessel 1 is made of heavy- wall borosilicate glass. The thickness of the glass wall, estimated to be approximately between 5 and 9 mm, is dependent on the internal pressure and the volume of the glass vessel. The glass vessels are designed to operate in atmospheric-, low- and medium- pressure systems. All glass vessels are pressure tested up to 2.5x working pressure. They are available in different volumes (50 mL to 4 L). The vessel has an internally threaded neck and includes a groove for receiving a seal 3. The largest glass vessel (4 L) is a round-bottom vessel to adopt an egg-shaped magnetic stir-bar.

The glass vessel is fitted with 25/25 (or other size) polyamide, e.g. Nylon, or a PTFE e.g., Teflon, externally threaded reusable adapter 4. The adapter is securely held by an O-ring compression seal 3 with, for example, 1/8" NPT female thread to accept a male stem 6 of the quick-release/connects fittings. No additional tools are needed, hand tightening or release suffices. The latter provides a simple, easy, and fast closure. Into the adapter 4 is screwed a male stem 6 (DESO).

A PTFE, e.g. Teflon® encapsulated magnetic stir-bar 2, at the bottom of the glass vessel, is used to agitate a reaction mixture. Similarly, a magnetic stir-bar can be suspended on a freely rotating shaft (not shown).

Snap-Manifold of Model-A (Figure 2) in the upper section of the chemical apparatus, is constructed of multiple modular parts that allow for the designing of a flexible hydrogen/reaction gas system. Snap-Manifold 200, in general, is comprised of five parts: (i) a four-way union cross 10; (ii) a needle valve 16; (iii) a pressure gauge 12; (iv) a female body of a quick- release/connects 8; (v) tube fittings 14. The union cross 10 has three 1/8" female threads for connecting to a female body (DESO/SESO) 8, a tube fitting 14 for connecting to plastic tubing 15 and then to a gas source, and needle valve 16. Needle valve 16 is further attached to male hose connector 17 that, in turn, is connected to a vacuum system. A fourth thread is 1/8" NPT adapted to a 1/4" NPT reducing adapter 11 for connecting to a 0-60 psig, 2.5" diameter pressure gauge 12. The female body 8 of Model-A of the Snap-Manifold 200 is compatible with the DESO or SESO of the male stem 6 inserted into adapter 4.

Model A is constructed in such a way that a reaction mixture is continuously charged with hydrogen gas (or reacting gas). Thus this model provides a constant pressure in the glass reaction vessel 1 during the chemical reaction process. Additionally, the pressure in the Snap- Manifold 200 is not affected during the addition of reagents or during sampling. Both SESO and DESO models, of the female body 8, can be used with a reaction mixture comprising liquid- reacting gas, liquid-liquid, or liquid-solid chemical systems. SESO and DESO differ in that the male stem 6 of DESO, screwed into adapter 4, has no opening when decoupled and the flow is restricted. Therefore, in this particular DESO case, of the male stem 6, the adapter 4 needs to be unscrewed prior to charging reagents or sampling processes. On the other hand, when dealing with moisture sensitive reagents it is advised to employ the quick-connects of a DESO male stem 6 type, because reagents can be delivered ether in a glove box or under a blanket of an inert gas. In general, once required chemical components are added to a glass vessel in a glove box, the vessel is tightly closed with the adapter, having a DESO male stem 6, since it has a blocking poppet. Subsequently, Snap-Vessel 100 is removed from the glove box, and then attached to Snap-Manifold 200 via a female body 8 (DESO/SESO). The blocking properties of the DESO quick-connects assembly are very useful when dealing with extremely moisture- or oxygen-sensitive reagents.

Other models of Snap-Manifold relevant to Model-A are Models-Al, B, Bl, C, and D-G (Figures 2-10). Five models, A-C (Figures 2-6), bare similar functionality. They are attached permanently to a gas line during a chemical process via plastic tubing 15. The remaining four models D-G (Figures 7-10) can be detached from the gas line, by decoupling of the male stem 61 from a female body 81. Next, the Snap-Reactor can be transported into a desired place in the chemical laboratory. The optional design of Snap-Manifold depends not only on conducted chemical processes, but also on whether the Snap-Reactor is attached permanently (Figures 2-6) or temporarily (Figures 7-13) to a gas source or to a mono-port manifold (Figure 11) or a multi- port manifold (Figures 12-13). An example of a temporary attachment presented in Figures 7 and 8 can be also used as a permanent. Design models define which modular parts should be utilized. Parts presented in Table 1 are used for constructing various Snap-Reactor models (A-G). The listed parts are representative examples, and can be interchanged with equivalent parts according to the desired configuration of Snap-Manifold that is dictated by chemical processes.

For example, to construct Model Al (Figure 3), the male stem 6 of a DESO type was exchange for a male stem of the SESO type 5. Thus Model Al is used when the delivery of secondary reagents and sampling is through an opening in the male stem 5 when the quick- connects are decoupled.

To construct Model B (Figure 4), an additional ball valve 13 (optional a needle valve 16) was added to Model A. This additional valve is used to facilitate purging when the source of a gas is at an inconvenient distance from the Snap-Reactor. Model-Bl is similar to Model B, but instead of DESO male stem 6 it has SESO male stem 5, (Figure 5).

Another model, Model C (shown in Figure 6) similarly to Model A is permanently attached to a gas source. Opposite to Model A, in Model C chemical components can be delivered via a septum 18 or septa 24, since the quick-connects between the Snap-Vessel and the Snap-Manifold are a FF type. The Snap-Manifold of Model C comprises of the following parts: (i) a union cross 10; (ii) a pipe fitting hex reducing nipple, ¼" male NPT and 1/8" male NPT, 25; (iii) a female body (FF) 9; (iv) a needle valve 16; (v) a female hose connector 17; (vi) hose 31; (vii) a ball valve 131; (viii) a septum 18 or septa 24; (ix) a pipe fitting hex nipple 26; (x) a female branch tee 1/8" female NPT 21; (xi) a pipe fitting reducing adapter 1/8" male NPT adopted to ¼" female NPT 11; (xii) a pressure gauge 12; (xiii) a ball (or needle) valve 13; (xiv) female tube fitting 141; and (xv) a plastic tubing 15 to connect to a gas source. The main differences in Model C, comparing with previously illustrated models, relay on a type of the quick-connects fittings used and, consequently, on the way that chemical components are delivered. Thus the Snap-Manifold 202 of Model C has a female body 9 of a full-flow type. Consequently, the male stem 7 of the Snap-vessel is also a full flow type. Whether it is coupled or decoupled, it offers the high capacity straight-through flow with no restriction. Opposite to other models, in Model C the male stem 7 is not connected directly to the adapter 4, but it is coupled via the 1/4" - 1/8" reducing adapter 111. In Model C, one of the union cross threads has a 1/8" NPT adapted to a ¼" NPT hex reducing nipple 25 for connecting to the female body 9. Two remaining, the 1/8" female threads are for connecting to a ball valve 131 and the needle valve 16. The ball valve 131 is capped, on the top, with a septum 18 or septa 24. The needle valve 16 is further attached to a female hose connector 17 that, in turn, is connected to the hose 31 and then to a vacuum system. The fourth thread has a 1/8" NPT adapted to a pipe fitting hex nipple 26, that in turn is connected to a 1/8" female branch tee 21. To the female branch tee 21 are attached a 1/8" NPT adapted to a ¼" NPT reducing adapter 11 for connecting to the pressure gauge 12 and to the ball or (needle) valve 13. The ball valve 13 is connected further to the female tubing fitting 141 for connecting, to a gas source, via plastic tubing 15. The Snap- Reactor, and in particular, the Snap-Manifold 202, of Model C, was designed to permit air- sensitive liquid chemical components to be introduced, under strict inert conditions, via septum 18 or septa 24, using a syringe or cannula.

Other models of designed Snap-Manifolds (Figures 7-11) represent the Snap-Reactor that can be permanently or temporary attached to a gas line (Figures 7 and 9) or attached to a mono- port manifold (Figure 12), or a multi-port manifold (Figure 13) with some modifications. Following is an example of the portable Snap-Reactor (Figure 7) e.g., the Snap-Reactor is attached temporary to a gas line. The following steps are required: (i) charging the glass vessel 1 with a solvent and required chemical components.; (ii) coupling the Snap-Manifold 203 with the Snap-Vessel 100; (iii) connecting a female body 81 with a male stem 61; (iii) purging, and then filling the system with an inert gas or a reacting gas through plastic tubing 15 to a desire pressure; (iv) stopping the gas supply, by decoupling the female body 81 from the male stem 61; (v) detaching the hose 31 from the male hose connector 17; (vi) transporting the Snap-Reactor to a desire place in the laboratory. Five Snap-Reactors, Models A-E (Figures 2 - 8), were designed to operate as individual units, either attached permanently or temporarily to a gas line. Additionally, two Snap-Reactors, Model F and G (Figures 9 and 10), were designed to operate with a mono-port- 206 (Figure 11) or two port- 207 (Figure 12) or three-port manifold 210 (Figures 13).

Conceivably, multi-port manifolds 207 and 210 (Figures 12 and 13) can be build to include as many ports as desired, since in construction each individual port is added on the manifold via a certain inch diameter spacing tubing in the reactive, and vacuum/inert gas line. The exemplary multi-port manifold of the present teachings is represented by a 2-port design 207 (Figure 12). Spacing between the ports of about 10-16 in. comfortably allows for an individual magnetic stirring. The manifold can be anchored with clamps to a rigid grid in a fume hood, to enhance portability and minimize setup time.

While the multi-port manifolds, 207 and 210, accept more than one reactor (Figures 12 and 13), a mono-port manifold 206 is designed to accept one reactor at a time (Figure 11). The exemplary mono-port manifold of the present teachings (Figure 11) is assembled from the following parts: (i) plastic tubing 15; (ii) female tube fitting 141; (iii) a ball (or needle 16) valve 13; (iv) a female branch tee join 21; (v) needle valve 16; (vi) female hose connector 17; (vii) hose 31; (viii) male tube fitting 14; and (ix) a female body (DESO) 81. The mono-port manifold (Figure 11) combines a gas line and a vacuum line via the female branch tee join 21 to which a female body 81 (DESO/SESO) is attached via a plastic tube fitting 15. Further the female body connector 81 is coupled to a male stem (DESO) 61 of the Snap-Reactor 100/205 to construct the whole system.

An exemplary individual 2-port-manifold 207 is shown in Figure 12. It is constructed of

1/4 in. stainless steel tubing 19 and joined with the standard tube fitting tee 28 and female elbow tube fittings 30. The space tubing is joined together by a modular set comprising pressure regulator 29, the ball valve 13, the female branch tee 21, and the needle valve 16. This manifold combines lines for inert/reacting gases 209, a vacuum line 208, a pressure regulated relive valve 22. The 2-port manifold 207 delivers reactive gases from the line 209 to all ports at the pressure specified at the gas source. To enable variations of this parameter, in-line pressure regulator 29 is inserted. Additionally, the ball valve 13 and the needle valve 16 are connected to the two ends of the female branch tee 21. The third thread of the tee join 21 is attached to the male tube fitting 14 that is connected by the plastic tubing 15 via the female tube fitting 141 with the female body (DESO) 81. The female body 81 when coupled with the male stem (DESO) 61 of the Snap- Manifold-Snap-Vessel system, 205-100 is ready for purging.

Two of the Snap-Reactor models, F and G (Figures 9 and 10), can be attached both to mono- 206 and to multi-port manifolds (207 and 210). Flexible tubing 15 attaches the manifolds (Figures 12 and 13) assembly to selected Snap-Reactors.

Example of the Snap-Reactor use.

Although the Snap-Reactor can be used to perform many chemical reactions, as an example, steps for carrying out the hydrogenation process are described below. Thus the hydrogenation reaction is carried out in Model-A, for the continuous flow of a reacting gas. The procedure typically involves the following steps (see Figure 2):

1. Loading the glass vessel 1 with a magnetic PTFE coated stir-bar 2, solvent, a substrate(s), and/or a catalyst under an inert atmosphere (if required);

2. Assembling the Snap-Reactor by coupling of the male stem 6 (DESO) with the female body 8 (DESO/SESO);

3. Removing air from loaded components as well as the entire system (purging via overpresurizing);

4. Adding a catalyst or substrate, remove air from the added component (purging);

5. Running the chemical reaction under an overpresurized hydrogen gas (up to

require psig);

6. Sampling (for verifying whether the reaction is completed);

7. Removing excess of the hydrogen gas from the reaction mixture (venting); 8. Dissembling the Snap-Reactor by decoupling the male stem 6 from the female body 8 followed by unscrewing the adapter 4;

9. Filter off the solution from the catalyst, evaporate the solvent, and collect the product.

As mentioned previously, different chemical processes may require employing different Models of the Snap-Reactor while equipped with different the quick-connects fittings: DESO, SESO or FF. Similarly, the Snap-Reactor can be attached permanently or temporarily to a gas line.

Example of permanent attachment of the Snap-Reactor to a gas line for the hydrogenation process.

Quick-Release Connects:

DESO (double-end shutoff). Model A (see Figure 2). The DESO quick-connects coupling, 6 and 8, is used when a sample addition or sampling is planned to be done by unscrewing of the adapter 4. Mostly, it is done both for not very air/moisture sensitive reagents and as well as for solid reagents. This model is particularly useful when the loading of reagents must be performed in a glove-box. However, in some cases chemical components cannot be added in the glove box as halogenated compounds. Model A is also adequate for chemical components that can be added in air or under a stream of an inert gas. Similarly, the sampling is done, first, after the decoupling of the quick-connects 6 and 8, followed by unscrewing the adapter 4.

Assembling the Snap-Reactor: Once the solvent and chemical components are loaded, the glass vessel 1 is fitted with the adapter 4 to which the O-ring 3 and the male stem 6 (DESO) are attached. The Snap-Manifold (Model A) is mounted on top of the Snap-Vessel by snapping the male stem 6 (DESO) with the appropiate female body 8 (DESO). Next, the reaction mixture is agitated with a magnetic stirrer-bar 2.

Air removal: Once the quick-release connects are coupled, 6 with 8, reaction vessel 1 is concurrently vacuumed and pressurized (purged) with an inert gas, or a reacting gas, up to 20 psig. The process of purging is repeated 5 times by over-pressurizing followed by turning off the gas source. Secondary reagents addition (catalyst or/and substrate): Prior to the addition of secondary chemical components, the pressure in the reaction vessel should be equalized by slowly opening of needle valve 16 while disconnecting the vacuum hose 31 to release the inert/reacting gas. The gas can also be released by adding a spare valve in the vacuum system.

Once the pressure in reaction vessel 1 equals the atmospheric pressure, the quick-release connects, 6 and 8, is disconnected by pressing down the snap ring on the female body 8 (DESO). Adapter 4 is unscrewed and a catalyst (substrate), as a solid, or as slurry, or as a solution, is quickly added under a stream of an inert gas (optional). Next, the above process of assembly and purging is repeated. This time the removal of air is shorter, since only air from the added catalyst (or secondary reagents) must be removed. A good indication of the degassing progress is by carefully observing bubbles forming inside reaction vessel 1.

Once the second purging process is complete, the needle valve 16 is turned off, and the pressure of the reacting gas is adjusted to a required value by turning on the knob on the gas supply tank and observing the position of the needle on the pressure gauge 12. Progress of the reaction is monitored by analyzing reaction aliquots, periodically taken from the reaction mixture. Prior to sampling, the reaction vessel 1 is depressurized, as above, the male stem 6 is disconnected from the female body 8, the adapter 4 is unscrewed, and then a sample is taken out. When analysis of aliquots shows that the reaction is complete, the flow of the reacting gas is stopped by turning the gas knob off. Excess of hydrogen is removed from the reaction mixture by slow opening of needle valve 16 while vacuuming. The quick-connects, 6 an 8, are disconnected, the adapter 4 is unscrewed, the catalyst is filtered, the solvent evaporated, and then the product is collected.

Certain chemical reactions while progressing release a gas, for example C0₂ is released during the Sweren oxidation. Thus, an increase in pressure is a good indication of the progress of the reaction. For this purpose, a simplified Snap-Reactor, illustrated in Figure 14, may be employed, having quick-release couplings of a DESO type that are connected directly to the pressure gauge 12 via female body 6 (DESO) and the hex reducing coupling 25.

In general, during purging and during the whole reaction processes, the Snap-Manifold and Snap-Vessel form an inseparable unit. However, for certain models, for example Models A and B (Figures 2 and 4), the Snap-Manifold and the Snap-Vessel can be decoupled, and then the Snap-Vessel again coupled with the Snap-Manifold 211 (Figure 14). The connection is made by the snapping male stem 6 (DESO) with the female body 8 (DESO/SESO) that is further connected directly to pressure gauge 12 via hex reducing coupling 25.

SESO (single-end shutoff). Model Al (Figure 3). SESO quick-connects coupling is used when a sample addition or sampling is planned to be performed without unscrewing of the adapter 4. Once reaction vessel 1 has been loaded with primary reagents and a solvent, the Snap- Vessel 101 and Snap-Manifold 200 are coupled together via quick-release connects 5 (SESO) and 8 (SESO/DESO). Air is removed by the purging process. Next, secondary components, in a form of a liquid, are added with a syringe or via a cannula through an opening in the male stem 5 (SESO) under the stream of an inert gas (optional). Similarly, the sampling is done through an opening in male stem 5 (SESO). Model-Al may also be used for loading secondary reagents as solids, by unscrewing the adaptor 4. This particular model is not suitable if addition of reagents must be done in a glove-box, because of the opening in the male stem 5 (SESO).

FF (full-flow). Model C (Figure 6). Full Flow quick-release connects, 7 and 9, is employed when chemical components (solvent, reagents, or catalysts) are air/moisture sensitive and are not loaded in a glove-box, because this is not allowed or a glove -box is not available. The Snap-Manifold design permits the facile addition of liquid reagents via the septum 18 or septa 24 with no contact to the atmosphere. The addition of reagents as well as sampling is executed via septum/septa (18/ 24) after a 1/4 turn of ball valve 131 while adjusting pressure to the atmosphere.

The Snap-Vessel 102 and Snap-Manifold 202 are coupled together by snapping the FF male stem 7 with the FF female body 9, and then the whole internal system is purged with an inert or a reacting gas. Reagents are delivered by syringe or cannula via the septum 18 or septa 24 under a positive pressure of an inert/reacting gas stream. During the delivery operation the purging system can be vented by a slight opening of the needle valve 16 or via the needle being introduced into rubber septum 18 or septa 24.

Manual operations during the addition of chemical components as well as air removal for Model C (Figure 6) are as follows: once Phase I, e.g., loading of a solvent and a substrate followed by purging, has been done, Phase II, the introduction of secondary reagent(s), thorough septum 18 or septa 24 and protecting ball valve 13 is executed. Therefore, prior to the addition of secondary reagents the flow of the reacting (purging) gas should be ceased by turning off the ball valve 131. The pressure inside of reaction vessel 1 should be equalized by slowly opening of the needle valve 16. When the pressure has been equalized, needle valve 16 should be turned off. Next, ball valve 13 at the top, directly attached to the union cross, should be turned by a 1/4 turn. Next, a syringe with a long needle or a cannula is inserted via the septum 18 or septa 24 until the needle's (cannula) ending is seen in the reaction vessel, and then a secondary liquid reagent is added. After the addition of reagents, the needle (cannula) is removed; the top ball valve 13 is turned off, followed by opening of the ball valve 131 in the gas line. Optionally, the addition of a secondary reagent can also be done under a slightly positive pressure of an inert gas either by slightly opening the needle valve 16 or by inserting an additional needle into the septum 18 or septa 24 to create an opening (vent) into the atmosphere.

Example of temporary attachment of the Snap-Reactor to a gas line via n-port manifolds.

So far the Snap-Reactor systems were described that are permanently attached to a gas line while conducting chemical reactions. Other options include the portable Snap-Reactor represented by models D-G illustrated in Figures 7, 8, 9, 10, 11, and 12. The Snap-Manifolds of these models have an additional male stem 61 (DESO) of the quick-release connects screwed to the central union cross 10 (Figures 7 and 8) or the branch tee join 21 (Figure 10). Further, male stem 61 (DESO) is coupled to a female body 81 (DESO/SESO) that is permanently attached, either directly or indirectly, through a mono-port 206 (Figure 11) or a multi-port manifold 207 (Figure 12), to a gas/vacuum line. Since, in both cases (Figures 10 and 11), the gas lines have their own valve regulation system, configurations of some Snap-Manifolds 205 are simpler e.g., they do not have valves. Portable Snap-Reactors are represented by Models D and E (Figures 7 and 8), as well as by Models F and G (Figures 9 and 10). Their Snap-Manifolds are specially designed.

The Snap-Manifolds of Models D and E (Figures 7 and 8) resemble those of Models A and Al (Figures 2 and 3). In Models D and E, unlike in Models A and Al, the union cross 10 and female tube fitting 141 are bridged by the quick-release connects 61and 81 (DESO). There is no direct connection between the union cross 10 and female tube fitting 141, as in Models A and Al (Figures 2 and 3).

A second portable Snap-Reactor, Model F (Figure 9), is designed to allow chemical components to be introduced into the reaction vessel 1 through a septum 18 or septa 24. Thus the Snap-Manifold 204 of Model F (Figure 9) comprises of a four- way union cross 10 that has three 1/8" female threads for connecting to a ball valve 131, capped with the septum 18 or septa 24, to the male stem of the quick-connects 61 (DESO) for connecting to the female body 81 (DESO), and also to the female body 9 quick-connects (FF) for connecting to the male stem 7 of the Snap-Vessel 102. The fourth thread is a 1/8" NPT of the reducing female elbow 20 adapted to a 1/4" NPT for connecting to the 0-60 psi, 2.5" diameter pressure gauge 12. In Model F, the Snap-Manifold 204 is directly attached either to the gas source via plastic tubing 15 (Figure 9) or to a mono-port-manifold 206 (Fig 11) or to a multi-port manifold 207 or 210 (Figures 12 or 13)

A third portable Snap-Reactor is illustrated by Model G (Figure 10). It can be attached to n-port-manifolds, 206, 207, or 211 (Figures 11, 12 or 13). The Snap-Manifold 205 of Model G (Figure 10) consists of a female three-way branch tee join 21 that has two 1/8" female threads for connecting to a male stem 61 (DESO) that is connected to a female body 81 (DESO/SESO) that is further attached to the gas line via female tube fitting 141 and then plastic tubing 15. It also can be connected to n— port manifolds 206, 207, or 211 (Figures 11, 12, or 13). The third thread is a 1/8" NPT (11) adapted to a 1/4" NPT for connecting to the 0-60 psi, 2.5" diameter pressure gauge 12. The female body 8 (DESO/SESO) is connected to the male stem quick-connects 6 (DESO) that, in turn, is joined to the adapter 4. n-Port-Manifolds .

The mono-port manifold 206 (Figure 11, panel d) consists of a female branch tee 21 that has three 1/8" female threads for connecting to a needle valve 16, a ball (needle) valve 13, and the male tube fitting 14. The needle valve 16 is further connected to a vacuum system via the female hose connector 17 and the hose 31. On the other hand, the ball valve 13 is connected to the female tube fitting 141 and further directly to a gas line via plastic tubing 15. Finally the male tube fitting is connected with the female body 81 that in turn can be coupled with the male stem 61 of the Snap-Manifold 205.

Examples of multi-port manifolds, 2-port- 207 and 3-por-t 210, are illustrated in Figures 12 and 13. The n-port manifolds consist of two parallel lines of the stainless steel tubes 19 that are separated, as well as connected, by a set of ports. For example, the 3 -port manifold 210 (Figure 13) has three sets of ports: Port 1, Port 2 and Port 3. Port 1 comprises: (i) a female elbow 30; (ii) a needle valve 16; (iii) a female branch tee 21; (iv) a ball valve 13; (v) a pressure regulator 29; and (vi) a pressure relief valve 22. Port 2 comprises the same parts as port 1, however, the female elbow 30 is substituted with the female branch tee 2. Port 3 has the same parts as port 2 and, additionally, it is equipped with a tube fitting reducing union 27, for connecting to a gas line, and a tube hose connector 33 for connecting to a vacuum line via the hose 31.

Models F and G (Figures 9 and 10) can be attached to the female branch tee 21 of the n-port-manifolds 206 (Figure 11), 207 (Figure 12) or 211 (Figure 13) via coupling with the female body 81 that in turn is connected to the male tube fitting via the flexible plastic tubing 15.

Another Model-H is illustrated in Figure 14. Model-H is employed either to monitor a consumed or released gas during chemical reactions. In general, the Snap-Manifold 200 and the Snap-Vessel 100 form inseparable unit both during purging and during reaction processes. However, for selected DESO models, A and B, assuming that the reaction vessel has been overpressurized with a reacting gas, the Snap-Manifold 200 can be decoupled from the Snap- Vessel 100 and consequently substituted by a unit 211 (Figure 14). The unit 211 consists of a female body of quick-connects (8, DESO) and the pressure gauge 12 that are connected via the hex reducing coupling 25. A connection of the unit 211 with the Snap Vessel 100 is made by snapping the male stem 6 with the female body 8. This model would be useful in the teaching industries to monitor progress of a hydrogenation reaction by observing the gradual decrease of pressure on the pressure gauge 12.

Model-AR, illustrated in Figure 15, is an example of the Snap-Reactor (103 and 212) having a pressure relief valve 34. This valve protects from exploding of the glass vessel 1, when a reaction is conducted at higher temperatures or the thickness of the wall of the glass vessels used is smaller than 9 mm. Additionally, for larger volumes, e.g. 4, 000 mL, the bottom part of the Snap-Vessel 103 is rounded.

Extensions of Snap-Reactor models disclosed herein may include additional elements that can be mounted into the adapter. These elements may comprise: (i) a thermocouple to monitor the temperature in the reaction mixture; (ii) a septa that allows adding reagents or doing sampling; or (iii) a suspended magnetic stirrer.

Additionally, a simplified model of the Snap-Reactor can be employed for the Parr apparatus. This simplified Snap-Reactor has a glass vessel and an adapter. To the adapter is screwed the male stem (DESO) that can be coupled with a female body. The uncoupled end of the female body is directly connected with a hydrogen source via flexible PFE tubing. Advantage of this Snap-Parr hybrid is that when the hydrogenation reaction is complete and the reaction vessel is disconnected, work-up does not to be performed immediately, since the contents of the reaction are not directly exposed to the air atmosphere. Additionally, it also insures tight sealing and eliminates a rubber cork, traditionally used, in the Parr apparatus.

A simplified Model-H, illustrated in Figure 14, allows for monitoring the progress of chemical reactions during which any gas is released according to the nature of a particular reaction as well as is consumed as for hydro genations.

All fittings in the Snap-Reactor implementations described so far are piping systems. For improved adjustment of the alignment of parts like valve, pressure gauge, elbows, and tees, a male or female adapter fittings or a valve with integrated tube fittings or port connectors can be used.

A modified system is disclosed below based on tube fitting connections via port connectors for connecting all metal parts. The tube fitting connector is a sequential phase, controlled action and gripping device, consisting of a nut, back ferule, front ferule, and body. The tube fitting connector accepts tubing as well as port connectors. The port connectors are used: (i) to reduce space between parts being connected; (ii) eliminate cutting short lengths of tubing; (iii) to allow close coupling with pre-determined lengths; (iv) to eliminate pipe threads in the system; (v) to effect a union at every joint to permit complete disassembly for removal from the system.

For example, when installing valves, there is usually a preferred location for the valve handle. If the valve is connected to a piece of equipment, it is often desirable to have the valve handle as illustrated in Figure 16. If the connection on the equipment is a male or a female pipe thread, alignment may be extremely difficult, if not impossible. To save time, prevent leakage, and prevent valve damage during installation, it is advisable to use a valve with integral tube fittings. Moreover, if it is desired to shift the direction of the valve handle, the nut of the connection can be loosened, the valve can be moved and held at the desired location and the nuts retighten. Thus, alignments of all valves, pressure gauge, and other appropriate parts can be controlled by using tube fitting connections. In particular, port connectors are useful since they have small size and make the Snap-Manifold more compact.

Figure 16 shows an example of tube fitting connections, employing port connectors, for one of the models, Model-B2. The Snap-Manifold of Model-B2 consists of following parts: (i) a reducing adapter 100; (ii) a plug valve with two tube fittings on both ends 101; (iii) four port connectors 102; (iv) a needle valve with two tube fittings on both sides 103; (v) a hose adapter with the groove 104; (vi) a needle valve with two tube fittings on both sides 105; (vii) a union tee with three tube fittings at its ends 106; (viii) a union cross with four tube fittings on the four ends 107; (ix) a reducing port connector, from 1/4 to 1/8, 108; (x) QC regulator body ended with tube fitting (DESO/SESO) 109; (xi) a pressure gauge with grooved tubing 110.

The union cross 107 has four tube fittings, one of which is directly connected to a pressure gauge via a tube adapter. The remaining three are connected to a plug valve 101, a union tee 106, and a female body 106 via three port connectors. The plug valve 101 is further connected to a reducing adapter having a tube fitting on one of its end that if further connected to a gas tank via a PTFE tubing 15.

The union tee 106 is further connected to two needle valves, a vacuum valve 103 and a gas relief valve 105, via port connectors 102. The vacuum valve 103 is further connected to a hose adapter 104 and then via a hose to a vacuum pump. Similarly, tube fittings and port connectors are included, if required, into the mono-port manifold, the multi-port manifold, and other types of Snap-Manifolds described earlier. The arrangements of valves, the pressure gauge, the tee, and the union cross are shown for illustrative purposes only and are subject to change within the spirit of the disclosure.

Advantages of utilizing tube fittings with and without port connectors come from: (i) controlled alignment of required parts as valves, elbows, pressure gauges, tees, crosses without regard to pipe thread tightness; (ii) no PTFE type required for sealing the system; (iii) no pipe threads in the system; (iv) connections and disconnections and retightened can be done many times; (v) leak-proof can be obtained every time the connection is made; (vi) machined from bar stock for rigidity and strength. Tube fittings with the port connectors offer the following advantages: (1) are short in length to make a system compact; (2) are standardized in sizes; (3) as above.

Under laboratory conditions it may be desirable, for safety or other purposes, to protect certain portions of a manifold connected to the vessel. Such protection can be achieved by utilizing a removable cover made from a chemically resistant material. Examples of such removable covers are shown in Figures 17 and 18. Figure 17 shows an example of a round shaped protective cover 93, and Figure 18 shows an example of a rectangular shaped protective cover 95.

Following are some of the advantages of the Snap-Reactor of the present teachings: — Inexpensive and more accessible;

— Instant, easy, connections/disconnections of the Snap-Manifold with Snap- Vessel via quick-connects-release fittings (DESO, SESO, and FF);

— Visual observation of reaction mixture;

— Portable reactor, while employing a suitable configuration of modular components;

— Flexible plastic connections with gas and vacuum lines;

— Hand-tightening, by snapping, no tools required to assemble/dissemble the reactor;

— Variable operating volumes of glass vessels, while having the same adapter size (50 mL- 4 L);

— Temperature range from about -20 to about 100 °C;

— Easy to maintain;

— Pressure monitored;

— Optional reaction temperature monitoring;

— Optional sampling through a septa located in the adapter;

— Tightly isolated, no leaks;

— Easy delivery of reagents (liquid or slurry or solid) by accommodation of selected quick- connects fittings (DESO or SESO or FF);

— Suitable for a variety of gasses (argon, nitrogen, ammonia, hydrogen deuterium, carbon monoxide, carbon dioxide, ethylene, butane and others);

— Does not require balloons or needles;

— Steady gas delivery under constant pressure;

— Overpressure and conduct of reaction in an individual hood;

— Reactions are performed at atmospheric pressure as well as up to 100 psig;

— A pressure a relief valve protects the glass vessels from exploding;

— Adapted to multi-port external manifolds for parallel reactions; Modular components use for construction of the Snap-Manifold and the Snap-Vessel e.g., in LEGO-like fashion;

Simple purging systems;

The unisized adapter (one adapter size matches bottles of different volumes);

The Female body of DESO and FF quick-connects of the Snap-Manifold may also be utilized to different adapter sizes e.g., the same Snap-Manifold can be used for different sizes of adapters;

Mixing reaction mixture is by a magnetic stir-bar or a suspended magnetic stirrer;

Allows to fill a glass vessel, with a solution, more that 1/3 of the total volume, since there is no shaking as in the Parr apparatus;

Employed in chemical industries as well as in research and teaching institutions;

Appropriately assembled can be adapted to the Parr apparatus;

Although the invention has been described with respect to various embodiments, it should be realized that this invention is also capable of a wide variety of further and other embodiments within the spirit of the invention.

Table 1. Different types of Snap-Manifold and Snap-Vessel: number of individual parts in the model.

Examples Snap-Manifold: Models A-G (number of parts)

A A1 B B1 C D E F G

Part#

Fig-2 Fig3 Fig4 Fig-5 Fig-6 Fig-7 Fig-8 Fig-9

Union cross 10 1 1 1 1 1 1 1 1

Female body 8 1 1 1 1 - 2 2 1

(DESO/SESO)

Needle valve 16 1 1 1 1 1 1 1 -

Hose connector 17 1 1 1 1 1 1 1 -

Reductor to 1 1 1 1 1 1 1

pressure gauge 11

Pressure gauge 12 1 1 1 1 1 1 1 1

Tubing fittings 15 1 1 1 1 1 1 1 1

Ball valve 13 1 1 2 - - 1

Male stem 6 - 1 1 1

Female tee 21 - 1 - - -

Female body (FF) 9 1 1 1

Septum 18 - 1 - - 1

Expander 25 - 1 - - -

Elbow 20 1

Male stem (SESO, 5)

Male stem (DESO, 6)

Male stem (FF, 7)

PTFE adapter + O-ring

Glass vessel 1 Mono-Port Manifold (number of parts, Figure 12)

Ball valve 13 1

Needle valve 16 1

Female branch tee 21 1

Female Tube fitting 2

141

Male tube fitting 34 1

Hose male connector 1

17

Plastic tubing 15 1

Thus, in certain aspects the present disclosure provides for a chemical reactor which employs a quick-connects-release couplings, DESO, SESO or FF, comprising a male stem, or a female body, that are directly screwed into unisized adapters. The female body of the DESO and FF of quick-connects, as a part of the Snap-Manifolds, can be utilized not only to uni-sized adapter, but also with other sized adapters, smaller or bigger than standard with a 25/25 thread. Quick-connects, either DESO or SESO or FF, is not only used for instant (quick) and easy connections or disconnections, but, in particular, are used for different modes of delivery chemical components as well for sampling.

In certain aspects, The chemical reactor of the present teachings have the quick-connects couplings that can be raptdly connected and then disconnected. In particular, one part of the quick-connects couplings, a male stem, is screwed directly into the unisized {or even not unisized) adapter, which has an O-ring that in turn tightly seals the glass vessel 1 of the Snap- Vessels. The second part of the quick-connects couplings, a female body, is screwed into a modular Snap-Manifold that is a part of a purging, or purging-delivery system.

When both parts of the quick-connects couplings, a male stem and a female body, are connected, it couples a Snap-Vessel with a Snap-Manifold and allows for: (i) the removal of air and moisture from the reaction vessel 1, (ii) the filling of the reaction vessel 1 with an inert or reacting gas; (iii) the direct introduction of chemical components into the reaction vessel 1, via a septum 18 or septa 24, without decupling the quick-connects couplings (as for a FF type). When both parts of the quick-connects couplings are disconnected, the Snap-Reactor permits: (i) the addition of air sensitive reagents, in a glove box or under a stream of an inert gas, by unscrewing the adapter 4 (DESO); (ii) the further addition of solid reagents which are not air sensitive by unscrewing the adapter 4 with incorporated a male stem (DESO or SESO); (iii) the addition of liquid reagents, by syringe, via an opening in a male stem (SESO) under stream of an inert gas.

When both parts of the quick-connects couplings are of the FF type, the Snap-Reactor permits liquid chemical components to be added by syringe or cannula through a septum 18 or septa 24.

In general, the Snap-Reactor may operate when permanently attached to a gas line to perform a reaction under a steady pressure or as a detachable (portable) unit. When it is configurated as a portable unit, the Snap-Reactor is temporary attached to the purging line, to remove oxygen both from chemical components and from the reaction system. After disconnecting from the line, the chemical reaction is then continued in a desired place of the laboratory. Progress of the reaction is monitored by observing the gradual decrease of pressure on the pressure gauge 12. When more of the reacting gas is required the Snap-Reactor can be reattached to the purging system and then loaded with the gas. Purging is performed with a gas (inert or reacting) by over-pressurizing the Snap-Reactor to 20-30 psig or higher.

The FF quick-connects fittings can be used to incorporate a mechanical stirrer.

The neck of the glass vessel is internally threaded to which a treaded adapter together with the incorporated male stem of the quick-connects fittings are screwed. Gases are delivered via flexible PTFE tubing or others plastic tubing. All metal modular parts are made of brass or stainless steel (resistant to acids, bases, and other chemicals). The direct attachment of a male stem or a female body, of the quick-connects couplings, to the adapter 4 can be vertical or horizontal. Snap-Manifolds equipped with a female body quick-connects (DESO and FF) can be employed for differently sized adapters while having the relevant a male stem of quick-connect couplings (DESO, SESO, or FF). The Snap-Parr hydrid can be assembled.

Further, all metal parts, of all types of Snap-Manifolds, as well mono-port- and multi- port-manifolds can be connected, if required, via pipe fittings with or without male or female adapter, via tube fittings using tubing, and/or via tube fittings using port connectors, while all quick-connects utilizing as seals different elastomer O-rings or not utilizing such elastomer O- rings.

EQUIVALENTS

Those skilled in the art will recognize, or be able to ascertain using no more than routine experimentation, many equivalents to the specific embodiments of the invention described herein. Such equivalents are intended to be encompassed by the following claims.

Claims

CLAIMS at is claimed is:

A quick-assembly chemical reactor, comprising:

a vessel in which a chemical reaction may proceed;

a coupling configured for rapidly connecting a manifold to said vessel, said coupling comprising a male stem and a female body, wherein said male stem is configured for removable attachment to said vessel with an airtight adapter and said female body is configured for attachment to said manifold; and

wherein said chemical reactor when assembled is capable of supporting said chemical reaction under pressure.

The chemical reactor of claim 1 , wherein said coupling is selected from a group comprising a single-end shut-off (SESO) quick-release coupling, a double-end shut-off (DESO) quick- release coupling, and a full-flow quick-release coupling.

The chemical reactor of claim 1, wherein said vessel is comprised of glass.

The chemical reactor of claim 1 , wherein said reactor is a portable reactor.

The chemical reactor of claim 1 , further comprising an O-ring, and wherein said glass vessel comprises an internally threaded neck with a groove for accepting said O-ring, said male stem is externally threaded, and said adapter is externally threaded for connecting with said threaded neck and internally threaded for connecting said male stem.

The chemical reactor of claim 1 , further comprising said manifold.

The chemical reactor of claim 6, wherein said manifold comprises a component selected from a group comprising a union cross, a branch tee, and a hex reducing coupling.

The chemical reactor of claim 7, further comprising a removable protective cover configured to encompass at least a portion of said manifold.

9. The chemical reactor of claim 1, wherein said pressure is about 100 psig.

10. The chemical reactor of claim 1, wherein said chemical reaction comprises a hydrogenation process.

11. A method for performing a chemical reaction, comprising the steps of:

selecting a quick-assembly chemical reactor, comprising a vessel in which a chemical reaction may proceed, a coupling configured for rapidly connecting a manifold to said vessel, said coupling comprising a male stem and a female body, wherein said male stem is configured for removable attachment to said vessel with an airtight adapter and said female body is configured for attachment to said manifold, and wherein said chemical reactor when assembled is capable of supporting said chemical reaction under pressure;

loading said vessel with a solvent;

loading said vessel with a substrate;

assembling the chemical reactor by coupling said male stem with said airtight adapter to said vessel and said male stem to said female body;

removing air from said chemical reactor;

allowing the chemical reaction to proceed under an overpresurized hydrogen gas;

removing excess of the hydrogen gas from the reaction mixture;

dissembling said chemical reactor by decoupling said male stem from said female body removing said airtight adapter from said vessel; and

collecting a product of said chemical reaction. 12. The method of claim 11, further comprising loading said vessel with a magnetic PTFE coated stir-bar.

13. The method of claim 11, further comprising the step of loading said vessel with a catalyst or another substrate.

14. The method of claim 11, further comprising the step of sampling to verify for completion of said chemical reaction.

5. The method of claim 12, wherein said coupling is of a DESO quick-connect type, and said removing air is performed by evacuating the reactor while stirring said stir-bar followed by filling the reactor with an inert gas.