WO2007051309A1

WO2007051309A1 - Process for preparing a metallic salt and recovering hydrogen gas

Info

Publication number: WO2007051309A1
Application number: PCT/CA2006/001810
Authority: WO
Inventors: Blaine Creston Froats; Sean Creston Froats
Original assignee: Alternate Energy Corporation
Priority date: 2005-11-04
Filing date: 2006-11-06
Publication date: 2007-05-10

Abstract

The present invention provides an improved process for the recovery of hydrogen gas and a metallic salt. The metallic salt may be calcium citrate, magnesium citrate, or ferric chloride.

Description

TITLE

PROCESS FOR PREPARING A METALLIC SALT AND RECOVERING HYDROGEN GAS

CROSS-REFERENCE TO RELATED APPLICATIONS

This application claims priority from U.S. patent application no. 60/733,931, filed November 4, 2005, entitled PROCESS TO MANUFACTURE HYDROGEN AND

MAGNESIUM CITRATE and U.S. patent application no. 60/781,026, filed March 9, 2006, entitled PROCESS TO MANUFACTURE HYDROGEN AND CALCIUM CITRATE, and both documents are incorporated herein by reference.

FIELD OF INVENTION

The present disclosure relates to the preparation of a metallic salt useful as a food additive and recovery of hydrogen gas, and more particularly, the present disclosure relates to the preparation of calcium citrate, magnesium citrate, and ferric chloride concurrently with the generation of hydrogen gas by an improved process.

BACKGROUND

It is widely known that mixing a moderate-to-strong acid with almost any metal will release hydrogen gas and form an acid-salt of that initial acid. For example, calcium and magnesium will react spontaneously and exothermically with citric acid to release hydrogen gas and form calcium citrate and magnesium citrate respectively (see, for example, US patent no. 2,027,264, US patent no.

4,814,177, US patent publication no. 20010003002, UK patent no. 136,979, UK patent no. 435,586, UK patent no. 597,936, CA patent no. 2,376,017, PCT publication no. WO87/05507, CZ patent no. 9400928, EP patent no. EP0781756, EP patent no. 0221880, and JP patent publication no. 2003-221362, US patent publication no. 2005/0197402, US patent publication no. 2001/0027214, US patent no. 4,871,375, US patent no. 4,895,980, US patent no. 4,985,593, US patent no. 5,071,874, US patent no. 6,514,537, JP patent publication no. JP2004091422, JP patent publication no. JP411353377, JP patent publication no. 2003-221362, JP patent publication no. 08-073399, US patent no. 1,936,364, and US patent no. 2,260,004). In another example, iron will react spontaneously and exothermically with hydrochloric (HCI) acid to release hydrogen gas and to form ferric chloride.

Metallic salts such as calcium citrate, magnesium citrate and ferric chloride are used extensively. For example, calcium citrate and magnesium citrate can be used for food fortification, dietary supplements, skin care products, and plant nutrition, medications and medical applications. Ferric chloride can be used for color additives and flavourings. Ferric chloride is also used extensively in waste water and drinking water treatment as a flocculent.

Hydrogen gas which is generated during the preparation of such metallic salts discussed above, has, in the past, been treated as a by-product in the preparation of certain foodstuffs. Hydrogen gas is itself useful as a fuel and as a chemical ingredient.

Present methods of generating hydrogen gas do not provide hydrogen as an economically competitive energy source. Methods of making the preparation of hydrogen more economically competitive have been sought. See, for example,

US patent publication no. 2006/0011491, US patent publication no.

2003/0129122, US patent publication no. 2003/0091878, US patent no.

3,895,102, US patent publication no. 2003/0091503, US patent publication no. 2002/0155330.

As both metallic salts useful as food additives and hydrogen gas are of commercial value, methods capable of efficiently producing both these products are desirable. The present disclosure provides improved processes for the preparation of metallic citrates, and in particular calcium citrate and magnesium citrate, and for ferric chloride concurrently with the generation of hydrogen gas.

SUMMARY OF INVENTION

In one aspect, provided is a process for the concurrent generation of hydrogen gas and metal citrate comprising: reacting a metal capable of forming a foodstuff and a citric acid solution in a reactor vessel to provide hydrogen and metal citrate precipitate, evacuating and bottling the hydrogen; draining the remaining solution; feeding the metal citrate precipitate to a dryer; and utilizing the dryer to recover a dry metal citrate powder which can be used as a foodstuff.

In an embodiment, the process further comprises ensuring proper dispersal of feed in the dryer utilizing a paddle mixer.

In an embodiment, the process further comprises back-mixing dried product with the wet product.

In an embodiment, the dryer is a ring dryer.

In an embodiment, the temperature of the air in the ring dryer has an inlet temperature profile of about 400 degrees Celsius.

In an embodiment, the temperature of the air in the ring dryer has an outlet temperature of about 150 degrees Celsius.

In an embodiment, the pressure within the reactor vessel is atmospheric pressure.

In an embodiment, the metal comprises 1/4 inch granules.

In an embodiment, the metal is calcium and the concentration of the citric acid solution is 400 grams per liter of water.

In an embodiment, the metal is magnesium and the concentration of the citric acid solution is 200 grams per liter of water.

In an embodiment, the reactor vessel is maintained at a temperature of about 100 ⁰C.

In an embodiment, the hydrogen is scrubbed prior to bottling.

In an embodiment, the hydrogen is dehydrated prior to bottling. In an embodiment, the reactor vessel is about 10000 to about 15000 liters.

In an embodiment, the reactor vessel is about 100 to 300 liters.

In an embodiment, the reactor vessel is about 100 to 300 liters

In an embodiment, the reactants are fed to the reactor vessel at ambient temperatures.

In an embodiment, the process further comprises the step of recovering heat from said reaction for use as a heat source or energy source.

In another aspect, provided is a process for the concurrent generation of hydrogen gas and ferric chloride comprising : reacting iron and HCI acid solution in a reactor vessel to provide hydrogen and a ferric chloride enriched solution, evacuating and bottling the hydrogen; and recovering the ferric chloride enriched solution.

In an embodiment, the process further comprises the step of concentrating the ferric chloride enriched solution using a vacuum condenser.

In an embodiment, the concentration of ferric chloride in the ferric chloride enriched solution is about 25 to 45 percent by weight.

In an embodiment, the concentration of HCI acid in the ferric chloride enriched solution is less than 3 percent by weight.

In an embodiment, the process further comprises the step of removing the ferric chloride from solution to provide anhydrous ferric chloride.

In an embodiment, the reactor vessel is maintained at a temperature of about 50 to 75 ⁰C.

In an embodiment, the hydrogen is scrubbed prior to bottling.

BRIEF DESCRIPTION OF THE DRAWINGS

Preferred embodiments of the invention will now be described, by way of example, with reference to the accompanying drawings, in which:

FIG. l is a diagram depicting an exemplary process for preparing a metallic citrate and generating hydrogen gas; and

FIG.2 is a diagram depicting an exemplary process for preparing ferric chloride and generating hydrogen gas.

DETAILED DESCRIPTION

Concurrent Preparation of a Metallic Citrate and Generation of Hydrogen Gas

Metallic citrates, uses thereof, and methods of preparation thereof of are known. The present disclosure provides an improved process for the preparation of metallic citrates, such as for example, calcium citrate and magnesium citrate, concurrently with the generation of hydrogen gas.

Calcium citrate is a white, odorless powder and is a useful product with many applications. Generally, such applications include, for example, use as a safe nutrient and food additive having functions of acidity regulator, sequestering and stabilizing agent, antioxidants synergist, firming agent, calcium enrichment In foods and medicine. Calcium citrate is also useful in many medications and medical application. It is commonly used as a food additive, usually as a preservative, but sometimes for flavor. Calcium citrate is also used as a water softener.

The production of calcium citrate is a known process. In this process, citric acid is reacted with calcium to form calcium citrate and hydrogen. The representative chemical reaction is illustrated below.

2C₆H₈O₇ +3Ca → Ca₃(C₆H₅O₇)₂ + 3H₂

Magnesium citrate is a useful product in the pharmaceutical industry. The product is used in several applications, including, for example, food fortification, dietary supplements, skin care products, and plant nutrition. Magnesium citrate is also useful in many medications and medical applications.

The production of magnesium citrate is a known process. In this process, citric acid is reacted with magnesium to form magnesium citrate and hydrogen. A typical chemical reaction is illustrated below.

2H₃C₆H₈O₇ +3Mg → Mg₃(C₆H₅O₇)₂ + 6H₂

The present disclosure provides an improved process for the concurrent preparation of a metallic citrate and recovery of hydrogen gas. The improved process of the present disclosure provides a safe and more efficient and effective process for providing both a metallic citrate and hydrogen gas. The improved process of the present disclosure provides the advantage that single process, and accordingly a single reactor system can be employed for the obtaining both metallic citrates and hydrogen gas, both of which are valuable commercial products.

In one implementation of the present disclosure, an efficient and safe process for concurrent preparation of calcium citrate and generation of hydrogen gas is disclosed. In other implementations of the process, other metallic elements can be utilized to produce various metallic citrates. In an exemplary implementation, calcium citrate tetrahydrate is produced. Calcium citrate tetrahydrate is depicted by the chemical formula Ca₃(C₈H₅θ₇)₂-4H₂O. An exemplary chemical structure of calcium citrate is illustrated below.

Ca2+ Ca2+ Ca2+

In another exemplary implementation, anhydrous tricalcium citrate is produced. Anhydrous tricalcium citrate is depicted by the chemical formula Ca₃(C₈H₅O₇)₂.

In another implementation of the present disclosure, an efficient and safe process for concurrent preparation of magnesium citrate and generation of hydrogen gas is disclosed.

In an exemplary implementation, magnesium citrate nonahydrate is produced. Magnesium citrate nonahydrate is depicted by the chemical formula

An exemplary chemical structure of magnesium citrate is illustrated below.

In a particular implementation, a reactor vessel is provided in which calcium or magnesium and a citric acid solution are reacted. The reactor vessel may be batch reactor. Advantageously, no electrolysis or external influence is involved in the reaction. Where the reactants are calcium and citric acid, as the reaction continues, the reactants form a powder of calcium citrate tetrahydrate that forms a precipitate at the bottom of the reaction vessel.

Where the reactants are magnesium and citric acid, as the reaction continues, the reactants form a powder of magnesium citrate nonahydrate that forms a precipitate at the bottom of the reactor vessel.

During the reaction, hydrogen gas is also generated. The reaction bubbles vigorously and hydrogen is expelled from the reaction mixture along with some water vapor. The hydrogen gas is evacuated from the reactor vessel during the reaction and is bottled. In another exemplary implementation, the hydrogen is evacuated, scrubbed, dehydrated and bottled to provide clean hydrogen gas suitable for use in the food industry or as a fuel.

In an exemplary implementation, the vessel is maintained at or near atmospheric pressure. Conducting the reaction at atmospheric pressure prevents formation of a crystallized layer of the product on the inside of the reactor.

However, other pressures may also be utilized and are within the scope of the present disclosure. For example, a slightly elevated pressure will be utilized in the reactor if the temperature is slightly greater than 100 ⁰C.

In particular implementations, the reactants are fed into the reactor vessel or reactor at ambient temperature. However, the reaction of calcium and citric acid and the reaction of magnesium and citric acid are exothermic. Therefore, the temperature of the reactants will increase and be maintained at a higher temperature. Heat produced by the reaction can be recovered and utilized, either directly, e.g. in heating nearby buildings or indirectly, e.g. supplying heat to other processes, e.g. to generate power via steam.

In particular implementations, the reaction is maintained at as high of a temperature as practical. As the temperature increases, the rate of reaction also increases. In an exemplary implementation, the temperature will be just below the boiling point of water. In another implementation the temperature of the reaction will be at the boiling point of water. The temperature can be varied to control the speed of the reaction.

In an exemplary implementation, the calcium or magnesium is utilized in the form of ¹A inch granules. Utilization of granules increases the surface area of the calcium or magnesium and increases the speed of the reaction, while also maintaining the safety of the reaction. Of course, other forms of calcium or magnesium may also be utilized. For example, calcium or magnesium in the form of plates, rods, powder, or alternative sized granules area also contemplated as being useful and are within the scope of the present disclosure.

The exemplary utilization of calcium or magnesium granules also allows for easier handling of the metal feed. In particular implementations, the calcium or magnesium is in the form of granules to facilitate easier automatic handling and feed systems to provide the calcium or magnesium to the reactor vessel than larger forms of the calcium or magnesium.

The rate of the reaction for the preparation of the desired metallic citrate and hydrogen is dependent on the concentration of the citric acid.

In particular implementations for the preparation calcium citrate and generation of hydrogen gas, the concentration of the citric acid solution is about 400 grams per liter of water. A calcium citrate precipitate is formed very quickly when metallic calcium is reacted with citric acid. In further exemplary implementations, calcium can be used in a ratio of approximately 1 kilogram of calcium to 3 kilograms of citric acid. Other ratios of calcium to citric acid may also be used in various implementations.

In particular implementations for the preparation of magnesium citrate and generation of hydrogen gas, the concentration of the citric acid solution is about 200 grams per liter of water. The rate of the reaction is dependent on the concentration of the citric acid. A lower concentration slows the rate of reaction. A higher concentration makes the solution much more viscous, and prevents free circulation of the acid around the magnesium, slowing the reaction. In further exemplary implementations, magnesium can be used in a ratio of approximately 1 kilogram of magnesium to 3 kilograms of citric acid. In an exemplary implementation, the reactor vessel has a capacity of about 10000 to about 15000 liters. A reactor this size will enable a larger scale reaction. In another exemplary implementation, the reactor vessel has a capacity of about 100 to 300 liters. In a particular implementation, production of calcium citrate or magnesium citrate will be accomplished at about 100 pounds per minute. The reaction rate for the preparation of calcium citrate or magnesium citrate may be varied to achieve a desired output by varying the temperature, the size of the reactor vessel, and the amount of reactants.

As the reaction comes to completion, the reaction mixture is drained from the reactor vessel to a settling tank where the calcium citrate or magnesium citrate then sttles to the bottom of the settling tank in a sludge-like deposit. The clear solution remaining above the precipitate is drained from the settling tank and can be recycled into the process for preparing calcium citrate or magnesium citrate. The remaining precipitate can be transferred for drying as described below.

In a particular implementation of the present disclosure, a drying method is utilized to obtain the product from the precipitate. In an exemplary implementation, a ring drying method is utilized. In a ring drying method the material to be dried is dispersed through the dryer in a hot air stream. The ring dryer incorporates a centrifugal classifier, allowing internal recirculation of the semi-dried solids. This allows lengthening the time that the larger particles are in the dryer, while the finer particles, which dry more rapidly, leave the dryer. This accelerates the process of drying the product.

In other implementations, alternative drying methods may also be utilized. Exemplary drying methods comprise flash dryers, fluidized bed dryers, rotary dryers, paddle dryers and column dryers. It is also contemplated that a combination of dryers may be utilized to expedite the process. An exemplary system for an improved and efficient generation of hydrogen concurrently with the preparation of metallic salts such as calcium citrate or magnesium citrate is depicted in FIG. 1. First, the desired metallic salt is prepared in the reactor 100 as described above. The hydrogen gas generated during the course of the reaction is evacuated to a storage vessel 170 for subsequent bottling. A metallic salt feed 105 enters the dryer via a screw feed conveyor into a paddle mixer 110.

To ensure proper efficiency when utilizing a ring drying method, proper dispersal of the feed is required. If the feed is too wet or too sticky, efficient drying cannot be accomplished. In an exemplary implementation, proper dispersal is ensured through external back-mixing of some of the recycled, dried product. This may be accomplished utilizing a paddle mixer 110.

In a particular implementation, the metallic salt enters the ring dryer, which contains a disintegrator 115. The disintegrator 115 breaks up large particles of the metallic salt, enabling faster drying of the feed. The feed is entered into a hot air stream after the disintegrator 115. The stream of air and magnesium citrate goes through the ring duct 120 to the centrifugal classifier 125.

Air 130 is entered into the system through an induced draught fan 135. The fan 135 pulls in the air 130 through an air filter. The fan 135 then sends the air to a heater 140 when the air is heated before entering the ring dryer. In some implementations, the temperature of the air in the ring dryer has an inlet temperature of about 400 degrees Celsius. The temperature of the air in the ring dryer has an outlet temperature of about 150 degrees Celsius.

The centrifugal classifier 125 has a series of adjustable deflector blades to control the amount of recirculation within the dryer. The centrifugal classifier 125 provides selective classification of the larger, wetter particles and recirculates the wetter particles of the metallic salt back through the drying duct for an extended drying time. The smaller dry particles leave the dryer from the centrifugal classifier 125 and enter a dust collector 145. In the dust collector 145, the dried metallic salt product 155 is collected. A portion of the product 155 is placed back into the dryer through a recirculation feed 150 to the paddle mixer 110 ensuring proper dispersal of the feed in the dryer.

After the final product is collected, other facilities will also be utilized. For example, storage and packaging facilities will be used to prepare the metallic salt for sale.

After utilizing the drying step of the process, the final product, a dry powder of metallic salt, is suitable for USP certification and use in several applications. For example, calcium citrate and magnesium citrate can be used for food fortification, dietary supplements, skin care products, and plant nutrition, medications and medical applications.

Concurrent Preparation of Ferric Chloride and Generation of Hydrogen Gas

Ferric chloride is a reddish brown liquid which commonly has a concentration of 33 to 45% in water. Anhydrous ferric chloride crystals are dark in color and hexagonal in shape. Ferric chloride is a multipurpose food additive and is used for colorings and flavorings. Ferric chloride is also used extensively as a flocculent in several water treatment applications including the treatment of waste water and potable drinking water

Ferric chloride is depicted by the chemical formula FeCI₃. The production of ferric chloride is a known process. In this process, hydrochloric (HCI) acid is reacted with iron to form ferric chloride and hydrogen. A typical chemical reaction is illustrated below.

2Fe + 6HCI → 2FeCI₃ + 3H₂

It is desirable to improve the process of making ferric chloride by reducing the number of steps required in the making of ferric chloride. Moreover, it is further desirable to minimize the HCI concentration in the product to make it suitable for use in waste water treatment.

In one implementation of the present disclosure, an improved process for concurrently preparing ferric chloride and generating hydrogen gas is disclosed.

FIG.2 shows an exemplary process for the concurrent preparation of ferric chloride and generation of hydrogen gas.

In a particular implementation, a reactor vessel 200 is provided in which iron and a hydrochloric (HCI) acid solution are reacted. The reactor vessel may be a batch reactor. Advantageously, no electrolysis or external influence is involved in the reaction.

The reaction provides an enriched solution of ferric chloride and the generation of hydrogen gas. Hydrogen gas is expelled from the reaction mixture along with some water vapor. The hydrogen gas is evacuated from the reactor vessel during the reaction and is bottled.

In another exemplary implementation, the hydrogen is evacuated, scrubbed, dehydrated and bottled to provide clean hydrogen gas suitable for use in the food industry or as a fuel.

In an exemplary implementation, the reactor vessel is maintained at or near atmospheric pressure. Conducting the reaction at atmospheric pressure eliminates the need for pressure vessels and special procedures required for them. However, other pressures may be utilized and are within the scope of the present disclosure.

In particular implementations the temperature is maintained between 50 and 75 ⁰C. As the temperature increases from ambient, the reaction progresses more vigorously. If the temperature rises higher than nominally 75 ⁰C, the vaporization of the hydrochloric acid increases and becomes excessive. Since the reaction is exothermic, the temperature can be controlled by removing excess heat as required. This excess heat may also be used as a source of energy for other stages of the process. Heat produced by the reaction can be recovered and utilized, either directly, e.g. in heating nearby buildings or indirectly, e.g. supplying heat to other processes, e.g. to generate power via steam.

In an exemplary implementation, metallic iron in the form of granulated iron or mil) scale is preferentially used. Utilization of granulated iron or mill scale increases the surface area and increases the rate of the reaction, while also maintaining the safety of the reaction. Other forms of iron can be used including scrap and recycled material from stamping plants, mills, machine shops and other industries and are also contemplated as being useful within the scope of the present disclosure.

The exemplary utilization of iron also allows for easier handling of the metal feed. In particular implementations, the to the use of granulated iron facilitates easier automatic handling and feed systems to provide the iron to the reactor vessel than larger forms of the iron.

In particular implementations, the concentration of hydrochloric acid is between 25 percent and 38 percent. The rate of the reaction is dependent on the concentration of the hydrochloric acid. A lower or higher concentration affects the rate of the reaction.

A stochiometric excess of iron is made available in the reaction. As the reaction approaches completion the the hydrogen production falls below a predetermined level. At this point the hydrochloric acid is substantially consumed. The desired product, ferric chloride, is held in solution. The solution is then filtered, concentrated, and packaged for transportation.

In an exemplary implementation the reactor vessel has a capacity of about

10000 to 15000 liters. A reactor this size will enable a larger scale reaction. In another exemplary implementation, the reactor vessel has a capacity of about 100 to 300 liters. The reactor may be fabricated from polymer resin impregnated fiberglass or a stainless steel or other material impervious to the reactants. In a particular implementation, production of ferric chloride will be accomplished at 100 pounds per minute.

The reaction rate for ferric chloride may be varied to achieve a desired output by varying the size of the reactor vessel, the temperature of the reactants and the amount and form of reactants.

During the reaction hydrogen gas is also produced. In an exemplary implementation, the hydrogen gas is evacuated from the vessel during the reaction and is bottled. In another exemplary implementation, the hydrogen is evacuated, scrubbed, dehydrated and bottled.

In a particular implementation of the present disclosure, a concentrating method is utilized to achieve the necessary concentration. In an exemplary implementation a decompression method is used. This decompression effects a partial vaporization of the water present in the ferric chloride solution. A concentration of the ferric chloride solution thus results. The geometry of the vessel only needs to permit the separation of the vapor phase from the liquid phase.

In a particular implementation of the present disclosure, the reaction product is advantageously heated during decompression to assist the evaporation of the excess water. In an exemplary implementation, temperature will be maintained at less than 110 ⁰C to avoid the decomposition of the ferric chloride. In exemplary implementations, the ferric chloride concentration is preferably between 28 and 45 % by weight of the ferric chloride enriched solution. In further exemplary implementations, the HCI concentration of the ferric chloride enriched solution is preferably less than 3% by weight.

The decompression stage incorporates a vacuum condenser 210 which typically comprises a filter, condenser, vacuum pump and condensate receiving vessel. The pump may be a Coanda effect pump, steam ejector or any other suitable pump. In other implementations, alternative concentrating methods may also be utilized. Exemplary concentrating methods include solar and electrical. It is also contemplated that other concentrating methods may be used, alone or in combination with these.

After the required concentration is achieved, other facilities will also be utilized. In an exemplary implementation storage and bottling facilities will also be needed to prepare the ferric chloride for transportation.

After performing the concentration step the final product, an aqueous solution of ferric chloride, can be certified for use in flocculation of all and any water treatment process.

Optionally, the ferric chloride may be substantially removed from solution using a concentrator 220 or other suitable means to provide crystalline anhydrous ferric chloride.

While the above description contains many particulars, these should not be considered limitations on the scope of the invention, but rather a demonstration of implementations thereof. Accordingly, it is not intended that the scope of the invention in any way be limited by the above description. The various elements of the claims and claims themselves may be combined any combination, in accordance with the teachings of the present disclosure, which includes the claims.

Claims

What is claimed is:

1. A process for the concurrent generation of hydrogen gas and metal citrate comprising :

reacting a metal capable of forming a foodstuff and a citric acid solution in a reactor vessel to provide hydrogen and metal citrate precipitate,

evacuating and bottling the hydrogen;

draining the remaining solution;

feeding the metal citrate precipitate to a dryer; and

utilizing the dryer to recover a dry metal citrate powder which can be used as a foodstuff.

2. The process in claim 1 further comprising ensuring proper dispersal of feed in the dryer utilizing a paddle mixer.

3. The process in claims lor 2 further comprising back-mixing dried product with the wet product.

4. The process according to any one of claims 1 to 3, wherein the dryer is a ring dryer.

5. The process in claim 4 wherein the temperature of the air in the ring dryer has an inlet temperature profile of about 400 degrees Celsius.

6. The process in claims 4 or 5 wherein the temperature of the air in the ring dryer has an outlet temperature of about 150 degrees Celsius.

7. The process according to any one of claims 1 to 6, wherein the pressure within the reactor vessel is at or near atmospheric pressure.

8. The process according to any one of claims 1 to 7 wherein the metal comprises 1/4 inch granules.

9. The process according to any one of claims 1 to 8 wherein the metal is calcium.

10. The process according to claim 9 wherein a concentration of the citric acid solution is 400 grams per liter of water.

11. The process according to any one of claims 1 to 8 wherein the metal is magnesium.

12. The process according to claim 11 wherein a concentration of the citric acid solution is 200 grams per liter of water.

13. The process according to any one of claims 1 to 12 wherein the reactor vessel is maintained at a temperature of about 100 ⁰C.

14. The process according to any one of claims 1 to 13 wherein the hydrogen is scrubbed prior to bottling.

15. The process according to any one of claims 1 to 14 wherein the hydrogen is dehydrated prior to bottling.

16. A process for the concurrent generation of hydrogen gas and ferric chloride comprising:

reacting iron and HCI acid solution in a reactor vessel to provide hydrogen and a ferric chloride enriched solution,

evacuating and bottling the hydrogen; and

recovering the ferric chloride enriched solution.

17. The process according to claim 16 further comprising the step of concentrating the ferric chloride enriched solution using a vacuum condenser.

18. The process according to claim 16 or 17 wherein the concentration of ferric chloride in the ferric chloride enriched solution is about 25 to 45 percent by weight.

19. The process according to any one of claims 16 to 18 wherein the concentration of HCI acid in the ferric chloride enriched solution is less than 3 percent by weight.

20. The process according to claim 16 or 17 further comprising the step of removing the ferric chloride from solution to provide anhydrous ferric chloride.

21. The process according to any one of claims 15 to 20, wherein the reactor vessel is maintained at a temperature of about 50 to 75 ⁰C.

22. The process according to any one of claims 15 to 21 wherein the hydrogen is scrubbed prior to bottling.

23. The process according to any one of claims 1 to 22 wherein the hydrogen is dehydrated prior to bottling.

24. The process according to any one of claims 1 to 23, further comprising recovering heat from said reaction for use as a heat source or energy source.

25. The process according to any one of claims 1 to 24 wherein the reactor vessel is about 10000 to about 15000 liters.

26. The process according to any one of claims 1 to 24 wherein the reactor vessel is about 100 to about 300 liters

27. The process according to any one of claims 1 to 26 wherein the reactants are fed to the reactor vessel at ambient temperatures.