Title of Invention

"A PROCESS FOR PREPARATION OF GRANULATED ETHYLENE ABSORBENT COMPOSITION"

Abstract "A process for preparation of granulated ethylene absorbent composition" This invention relates to a process for preparation of granulated ethylene absorbent composition comprising of 20 to 50 wt % of limestone powder, 25 to 35 wt % of white cement and 5 to 20 wt % of calcium sulphate wherein the process steps comprising of granulation step is carried by dry mixing of inert matrix as herein described, extrusion step is carried by known method to form beadlets, control moisturisation step is controlled between 0-30%, curing step is carried at ambient temperature of 30 to 36°C for about 24 hours, final controlled moisturisation step.
Full Text TITLE OF THE INVENTION
A process for preparation of granulated ethylene absorbent/a**d products t-feererrf.
FIELD OF THE INVENTION
The present invention relates to an ethylene absorbent, particularly, this invention relates to an ethylene absorbent, and to the process of preparation and products thereof. More particularly, this invention relates to the process of preparation of granulated ethylene absorbent and products thereof, for increasing the shelflife of fruits, vegetables, processed foodstuffs and like, and to the packaging thereof.
BACKGROUND OF THE INVENTION
The preservation of fruits, vegetables, fishes, meats, processed foodstuffs and like products to extend their shelf life of importance. Microorganisms, bacteria, eumycetes mold and insects grow in the presence of oxygen and cause deterioration of food and foodstuffs etc. The reductive substances, generally, cause discoloration or malfunction due to their oxidation which also takes place in the presence of oxygen.
Oxygen }Ls absorbed from atmospheric air, and hence atmospheric oxygen plays an important role in metabolic activity of respiring bodies like fresh fruits and vegetables. The fruits on exposure to air, and hence oxygen, get overripe within a short period and this over-ripening decreases their value as a commodity. Similarly, the vegetables, fishes etc. get moldy or rotten, on exposure to air, and hence their value as commodity is also reduced.
The over ripening of fruits, vegetables and food stuffs particularly of fruits is promoted by ethylene, which in turn is produced by biosynthesis on the absorption of oxygen from atmospheric air.
Reduction in oxygen concentration has been observed to extend the shelf life of fruits, vegetables, food, foodstudds and like, as it results in reduced biosynthesis thereby restricting the formation of ethylene leading towards ripening/ageing of the fruits and vegetables etc. In cases of oxidation susceptible processed foods, oxidative deterioration leads towards discolouration and off-flavour development which are not desirable from aesthetic and nutritional point of view.
Therefore, the reduced concentration of oxygen can restrict or prevent these deteriorative changes, such as oxidation of oils of food and food stuffs, particularly proliferation of fungi, bacteria and insects etc., more particularly over—ripening of fruits and vegetables etc. and extend the shelf like of fruits, vegetables, fishes, foods and processed food stuffs and like.
Various means, such as, cold storage, freeze storage, refrigeration, vacuum packaging, inert gas purging methods and/or use of insecticidals, fungicidals and food additives like antioxidants etc. to protect such damages to foods and foodstuffs and thus to enhance the shelflife of foods and food stuffs have been proposed in the prior art. In order to protect fruits etc. from over—ripening, they are generally stored in cold storages at a tempera^ture of about O'C, particularly they are stored in gas cold storages at about O'C temperature. The ordinary cold storages help in preservation for short—term and gas cold storages help in preservation for longer duration. The storage of fruits at O'C helps in preserving their freshness by keeping them in suspended animation. A
major disadvantage of storing the fruits in ordinary cold storage at O'C temperature is that it requires for selected huge space, heavy machinery in addition to increasing the cost of the commodity. Gas cold storage further adds to the cost of commodity. Yet another disadvantage of storing fruits in ordinary cold storage or gas cold storage at O'C temperature is that during transportation from one place to another place, which generXally is of sufficiently longer period, particularly in case of fruits and foodstuffs and during display of such commodities in sales, it is neither feasible nor practicable to keep them at the temperature of O'C. If by any menas they are stored at this temperature, this would be unaffordable from economical point of view.
The use of insecticides and fungicides is also limited, due to their high toxicity even to human beings. The use of food additives, like the antioxidants etc. is also controversial now a days, due to their recently noticed adverse effects on human beings.
Vacuum packaging for total elimination of air, and hence of oxygen, from the atmosphere of containers and bags carrying food and foodstuffs is extremely difficult
and highly expensive. The total sealing of the containers and bags to create vacuum or to replace air by an inert gas like nitrogen, is practically not feasible. A major disadvantage of vacuum packaging or inert gas purging method is that the complete elimination of air or replacement of air by inert gas respectively, is not feasible because of the permeability of packing sheets.
Various oxygen scrubbers are known in the prior art for absorption of oxygen. Such known oxygen scrubbers are generally ascorbic acid and/or salts of ascorbic acid based, enzyme catalysed, palladium based or iron based.
Ascorbic acid and/or ascorbic acid salt based oxygen scrubbers have a major disadvantage of having poor flowability, which limits their packaging by automatic machines, and further such scrubbers are uneconomical as during sealing, part of such scrubber is adhered to the sealed portion of the packagings. Enzyme catalysed oxygen scrubber comprises of glucose oxidase and catalase enzymes. Glucose oxidase oxidises glucose to gluconic acid and hydrogen peroxide and the catalase dissociates hydrogen peroxide. The disadvantage of such oxygen scrubber is the requirement of glucose oxidase and catalase enzymes, which are costlier and

hence make the product expensive, and further the stability of enzymes is suspected without immobilisation, which is a highly specialised area where high capitals investments are required. Therefore, the enzyme catalysed oxygen scrubbers could not be used widely.
Palladium based oxygen scrubbers have disadvantages of requirement of filling of hydrogen gas. At least 8% of hydrogen gas is required to be filled in the pack. The major disadvantage of requirement of hydrogen is that, the hydrogen gas is highly inflammable and explosive in nature.
Iron based oxygen scrubber known in the prior art, generally comprises of iron in powder form, which results in poor flowability of such scrubbers and hence the disadvantage of ascorbic acid based oxygen scrubbers as described herein above.
In addition, iron based oxygen scrubbers comprising of iron in powder form have risk of leakage of iron from the pack/sachet, if the seal of later is broken while in use. This leakage of iron powder and of any such oxygen scrubber increases the risk of poisoning of food and food stuffs with such oxygen scrubber, arid hence limiting the use of such scrubber, particularly in powder form.
In order to overcome, the disadvantages of powder form oxygen scrubbers, an attempt has been made to granulate the oxygen scrubber to use them in tablet form.
The particulate or granular form of oxygen scrubbers as known in the prior art are generally prepared by blending granulation or extruding granulation or fluidized bed granulation or rolling granulation or stirring granulation or grinding granulation technique, which in-turn calls for heavy machinery and hence again making the process uneconomical and complicated.
The granular form of oxygen scrubbers are generally used after coating. Such coating calls for covering the part or whole of the particulate or granular oxygen scrubber with fine particles of coating material, which in turn is required to be carried out in S-shaped blender or V-shaped

blender or coating pan or concrete mixer. This requirement again makes the product expensive and process inconvenient.
A further disadvantage of such coating requirement is that, the particle size of coating materials is required to be controlled precisely.
Another drawback of such known oxygen scrubbers is that, generally they comprise of a filler, such as activated carbon or carbon black etc., which in turn necessitates the use of binder in order to convert the powder form of oxygen scrubber into granular form.
The disadvantage of using the binder as one of the constituent in known oxygen scrubbers is that, it (binder) lowers the oxygen absorbing property of the oxygen scrubber.
The packaging of oxygen scrubber is also essential, as its exposure to air or oxygen will result in utility of the oxygen scrubber itself before it is really required to be used or being used.
The known packaging techniques and packages are generally uneconomical and further requires high class of instrumentation.
In addition to the disadvantages/drawbacks of oxygen scrubbers, as stated above, the another major drawback of all such known oxygen scrubbers is that, the oxygen is not completely eliminated or removed from the pack or surrounding of the fruits etc.
Further major disadvantage of known oxygen scrubbers is that, their packs are not completely (100%) impermeable to the air, that is oxygen.
Therefore, at least some percentage of oxygen is always present in the surrounding atmosphere of the fruits etc. This even small percentage (2% to 8% ) of oxygen helps in the biosynthesis process of fruits, which in turn helps in production of ethylene, as stated herein above. This production of ethylene helps in ripenning, particularly over riperming of the fruits and once such process initiates this continues then on its own and spreads to the surrounding fruits also and thus spoiling other adjoining fruits etc and in-turn reducing the value of the commodity, as described herein above.
Such disadvantages/drawbacks as described herein above of such means to reduce the percentage of oxygen (which are also present in some of the known ethylene scrubbers) in order to avoid biosynthesis of fruits etc, in turn to avoid production of ethylene, further in turn to avoid overrfipenning of fruits etc and still further in turn to protect the freshness of fruits etc . till they reach to real consumers, necessitates the requirement of ethylene scrubber in addition to oxygen scrubbers or as substitute to oxygen scrubber.
The ethylene scrubbers as known in the prior art, generally comprises of active absorbing means, incorporated in the active matrix.
The active matrix, as stated herein above, known in the prior art, of such known ethylene scrubbers generally comprise of perlite, cedelite, vermiculite and/or zeolite, which are not only active in nature but also very expensive.
Another drawback of such known active matrices is that they have poor granulation which in turn reduces the surface area and hence the rate of absorption of ethylene.
•Still another drawback of such known active matrices is that they have poor porosity which also adversely effect the absorption of ethylene.
A further drawback of such known active matrices of ethylene scrubber is their poor shelf stability due to their active nature.
Still further disadvantage of the known active matrices of known ethylene scrubbers is that, they are generally not firm, so during packing, these get convert to powder form which in-turn has the disadvantages of their own, as stated herein above.
A main object of this invention to propose an ethylene scrubber, which is prepared in the granular form and eliminates all disadvantages of ethylene scrubbers comprising of active matrices by eliminating the active matrices and proposing for ethylene scrubbers comprising of inert matrices.
A further an object of this invention to propose for an ethylene scrubber, which has higher porosity, shelf stability and is firm and comprises of granular form.
A further object of this invention is to propose an ethylene scrubber which can overcome the disadvantage of powder form scrubbers, such as of poor flowability, wastage during packaging, leakage on sudden breakage of seal of pack etc.
A further an object of this invention is to propose a disclosure of the process of preparation of the proposed ethylene scrubber which can be prepared even at very low energy input with minimum infrastructure.
Another object of the present invention is to propose? an ethylene scrubber, which is free from filler and binder, and hence free from the disadyvantages of use of fillers and binders which in turn are responsible to reduce the oxygen/ethylene absorption capability.
A further object of this invention is to propose an ethylene scrubber which does not require any coating material and hence eliminates the disadvantages of the requirement of the coating material, as described herein above.
Another object of the present invention is to propose an ethylene scrubber and of the process for preparation thereof, which are convenient to be prepared and are highly economical.
Still another object of this invention is to propose an ethylene scrubber and process of preparation and product thereof, which in-turn does not need heavy machinery.
BRIEF DESCRIPTION AND PREFERRED EMBODIMENTS OF THE INVENTION
BRIEF DESCRIPTION AND PREFERRED EMBODIMENTS OF THE INVENTION
According to the present invention there is provided a process for preparation of granulated ethylene absorbent composition comprising of 20 to 50 wt % of limestone powder, 25 to 35 wt % of white cement and 5 to 20 wt % of calcium sulphate wherein the process steps comprising of:
i) granulation step is carried by dry mixing of inert matrix
as herein described, ii) extrusion step is carried by known method to form
beadlets,
iii) control moisturisation step is controlled between 0-30%, iv) curing step is carried at ambient temperature of 30 to
36°C for about 24 hours, v) final controlled moisturisation step.
According to the preferred embodiment of the present invention the active absorbing means is selected from permagnate salt, more particularly, potassium permagnate and present in the amount of 1 to 10 wt%.
According to the preferred embodiment of the present invention the inert matrix comprises of:
i) limestone powder
ii) alumina oxide
iii) white cement and
iv) calcium sulphate.
In accordance to the preferred embodiment of the present invention the limestone powder is of a grade having 16-80 mesh and specific gravity and is taken
between 2O to 5O wt7., alumina oxide is taken between 25 to 45 wt%, white cement is taken between 15 to 35 wt% and calcium sulphate is taken between 5 to 2O wtX.
According to one of the preferred embodiments of this invention the granulation step is characterised by dry-mixing of ingradients of inert matrix followed by controlled moisturisation.
The extrusion step, in accordance to the preferred embodiment of this invention is done by any such conventional means to form the beadlets.
According to the most preferred embodiment of the presently disclosed process of this invention curing is carried out after covering the inert matrix and is carried out at ambient temperature for about 24 hours.
In accordance to the preferred embodiment of the present invention the ethylene scrubber prepared in accordance to the preferred embodiments of the present invention definitely has the advantage of good porosity,
good shelf-stability, good granulation and good firmness.

DETAILED DESCRIPTION OF THE INVENTION
Accordingly, the present invention makes a complete disclosure of an ethylene absorbent, particularly, of an ethylene absorbent, and to the process of preparation and products thereof. More particularly, this invention makes a complete disclosure of the process of preparation of an ethylene absorbent and products thereof, for increasing the shelflife of fruits, vegetables, processed foodstuffs and like particularly of fruits which primarily comprises of an active absorbing means and an inert absorbing means and is prepared in accordance to the process of the present invention which in turn primarily comprises of following steps:-
i) granulation step
ii) extrusion step
iii) control moisturisation step
iv) curing step
v) final controlled moisturisation step
The controlled moisturisation, in accordance to the preferred embodiment of this invention is carried out by addition of about 3OO to 4OO ml of water per kg wt of total inert matrix and the moisturisation is controlled between 25-3OX.
The moisturisation in step (iii), as stated above is ccontrolled between 15 to 2O%, essentially above 15%.
According to the most preferred embodiment of the presently disclosed process of this invention curing is carried out after convering the inert matrix, generated as stated above, with the impregnated active absorbing polyethylene sheet, more preferably sheet of about 3OO gaugee.
The curing step as stated above is carried out at ambient temperature preferably between 3O to 36 degree centrigrade, preferably for about 24 hours.
The moisturisation at this stage is controlled between 8 to 1O%.
This is the additional advantage of the presently disclosed process of this invention that the step (i) to

(iii), as stated herein above, require low eneffrrgy input and steps (iv) and (v) require zero energy input.
The foregoing invention is explained with specific grades and gravity of limestone, however the incorporation of limestone of other such known grades and gravities do not restrict the scope of this invention. The present invention is restricted by the following claims.




WE CLAIM;
1. A process for preparation of granulated ethylene absorbent composition comprising of 20 to 50 wt % of limestone powder, 25 to 35 wt % of white cement and 5 to 20 wt % of calcium sulphate wherein the process steps comprising of:
i) granulation step is carried by dry mixing of inert matrix
as herein described, ii) extrusion step is carried by known method to form
beadlets,
iii) control moisturisation step is controlled between 0-30%, iv) curing step is carried at ambient temperature of 30 to
36°C for about 24 hours, v) final controlled moisturisation step.
2. A process as claimed in claim 1 wherein said moisturation is
carried out by addition of about 300 to 400 ml of water per kg wt of
inert matrix.
3. A process as claimed in claim 1 wherein said moisturisation in said
step (iii) is maintained between 15 to 20%.
4. A process as claimed in claim 1 wherein curing is carried out after
covering the said inert matrix impregnated with active absorbing
polyethylene sheet, more preferably sheet of about 300 gauge.
5. A process as claimed in claim 1 wherein said moisturisation is
controlled between 8 to 10%.
6. 6. A process for preparation granulated ethylene absorbent as claimed in preceeding claims and described herein above.

Documents:

620-del-1997-abstract.pdf

620-del-1997-claims.pdf

620-DEL-1997-Correspondence-Others-(19-08-2010).pdf

620-del-1997-correspondence-others.pdf

620-del-1997-correspondence-po.pdf

620-del-1997-description (complete).pdf

620-del-1997-form-1.pdf

620-DEL-1997-Form-15-(19-08-2010).pdf

620-del-1997-form-19.pdf

620-del-1997-form-2.pdf

620-del-1997-form-3.pdf

620-del-1997-gpa.pdf


Patent Number 217735
Indian Patent Application Number 620/DEL/1997
PG Journal Number 17/2008
Publication Date 25-Apr-2008
Grant Date 28-Mar-2008
Date of Filing 12-Mar-1997
Name of Patentee CHIEF CONTROLLER RESEARCH AND DEVELOPMENT
Applicant Address MINISTRY OF DEFENCE, GOVERNMENT OF INDIA, TECHNICAL COORDINATION DTE. B - 341 SENA BHAWAN DHQ P.O., NEW DELHI : 110011
Inventors:
# Inventor's Name Inventor's Address
1 BYADARAHALLI LAKKEGOWDA MOHAN KUMAR TECHNICAL COORDINATION DTE. B - 341 SENA BHAWAN DHQ P.O., NEW DELHI : 110011
2 KAVERIPATTINAM SUNDARARAMAN JAYARAMAN TECHNICAL COORDINATION DTE. B - 341 SENA BHAWAN DHQ P.O., NEW DELHI : 110011
3 PAKALAPATI SRINIVAS RAJU TECHNICAL COORDINATION DTE. B - 341 SENA BHAWAN DHQ P.O., NEW DELHI : 110011
PCT International Classification Number A23L 3/3598
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA