DESC:-: Complete Specification :-

METHOD, AND SYSTEM IMPLEMENTING SAID METHOD, FOR SYNTHESIS OF SODIUM TERT-BUTOXIDE

Cross references to related applications: This complete specification is filed further to application for patent No. 201921039855 filed on 02/10/2019 with provisional specification, the contents of which are incorporated herein in their entirety, by reference.

Field of the invention
This invention belongs to the field of green chemistry, and relates therein to an inventive method and assembly for implementing said method, to thereby synthesize a non-nucleophilic base, sodium tert-butoxide in particular.

Background of the invention and description of related art
Sodium tert-butoxide (sodium butylate) is a safe and effective alternative to sodium hydride, and finds use as a powerful deprotonating agent for many organic reactions as well as a desiccant or drying agent for laboratory chemicals. Considering such a wide applicability, the industrial demand for sodium tert-butoxide is high the world over, which exerts sizeable demand on its efficient bulk production and supply.

Conventionally, sodium tert-butoxide is prepared by refluxing sodium metal pieces with tertiary butanol. Alternatively, production of sodium tert-butoxide is undertaken via methods employing sodium hydride or sodium amide. Another conventional method for production of sodium tert-butoxide involves atomizing molten sodium in tert-butanol containing 5-15% of hydrocarbon solvent as softening agent.

However, those skilled in the art shall immediately realize that the aforementioned conventional methods for the production of sodium tert-butoxide are inundated with issues which persist today as unaddressed technical problems, including-
1) Very slow reaction rate;
2) High reflux time (about 24 to 48 hours) required for the complete conversion of sodium into sodium tert-butoxide;
3) Need for constant heating and monitoring the reflux assembly;
4) Hazard due to that hydrogen gas was accumulated;
5) Formation of hard lumps of sodium tert-butoxide, which necessitated it being broken into small pieces under nitrogen atmosphere for retrieval from the reaction vessel;
6) Risk of serious health hazards like eye, nasal and throat irritation when exposed to the synthesized sodium tert-butoxide powder (exposure during the powdering process);
7) Low quality of end-product because of its susceptibility to atmospheric moisture; and
8) Un-reacted pieces of active sodium remaining entrapped in final product, which is a serious fire hazard.
9) High electrical consumption to sustain heating and stirring

While there were many art references researched by the inventor(s) in ensuring that the present invention is novel, the following art was identified as more closely related to the present invention, and thus worthwhile to discuss in more detail in context of the present invention.

For example, US3479381 (assigned to Atlantic Richfield Co) teaches a method for preparation and preservation of metal alkoxides, in which Zeolite material (molecular sieves) is used to remove water from the alcoholic solution. Zeolite sieves are used as dehydrant / desiccant. However this process is not an ideal solution, since the Zeolite molecular sieves need heating prior to use. Another reference, US5276219 (assigned to FMC Corp) teaches a process for preparation of lithium tertiary alkoxides by the reaction of lithium metal with a tertiary alkyl alcohol in a polar reaction solvent solvent. The method involves reacting dispersion of lithium metal (particle size less than 300 microns) in a polar reaction solvent at a temperature between 50oC and the boiling point of the solvent under inert atmosphere – however, which is still not an ideal proposition because it is limited in necessarily having to react a dispersion of lithium, needs polar cosolvent, and involves extrinsic heating.

Yet another reference, EP0721445B1 (assigned to FMC Corp) teaches a process for preparing lithium tertiary alkoxides by reacting lithium metal in gross or bulk form with a tertiary alcohol. Here, lithium metal cubes are reacted with t-BuOH, and stirred mechanically, refluxed. Tetrahydrofuran is used as solvent. However, this process is squarely dependent on involvement of stirring, heating and THF as cosolvent. Another reference, CN201010510514 (filed by Wang Yuqin) discloses a method for production of granular sodium tert-butoxide by reacting t-BuOH and sodium in inert organic solvent under nitrogen, heating/reflux for 8-40 hours, with constant stirring. This method falls short of ideal, as it needs cosolvent, heating for a long time of 8-40 hours and stirring.

Prior art contains other references to process for preparing sodium tert-butoxide, such as those referred in CN106699516, JPH05170680, WO9509141, CN102001914, CA1199035A, US1712830, US1816843, US1910331, US3418383, US4327230, and US4577045, however none of these is able to overcome the encumbrances voiced hereinabove.

Prior art thus, to the limited extent presently surveyed, does not list a single effective solution embracing all considerations mentioned hereinabove, thus preserving an acute necessity-to-invent for the present inventor.Improvised methods and energy efficient systems which characteristically avoid the aforementioned issues, are hence a sore need in the art -this niche has been the locus of research undertaken by the inventor named herein who therefore as result of his focused research, has come up with a novel solution for resolving all needs of the art once and for all.

It shall be emphasized herein, that work of the inventor named herein, specifically directed against the technical problems recited hereinabove and currently part of the public domain including earlier filed patent applications, is neither expressly nor impliedly admitted as prior art against the present disclosures.

A better understanding of underlying principles of the present invention will be obtained from the narration to follow which sets forth an illustrative yet-preferred embodiment.

Objectives of the present invention
The present invention is identified in addressing at least all major deficiencies of art discussed in the foregoing section by effectively addressing the objectives stated under, of which-

It is a primary objective to provide a safe, easy and rapid method for production of sodium tert-butoxide, and a simplified yet efficient system assembly for implementation of said method.
It is another objective besides to the aforesaid objective(s) that the method for production of sodium tert-butoxide so provided has a highreaction rate, and minimalreflux time.

It is another objective besides to the aforesaid objective(s) that the method for production of sodium tert-butoxide so provided does not need constant heating and monitoring the reflux assembly.

It is another objective besides to the aforesaid objective(s) that the method for production of sodium tert-butoxide so provided does not lead to accumulation of hydrogen gas, and allied hazards of such accumulation.

It is another objective besides to the aforesaid objective(s) that the method for production of sodium tert-butoxide so provided results in powder form of sodium tert-butoxide, which is convenient for retrieval from the reaction vessel, as well as avoids user irritation while pulverization otherwise required in conventional processes.

It is another objective besides to the aforesaid objective(s) that the method for production of sodium tert-butoxide so provided leaves no un-reacted pieces of active sodium remaining entrapped in final product.

It is another objective besides to the aforesaid objective(s) that the method for production of sodium tert-butoxide so provided results in an end-product which has minimal susceptibility to atmospheric moisture.

It is another objective further to the aforesaid objective(s) that implementation of the present invention does not incur any undue costs and/ or technical complexities.

It is another objective further to the aforesaid objective(s) that implementation of the present invention to reduce the electrical consumption.

The manner in which the above objectives are achieved, together with other objects and advantages which will become subsequently apparent, reside in the detailed description set forth below in reference to the accompanying drawings and furthermore specifically outlined in the independent claim 1. Other advantageous embodiments of the invention are specified in the dependent claims.
Attention of the reader is now requested to the narration to follow which elaborates a preferred embodiment of the present invention and such other ways in which principles of the invention may be employed without parting from the essence of the invention claimed herein.

Statement / Summary of the present invention
The present invention is identified in provisioning asafe, easy and rapid method for production of sodium tert-butoxide by reactingtert-butanol with sodium and an assembly for implementing said method. The assembly comprises a thermal insulation module (01), a reaction vessel (02) and an alcohol exchanger pocket with reversible two-chambered mineral oil bubbler (03). Implementation of said method using said assembly is characterised in having a highreaction rate, minimal reflux time, no need of heating and monitoring the reflux assembly, avoids accumulation of hydrogen gas and importantly, results in powder form of sodium tert-butoxide as an easy-to-recover end product. The sodium tert-butoxide so prepared has no un-reacted pieces of active sodium remaining entrapped therein, and hence minimal susceptibility to atmospheric moisture.

Brief description of drawings
The present invention is explained herein under with reference to the following drawings, in which:

Figure 1 is a schematic illustration of a first embodiment of the glassware assembly as per the present invention.

Figure 2 is a schematic illustration of a second embodiment of the glassware assembly as per the present invention.

Figure 3 is a graph illustrating Temperature variation noted in thermally insulated and non-insulated systems as per the disclosures hereof.

Figure 4 is a graph illustrating Complete temperature variation during the reactions as per the disclosures hereof.

Figure 5 is a microphotograph of the loose mass of crystalline t-BuONa synthesized as per the disclosures hereof.
The above drawings are illustrative of particular examples of the present invention but are not intended to limit the scope thereof. The drawings are not to scale (unless so stated) and are intended for use solely in conjunction with their explanations in the following detailed description. In above drawings, wherever possible, the same references and symbols have been used throughout to refer to the same or similar parts. Though numbering has been introduced to demarcate reference to specific components in relation to such references being made in different sections of this specification, all components are not shown or numbered in each drawing to avoid obscuring the invention proposed.

Detailed description
Principally, general purpose of the present invention is to assess disabilities and shortcomings inherent to known systems comprising state of the art and develop new systems incorporating all available advantages of known art and none of its disadvantages.

Accordingly in a first aspect, the disclosures herein are directed towardsthe construction, assembly, and operations of a highly cost effective, compact, portable, easy to fabricate and convenient to use glassware setup for preparation of sodium tert-butoxide. And in natural progression thereof, the disclosures herein are directed towardsa related second aspect, being the establishment of a safe, easy and rapid method for the preparation of sodium tert-butoxide using the assembly so proposed, which is understood from the underlying illustrative examples.

Materials-
Tert-butanol was purchased from Merck India and was dried by refluxing with sodium wire under nitrogen atmosphere. The dried alcohol on complete dissolution of sodium was added fresh sodium wire and was distilled under nitrogen atmosphere. The sodium metal was purchased from Spectrochem India and was purified by melting it under mineral oil followed by washing the surface with petroleum ether and was extruded into 1mm thick wire using a screw sodium press. The ground glass joints were applied with Teflon ribbon coat to avoid locking of joints. No joints were secured with joint clips.

Agilent DMM, U1253B, with a U1181A immersion K-type temperature probe was used for automated data logging with an interval of 5 seconds. Agilent GUI 1.7.1.0 software was used to access and record the data. An external power supply of 9V DC was fed to the multimeter to sustain performance till completion of the experiment. Keysight Handheld Multimeter Logger Software 3.1.51130.01 was used to capture data and graphs were plotted in Origin.

Assembly and its construction-
As seen in the accompanying Figure 1, the glassware assembly of the present invention is seen to comprise three basic structures –thermal insulation module (01), a reaction vessel (02) and an alcohol exchanger pocket with reversible mineral oil bubbler (03). A round-bottom flaskserved as the reaction vessel (02). The central column was custom-fabricated, keeping depth of flask as main consideration.

As per a related aspect hereof, the thermal insulation module (01)is made from a protective Styrofoam packaging that comes with 2.5 litres chemical glass bottles (any other suitable packaging or packaging custom-made for the reaction vessel to be contained therewithin may be used as well without departing from the essence hereof). Its length was trimmed as per the height of the flask (02) and a hole of an appropriate size was made in the lid to accommodate the neck of said flask (02).

Thermal insulation of the system was found to play an important role in conserving the heat of the reaction and propelling it towards completion. This was well established by two separate experiments. Figure 3 shows the temperature variations in an insulated and a non-insulated systems. The table 1 given below shows the extract of graph of Figure 3.
T Max (oC) tT Max tc
(29.1oC)
With Insulator 78.5oC 0.89167 Hrs
(53.50 Min) 4.88889 Hrs
(293.33 min)
Without Insulator 76.1oC 0.91111 Hrs
(54.66 Min) 4.46944 Hrs
(268.16 min)

Higher temperature was recorded in experiments in which an extra quantity of the t-BuOH was used.
Table 1
Wherein,
*These experiment were done when room temp was (28.4oC)
T Max = Peak temperature attained by the system
tT Max = time required to attain peak temperature
tc= Time required for cooling down of system to 29.1oC

Table-1 also revealed that the time required for cooling in an insulated reaction was more than the non-insulated system. A non-insulated assembly cooled faster by 25 minutes. A small change in procedure was introduced to address the issue. The assembly was kept in insulation till it attains the T-Max and the insulation jacket was removed afterwards. This helped rapid cooling of the system, however, the system can be insulated during entire course of reaction if time is not a constraint.

Thus it was well established that the insulation plays role by elevating the peak temperature. It had a negligible effect on reduction of time required to attain peak temperature. Peak temperature in a thermally insulated system was found higher by 2.4oC than the non-insulated system. Hence the reaction conditions in a thermally insulated system were more vigorous than a non-insulated system

As per another related aspect hereof, a reversible two chamber mineral oil bubbler (03) was employed which principally isolated the outside environment from inner reaction and avoids hazards arising through accumulation of hydrogen gas as the assembly keeps on releasing the hydrogen gas in very small volumes over the reaction time. Said exchanger pocket –bubbler (03) is specially fabricated, being a slender assembly made up of two concentric tubes (04 and 05) which extend towards bottom of the flask (02) keeping a distance of approximate 2.5cm from the inner surface. Inner tube (05) serves as a thermometer pocket (06) in which a digital probe thermometer (07) (can be replaced with a long stem digital thermometer as well in routine experimentation. Also, thermometer is not needed for production run) is inserted for temperature readouts. Mineral oil (1ml) was added to the thermometer pocket (06) in order to establish good thermal contact with the digital probe thermometer (07).

As per another related aspect hereof explained with continued reference to the accompanying Figure 1, the space (08) around the thermometer pocket (06) is initially empty but is subsequently filled with tert-butanol due to internal and simultaneous distillation, as the system attains peak temperature. Significant amount of the alcohol (22 to 25 ml) is automatically distilled off and was stored in this pocket (08). This distilled alcohol afterwards keeps reversibly exchanging the vapours in the flask (02).

As per another related aspect hereof explained with continued reference to the accompanying Figure 1, hydrogen gas generated inside the flask (02) made its way to outside environment through tiny pores (09 and 10) in the reversible mineral oil bubbler. A B14 inner glass joint (11) with a rubber septum (12) is provided to serve as a facility to inject more alcohol in case the same is required. Oil from the 1st pocket (3a)of bubbler migrates to 2nd(3b) under the action of hydrogen gas pressure and the gas is released in form of small bubbles. For additional safety, a flexible silicone tube (13) attached to the mineral oil bubbler can be placed in vicinity of a fume extractor (not shown in this drawing) so that the hydrogen gas released is disposed safely (Or the released gas can be used for some industrial process / manufacture).This feature keeps the system under a small positive pressure of H2 and avoids any hazards arising through its accumulation.

The system cools on completion of the reaction and the mineral oil returns to pocket(3a)under the action of vacuum generated inside the system while cooling. This moment along with the temperature readout can be taken as an indication of completion of the reaction and the assembly can be thereafter safely and easily dismantled for further processing / storage. Rate of the reaction can be approximated by observing the rate of H2 evolution. The reaction can be dismantled when bubbling in oil bubbler stops. The assembly can be left in the insulation during whole experiment if time is not a concern (taking it out of insulation helps rapid cooling).

Implementation of the present invention using the glassware (or any other inert material) assembly described above is explained now, with reference to an experimental protocol outlined in the disclosures to follow.

Protocol for implementation-
Wired sodium metal (23g, 1 atom equivalent approximately) was taken in flask (02), which was then placed in the insulating module (01). Lid of the module (01) was then closed. Tert-butanol 140g (1.89 moles, 180ml) was then added to the flask (02) and the exchanger pocket – bubbler (03) was then inserted into the flask. Thermometer pocket (06) was then filled with mineral oil and a K-type thermocouple (07) (any other thermocouple may also be used as well without departing from the essence hereof) was then inserted into the pocket (06). This thermocouple (07) was then connected to the Digital multimeter which was interfaced with a computer for data logging purposes.

The whole assembly was then left undisturbed till it attains the peak temperature. The insulation was then removed for rapid cooling. Time required to attain peak temperature was around 55-60 minutes. During this time, inner sodium and the alcohol was converted into a soft solid(as shown in the accompanying Figure 5). Inner alcohol exchanger pocket was then removed and the distilled alcohol was recovered. The flask was then attached to a rotary evaporator and excess of butanol was then distilled off. The condenser guarded with a nitrogen balloon and maintained at 25oC, vapour tube guarded with a cotton plug and water bath maintained at 95oC. Tert-butanol crystallizes in the condenser if cooled down).The solid itself got converted into fine powder at the end of the distillation and was then transferred into an air tight glass bottle and sealed with paraffin film. The base prepared in this way required no further pulverisation.

The tert-butanol distilled off using a rotary evaporator and that accumulated in the pocket was mixed and used for the next preparation. Sodium tert-butoxide made from this gave even good quality of the sodium tert-butoxide. The salt so generated dissolved evenly during the reaction.

Discussion-
1) The convenience introduced by the assembly and the method in the routine preparations encouraged us to use it time and again and with time we tried to investigate the thermal changes occurring in the assembly. With the intentions, reactions were carried out using the assembly and the heat changes were recorded with an automated data logger device to record the variation in temperature and the average peak temperature was found in the range of 77oC to 78.5oC. This is notable that the peak temperature is close to the boiling point of the tert-butanol (82oC). Two sets of experiments (at two different room temperatures) were rigorously investigated and the exothermic properties have been recorded from the beginning of the experiment until complete cooling. Figure 4 shows the temperature variations recorded in three different experiments and average peak temperature recorded was 77.42oC. Evolution of gas stopped at 55-60 minutes and the crude product was subjected for distillation of excess of alcohol using rotary evaporator.
2) It was noticed the excess of the tert-butanol works as co-solvent for the reaction and gives soft product.This feature completely eliminated the need of a cosolvent.The peak temperature of the reaction found dependant on the quantity of tert-butanol used. For instance the maximum temperature attained in an experiment with 250 ml of tert-butanol and 23 grams of sodium, was recorded to be the 99.87oC, however removal of excess of t-butanol took more time. The best textured product was achieved with a reaction between 180 ml of tert-butanol with 23 grams of sodium. 22 ml of the alcohol was automatically distilled off and was reserved in in the alcohol pocket during the course of reaction. This dramatically reduced processing time while recovery of the product.
3) There was no un-reacted metal in the base. This was confirmed by measuring the volume of H2 gas generated during the reaction using downward water displacement method and was close to one gram molar volume (22.4L). This indicated complete conversion of the sodium metal

End product-
The overall unprocessed yields of crude product in three subsequent experiments undertaken by the inventor named herein, were 122.21g, 118.78g and 117.62g (theoretical yield of pure product being 96.15 grams) respectively. It can be further concentrated by additional distillation of tert-butanol. The little increase in the weight was because of entrapped alcohol. The exact base to alcohol ratio was calculated by weighting the base. The product may be further concentrated by application of strong vacuum at 80oC.The tert-butanol distilled off using rotary evaporator and that accumulated in the pocket was mixed and used for the next preparation. Sodium tert-butoxide made from this gave even good quality of the sodium tert-butoxide. The salt so generated dissolved evenly during the reaction.

Reaction chemistry:

The above reaction equation shows the process needs not external heat and no cosolvent. Small excess of t-BuOH works as cosolvent and furnishes soft product. This feature completely eliminated the need of a co-solvent. The recovered t-BuOH is thus free from any impurities and can be used for next preparation/production without intermediate need of any purification. The assembly need not to heat externally, as the reaction is itself incubated by it’s own exothermic properties. This saves a lot of electrical energy and water required to maintain cooling.

Procedure for scale up (1 kg production)
The reactor was charged with 230 g of wired sodium (1mm OD) under nitrogen atmosphere and was closed with its lid. 1600 ml of tert-butanol was then poured through the central neck of the lid and the empty alcohol pocket was inserted in the reactor and was isolated using a mineral oil bubbler. The reaction was continued until the bubbling of hydrogen stopped. Un-reacted tert-butanol was then distilled off under vacuum. The procedure yielded 1082 gm of the product in powdered form, as per proforma provided in the Table 2 below.

Attribute Embodiment 1 Embodiment 2
1) Scale ~100-117g ~1000g
2) Reaction vessel 500 ml round bottom flask 5 Litre flask

Table 2

Industrial applicability
The present invention has been successfully reduced to practice by the inventor named herein. A miniature version of the assembly confirming to the illustration shown in the accompanying Figure 1 and using a 500ml flask was used to prepare about 50gm of sodium tert-butoxide within 1.5 hours.

Industrial scale- for example, pharmaceutical industry, need for sodium tert-butoxide is around ~1000 ton in India per year. For this, the inventor proposes making the reaction vessel of steel, thermal insulation (glass wool). Figure 6 is a schematic illustration of an industrial scale reactor for implementing the method of the present invention – as seen here, reactor is divided into two major portions i.e. main body and the lid. The reactor body (14) is built from stainless steel or other thermally stable material with PTFE lining. The lid is mounted on the main body using a rubber/silicone gasket (15). The lead and the main body carry required appendages/accessories as shown in the diagram. The outer surface of the reactor is thermally isolated from environment using insulation layer (16).

The reactor is flushed with Nitrogen (or any other inert atmosphere, or it may be vacuumed to draw all moisture out) and an appropriate amount of sodium metal is pressed inside the empty reactor in form of wire (1-2 mm) (17) diameter using a suitable wire press device / arrangement (hydraulic, screw press etc) (18). The reactor is then charged with tert-butanol through the chemical inlet port (19). The reactor is allowed to operate itself for 2 hours. No external heating or agitation is required at this stage. Reactor temperature rises up and the process is incubated itself. The H2 gas generated is discharged through a pressure release mechanism (20). The hydrogen can be harvested by connecting the outlet (21) to a hydrogen harvester/reservoir unit. The portion above the vacuum port (22) is cooled by cooling fins or a water jacket, which condense the vapours of tert-butanol and return to the alcohol pocket. A portion of excess tert-butanol is distilled inside the alcohol pocket (23) through pores (24) and can be drained out through the alcohol pocket drain (25). Drain (26) is to be used for draining main reactor space.

The product formed inside is crushed into powder by turning on the mechanical agitator (27) and the reactor is heated to 100 degrees. This may be done by electrical heater, hot oil or water circulation. Vacuum is applied through vacuum port (22) and the un-reacted tert-butanol is recovered. The vacuum is then turned off and the tert-butanol is again drained down through alcohol drain port (25). This process is repeated unless un-reacted alcohol is recovered maximum.

The reactor is then allowed to cool down at room temperature and the product is recovered from the reactor by rotating the screw conveyor (28). The product is discharged through port (29) which shall need not further processing.

Advantage over prior art of the present invention can be appreciated from that the reaction is nearly-adiabatically incubated by conservation of its own exothermic property and needs no external heating as the system is thermally isolated from the environment. Thus, the implementation suggested in this paper requires no heating (saves electricity) and reflux condensers (saves water). The assembly shown in Figure 1 also eliminates risks arising through accumulation of hydrogen gas as it safely disposes hydrogen gas in very small volumes whilst isolating the inner reaction from environmental moisture. Also, no co-solvent was required to soften the product. The distilled alcohol was absolutely dry, free from contamination and could be recycled for other reactions without any process and purifications.

As will be realized from the foregoing narration, the present invention is identified in comprising a method and aassembly for implementing said method, to thereby synthesize sodium tert-butoxide, which is green, convenient, cost effective, energy efficient, scalable and consumes less resources in terms of electricity, water and human labour and moreover significantly stands over and above state-of-art by that-
1) Need for supplying external heat is completely abrogated, hence saving on energy input. The preparative part goes with best efficiency at its own generated heat and needs no external heating thus it saves a lot of electricity;
2) preparative phase also need no stirring or any mechanical agitation This also saves electricity;
3) Need for refluxing is completely abrogated, hence saving on need for accessory equipment and water for refluxing;
4) Need for lengthy synthesis phase is completely abrogated, hence bringing down production cycle times–Time required for the process is too small as compare to other reported process. This enables rapid and convenient cost-effective industrial production;
5) Use of molten sodium is not required, wire can be safely handled (moderate surface area) – in line with the disclosures hereof, sodium is required in wired form, preparing sodium wire is easier than melting it or preparation of fine dispersion;
6) Formation of hazardous process by-products is completely abrogated, hence increasing safety of the process established, particularly, the slow release of hydrogen arranged in the assembly proposed herein make it entirely safe and convenient to use.
7) Need for bulky, complex and expensive equipment is completely abrogated, thereby enjoining a cost-effective, safe, compact, convenient and simple apparatus setup which negates inclusion of external appendages like condenser, water pipes, retort stand, heating mantles etc;
8) The method proposed herein does not use any organic solvent as cosolvent or softener. This helps in saving bucks required for solvents. Additionally no solvent traces passed in product and the product prepared in this way is free from hydrocarbon impurities. Traces of native t-BuOH is only the impurity and it the reaction by product (use of t-BuONa generates t-BuOH as by product in the reaction).
9) Need of continuous human attention is completely abrogated, which is otherwise required by an ordinary reflux assembly
10) Production of hard-to extract / lumpy end-products, therein conversely providing finely powdered and free flowing sodium tert-butoxide which needs no further pulverization and processing – the product is delivered in soft mass and needs no further grinding or pulverization.
11) The assembly is portable and need no electrical supply. It can be placed anywhere and independent of any outer appendages and / or anchorages
12) Assembly is stand alone, needs no electrical connections, water connections and is fully portable. This enables industrial scale reactors to installed in open places
13) No water mediated cooling is required, it saves lot of water otherwise required for cooling
14) The second stage where the crude product is processed yields find quality of super dried t-BuOH which can be directly recycled for preparation of the t-BuONa. The t-BuONa produced from this recycled t-BuOH gave high quality product
15) The method is scalable and allows many reactors to set together and simultaneously
16) It gives off purest form of hydrogen gas which can be used for Fuel cells and hydrogen vehicles. This a valuable by product is produced
17) Significant amount of t-BuOH is distilled off right inside the reactor assembly which facilitates the purification phase also shortens its time from reaction time from 24 hours in conventional processes to 1.5 hours; and
18) The reactor assembly is easy to manufacture and there aren’t any moving parts. This also saves money required to build reactors.

It shall be generally understood by the reader that although the present invention is described herein using specific terms, these are used in a generic and descriptive sense only and are not intended to be limiting. Furthermore, many modifications and other embodiments of the invention will be apparent to those skilled in the art to which the invention pertains in view of the above description and the teachings presented in the accompanying drawings, all of which are intended to be encompassed by spirit of the present invention.

Accordingly, the present invention has been illustrated herein by way of the specific exemplary embodiments disclosed in this paper, the variations and other embodiments of which shall be readily appreciated, however in that the present invention is restricted solely by the appended claims. ,CLAIMS:1) A system for synthesizing sodium tert-butoxide, comprising-
a) thermal insulation module (01),
b) a reaction vessel (02);
c) an alcohol exchanger pocket with reversible two-chambered mineral oil bubbler (03) or any other suitable appendage serving the purpose;
d) a inner glass joint (11) with a rubber septum (12) provisioned onto the oil bubbler (03) as a facility to inject more alcohol;
e) a flexible silicone tube (13) attached to the oil bubbler (03) for placement in vicinity of a fume extractor for safe disposal of hydrogen gas released.

2) The system for synthesizing sodium tert-butoxide as claimed in claim 1, wherein for a laboratory bench scale setup-
a) the reaction vessel (02) is a round-bottom flask; and
b) the thermal insulation module (01) is the Styrofoam packaging that comes with 2.5 litres chemical glass bottles of which length is trimmed as per the height of the flask (02) and a hole of adequate size is made in its lid to accommodate the neck of the flask (02).
c) the alcohol exchanger pocket with reversible two-chambered mineral oil bubbler (03) consists of-
i. two concentric tubes (04 and 05) which extend towards bottom of the reaction vessel (02) keeping a distance of approximate 2.5cm from the inner surface of reaction vessel (02); and
ii. tiny pores (09 and 10) for evacuation of hydrogen gas generated inside the reaction vessel (02) to the outside environment.

3) The system for synthesizing sodium tert-butoxide as claimed in claim 2, wherein the tube (05) serves as a thermometer pocket (06) in which a digital probe thermometer (07) may be received for monitoring temperature during trial runs of the system.

4) The system for synthesizing sodium tert-butoxide as claimed in claim 3, wherein the thermometer pocket (06) is pre-provisioned with 1 ml of mineral oil to establish good thermal contact with the digital probe thermometer (07).

5) The system for synthesizing sodium tert-butoxide as claimed in claim 4, wherein the empty space (08) around the thermometer pocket (06) is filled with tert-butanol due to internal and simultaneous distillation and as the reaction proceeds, is replaced by distilled alcohol afterwards which keeps reversibly exchanging the vapours in the reaction vessel (02).

6) The system for synthesizing sodium tert-butoxide as claimed in claim 1, wherein for a industrial scalesetup-
a) the thermal insulation module (01)
b) the reaction vessel (02) is a lidded reactor body (14) made of stainless steel with polytetrafluoroethylene lining, wherein said lid is mounted on the main body (14) using a rubber/silicone gasket (15);
c) reversible two-chambered mineral oil bubbler (03); and
d) accessories outfitted to the reaction vessel (02) and reversible two-chambered mineral oil bubbler (03) for synthesis of sodium tert-butoxide on an industrial scale.

7) The system for synthesizing sodium tert-butoxide as claimed in claim 1, wherein the accessories consist of-
a) A wire press device (18) connected to the reaction vessel (02) for charging wired sodium into the reaction vessel (02) amidst a nitrogen atmosphere provisioned inside said reaction vessel (02)
b) A chemical inlet port (19)for charging the the reaction vessel (02) with tert-butanol;
c) A pressure release mechanism (20) for discharging hydrogen gas generated during synthesis of sodium tert-butoxide;
d) vacuum port (22) outfitted to the reaction vessel (02)for recovery of the un-reacted tert-butanol remaining after synthesis of sodium tert-butoxide is completed;
e) pores (24) and an alcohol pocket (23) outfitted to the reversible two-chambered mineral oil bubbler (03)whereby a portion of excess tert-butanol is distilled inside the alcohol pocket (23) through said pores (24) and can be drained out through a alcohol pocket drain (25);
f) Drain (26) outfitted to the lidded reactor body (14) for draining the space within said lidded reactor body (14);
g) mechanical agitator (27)outfitted within the lidded reactor body (14) for crushing the sodium tert-butoxideproduct formed inside the reactor body (14)into powder; and
h) a discharge assembly outfitted within the lidded reactor body (14), said assembly comprising a screw conveyor (28) leading to a port (29) which is outfitted within the lidded reactor body (14) for recovery of the sodium tert-butoxide product from the reactor body (14).

8) The system for synthesizing sodium tert-butoxide as claimed in claims6 and 7, wherein thepressure release mechanism (20) is further connected to a hydrogen harvester / reservoir unit.

9) A method for synthesizing sodium tert-butoxide by using the system of either one between the claims 2 or 6, the method comprising-
a) Ensconcing the reaction vessel (02) with the thermal insulation module (01);
b) Charging wired sodium (17)under nitrogen atmosphere into the reaction vessel (02),
c) Introducing tert-butanolinto the reaction vessel (02);
d) Introducing the alcohol exchanger pocket with reversible two-chambered mineral oil bubbler (03) into the reaction vessel (02);
e) Allowing the reaction to continue until the bubbling of hydrogen stops; and
f) Distilling the remaining tert-butanol off using rotary evaporator to thereby yield the final sodium tert-butoxide product in powder form.
Characterized in that said method-
a) is a rapid process having a cycle time of 1.5 hours;
b) requires no supply of external heat;
c) requires no mechanical agitation during the reaction;
d) eliminates the need for refluxing;
e) eliminates the need for molten sodium as a reactant;
f) eliminates generation of any hazardous process by-products;
g) negates the need for any organic solvent as cosolvent;
h) renders the end product as a soft mass;
i) renders pure hydrogen gas;
j) returns the unreacted or excess tert-butanolin its purest form

10) A sodium tert-butoxide product obtained by the method of claim 2, characterized in-
a) Being rendered in powder form;
b) Having no un-reacted pieces of active sodium entrapped therein; and
c) Having minimal susceptibility to atmospheric moisture during production.