FORM-2
THE PATENTS ACT, 1970
(39 OF 1970)
PROVISIONAL SPECIFICATION (SEE SECTION 10)
Title of invention: A PROCESS FOR THE PREPERATION OF SODIUM FORMATE


Name and address of applicant:
SAJJAN INDIA LIMITED Matulya Centre, #2 Ground floor,
Senapati Bapat Marg, Lower Parel,
Mumbai- 400013, Maharashtra, India.

Following specification particularly describes the nature of invention and the manner, in which it is to be performed.


PREPERATION OF AZOXY
Field of Invention
The present invention relates to the process for the preparation of Sodium Formate and more particularly from the effluent of 2,2' Dichloroazoxybenzene/2,2' Dimethylazoxybenzene.
Prior Art
In order to prepare Sodium Formate there are three known processes of which one is not a commercial process and is performed generally in the laboratory {please detail the process (b) it is incompletej.The commonality in all the three methods for the production of Sodium Formate is that all of them are a threat to human life directly and also in directly as the effluent or discharge thereof is highly toxic. One of the methods of preparing Sodium Formate is by heating of carbon monoxide along with sodium hydroxide solid under pressure the effluent is discharged. The presence and use of carbon monoxide in the process is a health hazard not only to the life of humans but also the environment. In order to use this process special care needs to be taken of the carbon monoxide as the same is highly combustible i.e. causing it to easily explode when in contact with oxygen, thereby easily burning with a violent flame. It is also known that carbon monoxide is highly toxic and has an affinity to blood which i.e. the absorption of the carbon monoxide by the hemoglobin present in the blood is atleast 200 times more than Oxygen. Besides the additional care that is required to use Carbon Monoxide and the prevent any untoward incident on account of its use, the use of the highly inflammable Carbon Monoxide is under pressure in this method for preparing Sodium Formate makes it more dangerous as it
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enhances the possibilities of an explosion. The effluent that is discharged poses harm to the environment and requires special treatment thereby adding the costs to the production of Sodium Formate.
In another process by which Sodium Formate can be prepared requires the that Pentaerythritol is manufactured by reacting acetaldehyde with an excess of formaldehyde in alkaline medium wherein the by product is Sodium Formate. In order to get Sodium Formate from this process, the residual liquid or aqueous solution left from the preparation of Pentaerythritol is to be treated i.e. it requires to be neutralized by using formic acid and sodium carbonate. This method has two primary draw backs i.e. (i) it is necessary to produce Pentaerythritol and (ii) that after the Sodium Formate is recovered, the effluent or residual aqueous solution is sodium chloride and water and cannot be discharged into environment without special treatment as the same is harmful and dangerous to plant and animal life, thereby causing this method to be expensive and not commercially viable.
There is also another method which is used commercially for preparing Sodium Formate and requires the reacting of chloroform with an alcoholic solution of sodium hydroxide or by reacting sodium hydroxide with chloral hydrate. This method, for the production of Sodium Formate requires to cause the reaction of the ingredients under extreme conditions i.e. requiring immense pressure and heat. The primary draw back for using this process is that on account of causing all the ingredients to react for producing Sodium Formate extreme pressure and heat is required thereby enhancing the risk of the blowing up of the equipment thereby posing a danger to the life of those taking part in the preparation thereof.
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BRIEF SUMMARY OF THE INVENTION
The above and other objects of the present invention are achieved by non use of Carbon Monoxide and extreme pressures and more particularly from the effluent that is discharges from the process of 2'2 Dichloroazoxybenzene/2'2 Dimethaylazoxybenzene.
The present invention provides for the commercial production of Sodium Formate from Orthonitrochlorobenzene (ONCB) or Orthonitrotoluene (ONT) by treating the residual aqueous solution of alkaline water comprising of 2'2 Dichloroazoxybenzene/2'2 Dimethaylazoxybenezene.
Another object of this invention is to provide a method for the production of Sodium Formate by using less raw material, energy and other resources and prevent any threat or harm to human life and hazardous substances being introduced into the environment.
The novelty in the present process is that the Sodium Hydroxide (NaOH) can be recovered and be reused in the initial part of the process.
In order to achieve the above objects for the preparation of Sodium Formate, either Orthonitrochlorobenzene (ONCB) or Orthonitrotoluene (ONT) is used. Either one of the main ingredients i.e. Orthonitrochlorobenzene (ONCB) or Orthonitrotoluene (ONT) are reacted with Sodium Hydroxide and mixed with water to dilute the mixture/solution. To this solution dichlone is charged and thereafter formaldehyde is added. During the process heat is kept constant and so is agitation. On completion of the reaction an aqueous solution of alkaline water comprising of 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene will be left (2'2
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Dichloroazoxybenzene is present when Orthonitrochlorobenzene (ONCB) is used, while 2'2 Dimethylazoxybenzene is present when Orthonitrotoluene (ONT) is used). The aqueous solution will be allowed to cool for filtering and separating the alkaline water from 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene. In the alternative the aqueous solution may also be heated to separate the organic layer from the alkaline water. The result depending on the main ingredient used would either be 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene, while the alkaline water would be separated. 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene is now ready for being used for the production of 2'2 Dichlorohydrazobenzene/2'2Dimethylhydrazobenzene.
In order to get a better quality of Sodium Formate the alkaline water is treated filtered or clarified with or without the use of carbon or is filtered by using a filtration oxide such as silicon dioxide or silicon oxide. Sodium Formate may also be obtained from the alkaline water by using the process of either crystallization or isolation but using the process distillation of the alkaline water is necessary so that Sodium Formate, Sodium Hydroxide (NaOH) solution and distilled water is derived and used to prepare 2'2 Dichloroazoxybenzene (used for the first step). In order to increase the quantity and concentration of Sodium Hydroxide (NaOH) maximum distillation is required whereby maximum water is removed or evaporated.
After distillation the reaction mass is cooled and Sodium Hydroxide (NaOH) and Sodium Formate are filtered in an Agitator Pressure Nutche Filter & Dryer (APND) which is made of MS/SS jacketed vessel thereby separating the two i.e. Sodium Formate and Sodium Hydroxide. In order to remove impurities Sodium Formate shall be washed with little quantity of any organic solvent, will be recovered by distillation.
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DETAILED DESCRIPTION OF THE INVENTION
The present invention now will be described more fully and particularly hereinafter.
STEP1
A MS/SS jacketed vessel with agitator is taken, in which Orthonitrochlorobenzene (ONCB) or Orthonitrotoluene (ONT) is introduced at temperatures varying between 17°C to 40°C. After the introduction of the Orthonirrochlorobenzene (ONCB) or Orthonitrotoluene (ONT), Sodium Hydroxide 48% will be charged. After all these ingredients are together the temperature of the MS/SS jacketed vessel is increased by 1°C to 25°C depending on the temperature at which the process was initiated. While increasing the temperature water is added to formation a mixture/solution and to also reduce the concentration of all the ingredients by 16% to 20% Pursuant to which Dichlone is added. On reaching the desired temperature between 20°C to 55°C Formaldehyde is added while maintaining the temperature constant for a period of 1.5 hours to 4 hours. Throughout the process the agitation and heating continues. On completion of the reaction an aqueous solution of alkaline water comprising of 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene is formed. The aqueous solution will be allowed to cool between 17°C to 40°C and on reaching the desired temperature the aqueous solution is settled or filtered whereby the alkaline water is separated from 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene. In the alternative the aqueous solution may also be heated between 55°C to 70°C to separate the organic layer of 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenezene from the alkaline water. The separation enables 2'2 Dichloroazoxybenzene/2'2
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Dimethylazoxybenezcne and alkaline water to be separate enabling 2'2 Dichloroazoxybenzene / 2'2 Dimethylbenezene to be ready for being used in production of 2'2 Dichlorohydrazobenzene /2'2 Dimethylhydrazobenzene.
STEP 2
The removal of 2'2 Dichloroazoxybenzene/2'2 Dimethylbenzene from the
aqueous solution as mentioned in the above step leaves behind the alkaline
water, it is from this alkaline water that Sodium Formate is procured. In
order to extract the Sodium Formate from the alkaline water five methods
can be used i.e. carbon treatment, clarification, filtration, crystallization /
isolation and distillation. For carbon treatment a small quantity of carbon is
required to treat the alkaline water so that the same is neutralized to
separate the Sodium Formate from the alkaline water. The alkaline water
can also be clarified (without carbon or filtration.) or may be filtered using
filtration mediums like silicon oxide or silicon dioxide. In the alternative the
process of crystallization or isolation may also be used to produce Sodium
Formate from the alkaline water. All these methods used do not cause the
recovery of Sodium Hydroxide and are expensive as they would either
require chilling (cooling) or isolation (introduction of other chemical), hence
in order to be able to procure Sodium Formate; and also 10% to 15% of
Sodium Hydroxide the best procedure is to distil the alkaline water thereby
causing the Sodium Formate of purity ranging between 98% to 99.5% is
recovered and also 10% to 15% of Sodium Hydroxide is recovered along
with water, both of which are reused in the initial stages to prepare 2'2
Dichloroazoxybenzene/2'2 Dimethylazoxybenzerie. In order to increase the
quantity and concentration of Sodium Hydroxide maximum distillation is
required whereby maximum water is removed or evaporated.
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STEP 3
After the process of distillation of the alkaline water the reaction mass/solution is cooled to 15°C to 25°C and filtered in an Agitator Pressure Nutche Filter & Dryer (APND) which is made of MS/SS jacketed vessel thereby separating the Sodium Formate and Sodium Hydroxide. To remove the impurities from the Sodium Formate, the Sodium Formate is washed with little quantity of any organic solvent (isopropyle alcohol, ethanol, ether, methanol, acetone, water) etc. The Sodium Formate is washed with an organic solvent and thereafter distilled in order to procure solid white crystalline material of Sodium Formate which is then removed form the vessel ad dried.
DIAGRAM
PREPARATION OF 2,2'-DICHLORO AZOXYBENZENE

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PREPARATION OF 2,2'-DIMETHYL AZOXYBENZENE

The typical example given below to describe the invention do not limit compositional ranges covered under the ambit and scope of the present invention only.
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EXAMPLE
STEP1
A round bottom flask with an agitator is taken in which either 3500 gms of
Orthonitrochlorobenzene (ONCB) or Orthonitrotoluene (ONT) is charged at temperatures varying between 17°C to 40°C. To the ONCB or ONT, 3400 gms of Sodium Hydroxide 48% is added. The temperature of round bottom flask is raised between 1°C to 25°C and 6700 ml of is added. While the temperature is being increased the mixture is constantly agitated. The contents or the reaction mass in the round bottom flask is diluted to be maintained between 16% to 20%, after which 15 gms of Dichlone is added. When the desired temperature is reached between 20°C to 55°C, 2390 gms of Formaldehyde is added while maintaining the temperature constant for a period of 1.5 hours to 4 hours. Throughout the process the agitation and heating continues. The reaction mass or solution is formed is alkaline water consisting of 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene. The alkaline water is allowed to cool between 17°C to 40°C and is settled, and therefrom 2'2 Dichloroazoxybenzene / 2'2 Dimethylazoxybenzene is recovered by filteration. In the alternative the aqueous solution may also be heated between 55°C to 70°C to separate the organic layer of 2'2 Dichloroazoxybenzene / 2'2 Dimethylazoxybenezene from the alkaline water. The recovered 2'2 Dichloroazoxybenzene / 2'2 Dimethylazoxybenezene is rea'dy to be used for preparing 2'2 Dichlorohydrazobenzene / 2'2 Dimethylhydrazobenzene.
STEP 2
From the alkaline water left behind from the aforementioned step contains Sodium Formate. In order to extract the Sodium Formate from the alkaline water five methods can be used i.e. carbon treatment, clarification, filtration,
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crystallization / isolation and distillation. All these methods used do not cause the recovery of Sodium Hydroxide and are expensive as they would either require chilling (cooling) or isolation (introduction of other chemical), hence the best method to procure Sodium Formate and also 10% to 15% of Sodium Hydroxide is to distil the alkaline water thereby causing the Sodium Formate of purity ranging between 98% to 99.5% is recovered and also 10% to 15% of Sodium Hydroxide is recovered along with water, both of which are reused in the initial stages to prepare 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene. Maximum distillation causes a larger and concentrated quality of Sodium Hydroxide to be recovered.
STEP 3
After the process of distillation of the alkaline water the reaction mass is cooled between 15°C to 25°C and is thereafter filtered into another vessel comprising of an agitator pressure nutche filter whereby the Sodium Formate and Sodium Hydroxide are seprated and dried. To remove the impurities from the Sodium Formate, the same is washed with a little quantity of any organic solvent (isopropyle alcohol, ethanol, ether, methanol, acetone, water) etc. The Sodium Formate washed with the organic solvent is again distilled in order to procure, Sodium Formate in the form of solid white crystalline material which is then removed and dried.
Variations
Yield is 800-850 grams of Sodium Formate having purity between 98% to 99.5% and also 200-250 grams of Sodium Hydroxide having a purity which ranges bel5% to 20% of Sodium Hydroxide.
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This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
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We Claim, :
1. A process for the preparation of Sodium Formate, either from
Orthonitrochlorobenzene (ONCB) or Orthonitrotoluene (ONT), comprising
the following steps, reacted with Sodium Hydroxide and mixed with water
to dilute the mixture/solution, to this solution dichlone is charged and
formaldehyde is added, during the process heat is kept constant under
agitation, on completion of the reaction an aqueous solution of alkaline
water containing of 2'2 Dichloroazoxybenzene/2'2 Dimethylazoxybenzene
will be left (2'2 Dichloroazoxybenzene is present when
Orthonitrochlorobenzene (ONCB) is used, while 2'2 Dimethylazoxybenzene
is present when Orthonitrotoluene (ONT) is used),the aqueous solution will
be allowed to cool for filtering and separating the alkaline water from 2'2
Dichloroazoxybenzene/2'2 Dimethylazoxybenzene, in the alternative the
aqueous solution heated to separate the organic layer from the alkaline
water, the resultant mixture 2'2 Dichloroazoxybenzene/2'2
Dimethylazoxybenzene, be separated. 2'2 Dichloroazoxybenzene/2'2
Dimethylazoxybenzene is now ready for being used for the production of
2'2 Dichlorohydrazobenzene/2'2 Dimethylhydrazobenezene.
2. Sodium Formate the alkaline water is treated filtered or clarified with or
without the use of carbon or is filtered by using a filtration oxide such as
silicon dioxide or silicon oxide. Sodium Formate obtained from the alkaline
water by using the process of either crystallization or isolation but using the
process distillation of the alkaline water is necessary so that Sodium
Formate, Sodium Hydroxide (NaOH) solution and distilled water is derived
and used to prepare 2'2 Dichloroazoxybenzene (used for the first step). In
order to increase the quantity and concentration of Sodium Hydroxide
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(NaOH) maximum distillation is required whereby maximum water is removed or evaporated.
3. After distillation the reaction mass is cooled and Sodium Hydroxide (NaOH) and Sodium Formate are filtered in an Agitator Pressure Nutche Filter & Dryer (APND) which is made of MS/SS jacketed vessel thereby separating the two i.e. Sodium Formate and Sodium Hydroxide. In order to remove impurities Sodium Formate shall be washed with little quantity of any organic solvent, will be recovered by distillation.
4. A process for the preparation of Sodium Formate such as here in described with reference to an examples.
Dated this 21st day of November, 2008
To:
The Controller of Patent, The Patent Office, at Mumbai.

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for SAJJAN INDIA LIMITED

Director