FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
The Patent Rules, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)
TITLE OF THE INVENTION
A REACTION CONTROL SYSTEM FOR THE CONTROLLED SYNTHESIS OF MAGNESIUM ALKOXIDE"
We, Reliance Industries Limited, of 3rd Floor, Maker Chamber-IV, 222, Nariman Point, Mumbai — 400 021, Maharashtra, India.
The following specification particularly describes the nature of the invention and the manner in which it is performed:

FIELD OF INVENTION
The present invention relates to a reaction control system to control the synthesis of magnesium alkoxide. The present invention also relates to improved process of preparing the magnesium alkoxide in a controlled manner. The present invention more specifically relates to a process of controlling the exothermic reaction of magnesium with alcohol in case of run away reaction.
BACKGROUND OF THE INVENTION
Magnesium alkoxide is an important family of chemical compounds which find variety of usage in pharmaceuticals, specialty chemicals and catalysis. Magnesium readily reacts with alcohol to form corresponding alkoxide in a highly exothermic reaction. This reaction of magnesium with alcohols produces hydrogen which is an explosive and highly flammable
gas.
Magnesium alkoxide precursor is prepared by reacting magnesium with alcohols in presence of halogen. Reaction of magnesium with ethanol is highly exothermic and generates hydrogen.
Mg +Alcohol ——► Mg Alkoxide + H2 (g)
Because of exothermic nature sometimes magnesium alkoxide precursor synthesis reaction can go violent and can generate hydrogen at a very high rate. In such case if hydrogen generation is not controlled or stopped or hydrogen venting is blocked the pressure may rise and can result in explosion.
Runway reaction is a probable situation due to the reactivity of magnesium with alcohols. Effects of runaway situations can be devastating as the process is highly exothermic and proceeds with hydrogen generation. The uncontrolled reaction can lead the reactor pressurization and explosion leading to major incident. Safety of this reaction is a major problem that needs to be addressed.
Several methodologies for synthesizing magnesium alkoxide are known. These methods involve improvement of the particle level properties of magnesium alkoxide or process improvements. However, till date no system or process for controlled synthesis of magnesium

alkoxide is known. None of the prior known processes describes or discloses any method or process to control or stop the reaction during runaway situation or emergency.
WO 2005/044873 discloses a process for preparing spherical particles of magnesium alkoxide by reacting magnesium with alcohol and halogen compound below the boliling point of the mixture. This patent application focuses on the particle morphology. The other patents which describe the synthesis of magnesium alkoxide are US20010012908, US5965478, US5917100, US4469648, EP0461268, and US5556820. However, none of these patents or patent application discloses the synthesis of magnesium alkoxide with measures to control or quench a runaway reaction.
The present invention provides reaction system to control the synthesis of magnesium alkoxide, an improved process for the preparation of magnesium alkoxide, a process of controlling or stopping the process of magnesium alkoxide synthesis in case of operational emergencies such as failure of agitator, power failure, excessive heating or addition of higher catalyst quantity and all those factors which can lead to runaway condition.
The present invention provides a controlled process for preparing magnesium alkoxide to prevent the uncontrolled reaction which can lead the reactor pressurization and explosion leading to major incident.
SUMMARY OF THE INVENTION
The present invention provides a reaction control system to control the synthesis of magnesium alkoxide. The present invention further provides a method for controlling the magnesium alkoxide synthesis. The invention also provides method for controlled synthesis of magnesium alkoxide.
OBJECTS OF THE INVENTION
Various operational emergencies such as failure of agitator, power failure, excessive heating or addition of higher catalyst quantity and other factors can lead to runaway reaction which can result in explosion. Therefore, it is an object of the present invention is to provide a reaction control system to carry out the synthesis of magnesium alkoxide with a feature of stopping runaway reaction.

Another object of the present invention is to provide a process for preparing magnesium alkoxide with enhanced safety feature(s) with a special feature to slow down or stop the reaction as required during any emergency.
Another object of present invention is to provide a method of stopping or controlling the reaction of magnesium with alcohol in case of operational emergencies.
STATEMENT OF INVENTION
The present invention provides a reaction control system comprising: a pressure sensor, a precursor synthesis reactor, a reaction control agent tank, a control valve; wherein sensor is attached to precursor synthesis reactor to detect reactor pressure, a control valve is fitted on precursor synthesis reactor connected with reaction control agent tank; wherein the sensor monitors the pressure in reactor and opens the valve to inject control agent into reactor thereby quenching the reaction when pressure goes beyond set pressure valve.
In an embodiment of the present invention the control agent is selected from group comprising of water or aqueous solution of NaOH or their mixture in any other solvent.
In an embodiment of the present invention the sensing device a pressure sensing device which is generally a diaphragm type sensor.
In another embodiment of the present invention the reaction control system further comprises pressure transmitters (PT).
In another embodiment of the present invention the pressure transmitters (PT) transmits the information from pressure sensor to the control valve.
In yet another embodiment the present invention provides a controlled process for preparing magnesium alkoxide comprising: reacting magnesium with alcohol in the presence of halogen; quenching the reaction of step a) by adding control agent.
In an embodiment the control agent is selected from the group consisting of water or aqueous solution of NaOH or their mixture with any other solvent.
In another embodiment the present invention provides a method for controlling the magnesium alkoxide synthesis comprising: reacting magnesium with alcohol in the presence

of halogen or halogen containing compound in precursor synthesis reactor; detecting the increase in pressure in the reaction of step a) in precursor synthesis reactor via pressure sensor; transmitting information of increase in pressure to safety control valve through pressure transmitter(PT) from pressure sensor to control valve; and quenching the reaction of step a) by releasing control agent from the control agent tank through control valve into the precursor synthesis reactor.
In an embodiment the control agent is selected from the group comprising of water or aqueous solution of NaOH or their mixture in any other solvent.
In another embodiment a reaction control system is used in the controlled synthesis of magnesium alkoxide.
In an embodiment of the invention the prepared aqueous solution of NaOH can have a concentration in the range of 1-40%.
BRIEF DESCRIPTION OF DRAWINGS
Fig 1: Reaction control system comprising a pressure sensor (2), a precursor synthesis reactor (1), a reaction control agent tank (3) and a control valve (4).
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a reaction control system comprising a pressure sensor attached to precursor synthesis reactor to detect reactor pressure; a reaction control agent tank and a control valve fitted on precursor synthesis reactor connected with reaction control agent tank; wherein the sensor monitors the pressure in reactor and transmits the signals to control valve to to inject control agent into reactor to quench the reaction when pressure goes beyond set pressure value.
Any pressure sensing device can be used in the reaction control system, usually diaphragm type sensors are used.
The pressure sensor sends information to safety control valve at the set pressure. Pressure can be decided based on the process requirement. The reactions are conducted at any pressure in the range of 0.01-10.0 kg/cm2 and preferably in the range of 0.2-0.3 bar (above atmosphere) to avoid moisture engress in the system.

The pressure of reaction can go up by 15-20 % for initial 5-10 seconds immediately after addition of control agent; this is also considered for setting the pressure.
In the reaction control system pressure transmitter (PT) are used to transmit the signals from pressure sensor to control valve.
Usually 60% by volume of reactor is used for reaction, 20% by volume of reactor of control agent may be added to quench the reaction and it may also act as cooling agent for reaction mixture.
Parallel to the quenching of reaction heating should be stopped and maximum cooling should be done to aid the stopping of reaction.
Whenever the reaction goes out of control then it can be regulated or quenched by adding small quantity of control agent. The control agent is selected from water, dilute NaOH solution, and their mixture in any other solvents. These agents react with magnesium and retard the reaction of magnesium with alcohol by forming a protective layer on magnesium surface and thus rendering it unavailable for reaction with alcohol.
The present invention also provides a process for controlled synthesis of magnesium alkoxide comprising the steps of:
a) Reacting magnesium and alcohol in the presence of halide;
b) quenching the reaction of step a) by adding control agent.
The control agent is water or aqueous solution of NaOH or their mixture with other solvents. NaOH solution with a concentration of 1-40% can be used. Any other solvent can be selected from a group of any non-reacting solvents such as alcohols, oils, paraffin etc.
The inventors found that water or aqueous solution of NaOH solution can quickly stop or slow down the reaction of magnesium with alcohol and hence reduce hydrogen generation.
The control agent reacts with Mg and forms magnesium hydroxide, which creates a coating over Mg particle and act as a barrier against alcohol and chemical agent to further react with

Mg. This leads to slowing down or stopping the reaction of Mg with either alcohol or control agent used for quenching reaction thus reduces hydrogen generation and associated risks.
When water alone is used to quench the reaction, it forms a gel like reaction mass whereas in case of NaOH solution in water, no gel formation happen and is easy to drain from reactor.
The present invention also provides a method for controlling runaway situations involved in a process of preparing magnesium alkoxide. A method for controlling the reaction of magnesium alkoxide synthesis comprises:
a) increase in the pressure during the reaction of magnesium with alcohol in precursor synthesis reactor;
b) pressure sensor send information to safety control valve via pressure transmitter(PT);
c) release of the control agent from the control agent tank via control valve to quench reaction of step a) in precursor synthesis reactor.
The present invention also provides a reaction control system comprising:
a) a pressure sensor (2) attached to precursor synthesis reactor (1) to detect reactor
pressure and
b) a control valve (4) fitted on precursor synthesis reactor (1) connected with reaction
control agent tank (3);
wherein said sensor monitors the pressure in the reactor and pressure transmitter (6) transmits the signals of increased pressure to control valve to to inject control agent into the reactor.
The control agent is either water or aq. solution of NaOH or their mixture with any other solvent. Water or aqueous solution of NaOH reacts with Mg and forms magnesium hydroxide, which creates a coating over Mg particle and act as a barrier against alcohol and chemical agent to further react with Mg. This leads to slow down or stop reaction of Mg with either alcohol or chemical agent used for quenching reaction thus reduces hydrogen generation and associated risks.

The present invention is illustrated and supported by the following examples. These are merely representative examples and optimization details and are not intended to restrict the scope of the present invention in any way.
EXAMPLES:
Example 1
Reacting 100ml of methanol with 3 gm of magnesium at room temperature. Continuously observing any change in hydrogen flow. Adding 5 ml of DM water to the reaction mixture when hydrogen flow reaches to ~900ml/min. The hydrogen flow reduces to nil within a period of 40 seconds of adding DM water.
Example 2
Reacting 100ml of Methanol with 3gm of magnesium at room temperature. Continuously observing any change in hydrogen flow. Adding 5ml of DM water to the reaction mixture using dropping funnel when hydrogen flow reaches ~450ml/min. After addition of DM water there is an immediate increase in hydrogen flow to 600 ml/min for a period of 3-4 seconds. However, the Hydrogen flow reduces to 0 ml/min within a period of 40 seconds of adding DM water.
Example 3
Reacting 100ml of Methanol with 3gm of magnesium at room temperature. Continuously observing any change in hydrogen flow. Adding 5 ml NaOH solution in DM water using dropping funnel when hydrogen flow reaches to ~500m!/min. After addition of NaOH solution there is an immediate increase in hydrogen flow to 600 ml/min for 3-4 seconds, which is then reduced to 0 ml/min in 40 seconds.
Example 4
Reacting 5gm of magnesium with 150ml of ethanol at room temperature, increasing reaction temperature to 70 °C in steps. At 70°C vigorous bubbling is observed in the reactor. 5 ml of DM water using dropping funnel is added to the reaction mixture. Bubbling in the reaction stops completely within seconds of DM water addition.

Advantages of the present invention:
1. The reaction control system of the present invention reduces the risk of explosion of reactor due to high pressure.
2. The process of present, invention is useful for controlled synthesis of magnesium alkoxide.
3. The process for preparing magnesium alkoxide according to present invention is safe.

We claim:
1. A reaction control system comprising: a pressure sensor, a precursor synthesis reactor,
a reaction control agent tank, a control valve;
wherein the sensor is attached to the precursor synthesis reactor to detect reactor pressure, the control valve is fitted on precursor synthesis reactor connected with reaction control agent tank;
wherein the sensor monitors the pressure in reactor and opens the valve to inject control agent into reactor thereby quenching the reaction when pressure goes beyond set pressure value.
2. The reaction control system as claimed in claim 1, wherein the control agent is selected from group consisting of water or aqueous solution of NaOH or their mixture in any other solvent.
3. The reaction control system as claimed in claim 1, wherein the sensing device is a pressure sensing device.
4. The reaction control system as claimed in claim 1, wherein the sensing device is a diaphragm type sensor.
5. The reaction control system as claimed in claim 1, wherein said reaction control system further comprises pressure transmitter (PT).
6. The reaction control system as claimed in claim 1, wherein the pressure transmitters transmits the information from pressure sensor to the control valve.
7. A controlled process for preparing magnesium alkoxide comprising:

a) reacting magnesium with alcohol in the presence of halogen;
b) quenching the reaction of step a) by adding control agent.

8. The controlled process for preparing magnesium alkoxide as claimed in. claim 7, wherein the control agent is selected from the group consisting of water or aqueous solution of NaOH or their mixture in any other solvent.
9. A process for controlling the magnesium alkoxide synthesis comprising:

a) reacting magnesium with alcohol in the optional presence of halogen or any halogen containing compound in a precursor synthesis reactor;
b) detecting the increase in pressure in the reaction of step a) in the precursor synthesis reactor;
c) transmitting information of increase in pressure to control valve through pressure transmitters from pressure sensor to control valve;
d) quenching the reaction of step a) by releasing control agent from the control agent tank through the control valve into the precursor synthesis reactor,

10. The process for controlling the reaction of magnesium alkoxide synthesis as claimed in claim 7, wherein the control agent is selected from the group consisting of water or aqueous solution of NaOH or their mixture in any other solvent.
11. A reaction control system as claimed in claim I whenever used in the controlled synthesis of magnesium alkoxide.
12. A reaction control system substantially as herein described in the specification and accompanying drawings.
13. A controlled process for preparing magnesium alkoxide substantially as herein described in the specification and accompanying drawings.
14. A process for controlling the reaction of magnesium alkoxide synthesis substantially as herein described in the specification and accompanying drawings.