Indian Patents. 194454:"AN IMPROVED PROCESS FOR THE MANUFACTURE OF ACETIC ACID FROM ETHYL LACOHOL USING NOVEL PACKING MATERIALS"

Title of Invention	"AN IMPROVED PROCESS FOR THE MANUFACTURE OF ACETIC ACID FROM ETHYL LACOHOL USING NOVEL PACKING MATERIALS"
Abstract	There is provided an improved method for the manufacture of acetic actd by Oxidation of ethyl alcohol in the presence of bacteria of the type in a counter-current contact in a packed column characterized by the improved that the counter current contact of liquid and air/oxygen is carried out using trough shaped packing materials, made of conventional high alumina ceramic.

Full Text	Field of the invention This invention relates to an Improved process for the Manufacture of Acetic Acid from Ethyl Alcohol using a novel packing material Prior art and draw backs It is already known to produce Vinegar by bacterial oxidation of dilute Ethyl Alcohol This process is the traditional process of slow fermentation through the alcohol state to the acid stage It is also known to trickle the fermented liquid mixed with some vinegar over shavings In order to quicker the process The drawbacks of this known process are many of which mention may be made of the following a) This is a slow process taking about 12 hours for fermentation. b) It is usually earned out in a packed tower where dilute alcohol containing bacteria is fed from the top and air is injected from the bottom It is necessary to circulate the alcohol solution several times within the tower in the presence of air c) The packing material used in the tower is of conventional shape Bearl Saddles, Raschig Rings and other shaped material and in the packed column channeling takes place. d) In the conventional towers the flow pattern of liquid is mostly laminar and less significant turbulence In the invented process the flow path of the liquid is mostly turbulent and hence resistance to diffusion by liquid layer is significantly reduced which results in higher rate of mass transfer. Objects of the invention It is an object of this invention to propose an improved process for the production of acetic acid of required concentration, in the quickset possible time, by the fermentation of ethyl alcohol 2 It is another object of this invention to propose such a process where the conversion rate is higher than a conversion rate of the conventional process It is further object of this invention to propose such an improved process, which can reduce the number of recycles of alcoholic solution Yet another object of this Invention is to propose an improved packed tower, operation of which will eliminate the channeling problem faced in the conventional tower A stiil further object of this invention is to propose such a process which will eliminate the distribution plates, required in the conventional process and absorption tower These and other objects of this invention will be apparent from the following description Brief Statement of the invention Thus, according to this invention, there is provided an improved method for the manufacture of acetic acid (Vinegar) by Oxidation of ethyl alcohol in the presence of bacteria of the type bacterium aceta in a counter-current contact in a packed column characterized by the improvement, that the counter current of liquids and air/oxygen is carried out using trough shaped packing materials made of conventional high alumina ceramic In carrying out the above method plurality of the trough shaped packing materials are loosely dumped in the packing area of the tower The trough shaped packing materials are of uniform shape and size and are made of conventional ceramic material Each packing material comprises a solid bottom part and a surrounding uprising wall part The bottom part is of circular elliptical, square, rectangular or polygonal shape with corresponding surrounding uprising walls divergent from the base 3 The liquid air/oxygen contact is earned out preferably by providing vibratory motion during the contact of liquid and oxygen Further, according to the invention, there is provided a novel packing material for gas-liquid counter Gurrent contact in a packed column wherein the liquid is fed from the top and the gas Is admitted from the lower part of the tower comprising a solid bottom wall or part and corresponding surrounding uprising wall/walls, divergent from the base, As stated before the bottom wall is of circular, elliptical square, rectangular or of any regular or irregular polygonal shape It is also possible to have combination of these troughs shaped materials wherein a pair of the packing materials are joined at their bases with the uprising wall portions contra located Brief description of the accompanying drawings. This invention will now be more fully described with reference to the accompanying drawings, in which Figure 1, schematically shows a single trough shaped packing materials, Figure-2 shows a top views of Figure-1, Figure-3, shows an Isometric view of another trough shaped packing material while, Figure-4, shows a pair of trough shaped packing material of Figure-1 joined at the bases As Is well known the raschig ring Is a hollow cylinder of regular shape and size When a plurality of such rings form the packing section on a support in a packed tower, the packed portion appears somewhat to produce channels According to requirements of the size, the raschig ring are loosely dumped into the tower on the supporting screen 4 While alcohol liquor and bacteria flow downwards Oxygen flows in the counter direction from below Conversion of alcohol to dilute acetic acid due to Oxidation in presence of bacterial takes place in the packed section Distributor plates are provided for recycles of alcoholic liquor from the bottom to the top, which is all common Similarly with the bearl saddles material similar details are applicable and chances of channeling are not eliminated Detailed description of the accompanying drawings Referring to improved packing material, this is made of as a single trough shaped material or a double trough shaped material or as a plurality of troughs made as a unitary item in any required Geometrical shape such as a polygon The trough comprises a base (1) and four side walls (2) The base can be circular or elliptical or of any other suitable size or shape The side wall is-divergent from the base and is of a required short height When plurality of such packing materials are dumped in the tower, and alcoholic liquor is admitted from the top, the liquid fills the trough and over flows continuously There is continuous filling and over flowing There is therefore, better contact between alcohol and Oxygen The rate of conversion is improved and conversion time is considerably reduced Further additional advantages can be obtained if the base of the trough, instead of being flat, is provided with an up riser section The novel packing material is made in the conventional manner from conventional high alumina ceramic material using suitable moulds to the required shape and size 5 Further improved results can be obtained by providing usual vibrating means at the bottom of the packed tower Vibration diminishes channeling in the tower Also rate of conversion is enhanced since each trough acts Tike a stirred tank reactor and eliminates diffusional transfer of Oxygen The Invention will now be illustrated by the following Examples 1 Feed is 215 liters of 4% alcohol in water, product is about 219 Kg of solution containing 5% acetic acid Fermentation time is 2 rigors with vibration tn presence of trough shaped particles of size 14 diameter The tower is T" in diameter and 3 feet height Rate of air introduced is 100 Ibs/hr No liquid distributor is used 2 For same feed rates in a conventional tower without vibration, the fermentation time is 12 hours Packing material is 1/2 diameter raschig ring Height of tower 4 Ft with one liquid distributor If we vibrate the tower containing conventional packing material e g Raschig Ring, there is some improvement in the rate of conversion but not so much as in the case of a trough shaped packing material The reason is as follows In the case of raschig ring the residual time is much less than in the case of a trough and in the present case reaction time is important apart from absorption rate The troughs act as small stirred tank reactors whereas In the case of raschig ring the liquid merely passes through the cylinders 3 Tower containing 1/2" raschig ring and the tower is vibrated Fermentation time is 9 hours Height of tower 3 Ft No liquid distributor is used 6 4 Tower containing 1/2" trough shaped particles without vibration Fermentation time is 6 hours Tower diameter same (7") height 4 Ft One liquid distributor is used The reason fermentation time is less compared to raschig ring although the tower is not vibrated is because there is continuous in flow and outflow, the packing being trough shaped and this gives the necessary reaction time is the tower in cash pass In case of raschig ring there is only hold up in the pockets and to exchange occurs between the steam and hold up 7 I Claim 1) An improved method for the manufacture of acetic acid by oxidation of ethyl alcohol in the presence of bacteria of the type bacterium aceta in a counter-current contact in a packed column characterized by the improved that the counter current contact of liquids and air/Oxygen is carried out using trough shaped packing materials made of conventional high alumina ceramic 2) A method as claimed in Claim -1, wherein plurality of the trough shaped packing materials are loosely dumped in the packing area of the tower 3) A method as claimed in Claim 1 or Claim 2, wherein the trough shaped packing materials are of uniform shape and size and a re made of conventional ceramic material 4) A method as claimed in Claim 3 wherein each packing material comprises a solid bottom part and a surrounding uprising wall part 5) A method as claimed in Claim 4, wherein the bottom part is of circular, square, rectangular or polygonal shape with corresponding surrounding uprising walls divergent from the base 6) A method as claimed in claims 1 to 5 wherein the liquid air/Oxygen contact is earned out preferably by providing vibratory motion during the contact of liquid and Oxygen 8 7 A novel packing material for gas-liquid counter current contact in a packed column wherein the liquid is fed from the top and the Oxygen is admitted from the lower part of the tower comprising as solid bottom wall or part and corresponding surrounding uprising wall/walls, divergent from the base 8 A novel packing material as claimed in Claim 7 wherein the bottom wall is of circular, elliptical, square, rectangular of any regular or irregular polygonal-shape 9 9 A novel packing material as claimed in claims 7 and 8 wherein a pair of the packing materials are joined at their bases with the uprising wall portions contra located. There is provided an improved method for the manufacture of acetic actd by Oxidation of ethyl alcohol in the presence of bacteria of the type in a counter-current contact in a packed column characterized by the improved that the counter current contact of liquid and air/oxygen is carried out using trough shaped packing materials, made of conventional high alumina ceramic.

Full Text

Field of the invention
This invention relates to an Improved process for the Manufacture of Acetic Acid from Ethyl Alcohol using a novel packing material
Prior art and draw backs
It is already known to produce Vinegar by bacterial oxidation of dilute Ethyl Alcohol This process is the traditional process of slow fermentation through the alcohol state to the acid stage It is also known to trickle the fermented liquid mixed with some vinegar over shavings In order to quicker the process The drawbacks of this known process are many of which mention may be made of the following
a) This is a slow process taking about 12 hours for fermentation.
b) It is usually earned out in a packed tower where dilute alcohol containing bacteria is fed from the top and air is injected from the bottom It is necessary to circulate the alcohol solution several times within the tower in the presence of air
c) The packing material used in the tower is of conventional shape Bearl Saddles, Raschig Rings and other shaped material and in the packed column channeling takes place.
d) In the conventional towers the flow pattern of liquid is mostly laminar and less significant turbulence In the invented process the flow path of the liquid is mostly turbulent and hence resistance to diffusion by liquid layer is significantly reduced which results in higher rate of mass transfer.
Objects of the invention
It is an object of this invention to propose an improved process for the production of acetic acid of required concentration, in the quickset possible time, by the fermentation of ethyl alcohol
2

It is another object of this invention to propose such a process where the conversion rate is higher than a conversion rate of the conventional process
It is further object of this invention to propose such an improved process, which can reduce the number of recycles of alcoholic solution
Yet another object of this Invention is to propose an improved packed tower, operation of which will eliminate the channeling problem faced in the conventional tower
A stiil further object of this invention is to propose such a process which will eliminate the distribution plates, required in the conventional process and absorption tower
These and other objects of this invention will be apparent from the following description
Brief Statement of the invention
Thus, according to this invention, there is provided an improved method for the manufacture of acetic acid (Vinegar) by Oxidation of ethyl alcohol in the presence of bacteria of the type bacterium aceta in a counter-current contact in a packed column characterized by the improvement, that the counter current of liquids and air/oxygen is carried out using trough shaped packing materials made of conventional high alumina ceramic
In carrying out the above method plurality of the trough shaped packing materials are loosely dumped in the packing area of the tower
The trough shaped packing materials are of uniform shape and size and are made of conventional ceramic material
Each packing material comprises a solid bottom part and a surrounding uprising wall part
The bottom part is of circular elliptical, square, rectangular or polygonal shape with corresponding surrounding uprising walls divergent from the base
3

The liquid air/oxygen contact is earned out preferably by providing vibratory motion during the contact of liquid and oxygen
Further, according to the invention, there is provided a novel packing material for gas-liquid counter Gurrent contact in a packed column wherein the liquid is fed from the top and the gas Is admitted from the lower part of the tower comprising a solid bottom wall or part and corresponding surrounding uprising wall/walls, divergent from the base,
As stated before the bottom wall is of circular, elliptical square, rectangular or of any regular or irregular polygonal shape
It is also possible to have combination of these troughs shaped materials wherein a pair of the packing materials are joined at their bases with the uprising wall portions contra located
Brief description of the accompanying drawings.
This invention will now be more fully described with reference to the accompanying drawings, in
which
Figure 1, schematically shows a single trough shaped packing materials,
Figure-2 shows a top views of Figure-1,
Figure-3, shows an Isometric view of another trough shaped packing material while,
Figure-4, shows a pair of trough shaped packing material of Figure-1 joined at the bases
As Is well known the raschig ring Is a hollow cylinder of regular shape and size When a plurality of such rings form the packing section on a support in a packed tower, the packed portion appears somewhat to produce channels According to requirements of the size, the raschig ring are loosely dumped into the tower on the supporting screen
4

While alcohol liquor and bacteria flow downwards Oxygen flows in the counter direction from below Conversion of alcohol to dilute acetic acid due to Oxidation in presence of bacterial takes place in the packed section Distributor plates are provided for recycles of alcoholic liquor from the bottom to the top, which is all common
Similarly with the bearl saddles material similar details are applicable and chances of channeling are not eliminated
Detailed description of the accompanying drawings
Referring to improved packing material, this is made of as a single trough shaped material or a double trough shaped material or as a plurality of troughs made as a unitary item in any required Geometrical shape such as a polygon
The trough comprises a base (1) and four side walls (2)
The base can be circular or elliptical or of any other suitable size or shape The side wall is-divergent from the base and is of a required short height When plurality of such packing materials are dumped in the tower, and alcoholic liquor is admitted from the top, the liquid fills the trough and over flows continuously There is continuous filling and over flowing There is therefore, better contact between alcohol and Oxygen The rate of conversion is improved and conversion time is considerably reduced
Further additional advantages can be obtained if the base of the trough, instead of being flat, is provided with an up riser section
The novel packing material is made in the conventional manner from conventional high alumina ceramic material using suitable moulds to the required shape and size
5

Further improved results can be obtained by providing usual vibrating means at the bottom of the packed tower
Vibration diminishes channeling in the tower Also rate of conversion is enhanced since each trough acts Tike a stirred tank reactor and eliminates diffusional transfer of Oxygen
The Invention will now be illustrated by the following Examples
1 Feed is 215 liters of 4% alcohol in water, product is about 219 Kg of solution containing 5%
acetic acid
Fermentation time is 2 rigors with vibration tn presence of trough shaped particles of size 14 diameter The tower is T" in diameter and 3 feet height Rate of air introduced is 100 Ibs/hr No liquid distributor is used
2 For same feed rates in a conventional tower without vibration, the fermentation time is 12
hours Packing material is 1/2 diameter raschig ring Height of tower 4 Ft with one liquid
distributor If we vibrate the tower containing conventional packing material e g Raschig Ring, there is some improvement in the rate of conversion but not so much as in the case of a trough shaped packing material The reason is as follows
In the case of raschig ring the residual time is much less than in the case of a trough and in the present case reaction time is important apart from absorption rate The troughs act as small stirred tank reactors whereas In the case of raschig ring the liquid merely passes through the cylinders
3 Tower containing 1/2" raschig ring and the tower is vibrated Fermentation time is 9 hours
Height of tower 3 Ft No liquid distributor is used
6

4 Tower containing 1/2" trough shaped particles without vibration Fermentation time is 6 hours Tower diameter same (7") height 4 Ft One liquid distributor is used
The reason fermentation time is less compared to raschig ring although the tower is not vibrated is because there is continuous in flow and outflow, the packing being trough shaped and this gives the necessary reaction time is the tower in cash pass In case of raschig ring there is only hold up in the pockets and to exchange occurs between the steam and hold up
7

I Claim
1) An improved method for the manufacture of acetic acid by oxidation of ethyl alcohol in the presence of bacteria of the type bacterium aceta in a counter-current contact in a packed column characterized by the improved that the counter current contact of liquids and air/Oxygen is carried out using trough shaped packing materials made of conventional high alumina ceramic
2) A method as claimed in Claim -1, wherein plurality of the trough shaped packing materials are loosely dumped in the packing area of the tower
3) A method as claimed in Claim 1 or Claim 2, wherein the trough shaped packing materials are of uniform shape and size and a re made of conventional ceramic material
4) A method as claimed in Claim 3 wherein each packing material comprises a solid bottom part and a surrounding uprising wall part
5) A method as claimed in Claim 4, wherein the bottom part is of circular, square, rectangular or polygonal shape with corresponding surrounding uprising walls divergent from the base
6) A method as claimed in claims 1 to 5 wherein the liquid air/Oxygen contact is earned out preferably by providing vibratory motion during the contact of liquid and Oxygen
8

7 A novel packing material for gas-liquid counter current contact in a packed column
wherein the liquid is fed from the top and the Oxygen is admitted from the lower part of the
tower comprising as solid bottom wall or part and corresponding surrounding uprising
wall/walls, divergent from the base
8 A novel packing material as claimed in Claim 7 wherein the bottom wall is of circular,
elliptical, square, rectangular of any regular or irregular polygonal-shape
9
9 A novel packing material as claimed in claims 7 and 8 wherein a pair of the packing materials are joined at their bases with the uprising wall portions contra located.
There is provided an improved method for the manufacture of acetic actd by Oxidation of ethyl alcohol in the presence of bacteria of the type in a counter-current contact in a packed column characterized by the improved that the counter current contact of liquid and air/oxygen is carried out using trough shaped packing materials, made of conventional high alumina ceramic.

Documents:

00150-cal-1998-abstract.pdf

00150-cal-1998-claims.pdf

00150-cal-1998-correspondence.pdf

00150-cal-1998-description(complete).pdf

00150-cal-1998-drawings.pdf

00150-cal-1998-form-1.pdf

00150-cal-1998-form-2.pdf

00150-cal-1998-form-3.pdf

00150-cal-1998-pa.pdf

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Patent Number

194454

Indian Patent Application Number

150/CAL/1998

PG Journal Number

30/2009

Publication Date

24-Jul-2009

Grant Date

19-Aug-2005

Date of Filing

29-Jan-1998

Name of Patentee

DR.AMALESH SIRKAR

Applicant Address

76/A,BONDEL ROAD,CALCUTTA-700019,

Inventors:

#	Inventor's Name	Inventor's Address
1	DR.AMALESH SIRKAR	76/A,BONDEL ROAD,CALCUTTA-700019,

PCT International Classification Number

C12J 1/04

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA