Title of Invention

"A PROCESS FOR DEVELOPMENT OF PROTECTIVE COATING"

Abstract The application describes a process for preparing protective coating specifically antifungal coating from lac waste thereby reusing the waste material for value added product while simultaneously managing environmental pollution. The process comprising subjecting lac waste to sequential acidification initially at a temperature ranging from 10 to 25°C so as to achieve pH between 4 & 7, removing the solids generated, continuing acidification till pH is further reduced to 2 to 4.5, removing the solids generated, followed by cooling to a temperature in the range of 5 to 20°C and isolating the solids generated, heating the isolated solids to a temperature ranging from 75°C to 100°C recovering the solid mass by decantation, then washing with water till the mass is free from chloride or sulphate ions and suspending in lower aliphatic alcohol with 1 to 3 carbon atoms optionally along with low boiling ester or ketone, or mixture there of salting out the suspension so obtained followed by coagulating the salted mass and combining with conventional microbicidal agent to get protective coating.
Full Text FIELD OF INVENTION:
The present invention relates to a process for development of protective coating preferably anti-fungal coating from lac wastes and product thereof, particularly the present invention relates to a process for development of anti-fungal coating from seed lac, shellac, kirilac and other lac waste and product thereof, more particularly the present invention relates to a process for development of anti-fungal coating from seed lac, shellac, kirilac and other lac wastes obtained after recovery of aleuritic acid, for generating the leather gloss on leather, raxine, shoes, upholstery, sports goods, and thereof, even more particularly it relates to a process for development of anti-fungal coating from seed lac, shellac, kirilac and other lac wastes obtained after recovery of aleuritic acid from such lac, for generating the leather gloss on leather articles and product thereof.
Background of the Invention
Aleuritic acid (9,10,16- trihydroxypalmitic acid) is a very important raw material for the synthesis of intermediates for and the manufacture of industrially important musk fragrances. Many fragrance components for use in the perfume industry, such as trans delta(9) isoambrettolide and abmrete seed oil musk called abmrettolide can be prepared from aleuritic acid. Musk odour is perhaps the most universally appreciated fragrance, which has higher demand as compared to many other fragrances. The limitation of this fragrance, which has higher demand as compared to many other fragrances. The limitation of this fragrance is that, it has a low supply. Therefore, numerous attempts have been made to duplicate this musk fragrance by using synthetic reaction schemes.
One such scheme to duplicate the musk fragrance by synthetic process is by involving aleuritic acid as a starting raw material, which has led to its high demand and controlled supply. The foremost requirement of aleuritic for use in the manufacturer of perfumes is its high purity, which is the controlling factor in its acceptance in the market, being the controlling factor in the quality of the manufactured perfume.
Therefore, there had been great emphasis on production of aleuritic acid due to its great demand with special emphasis on its purity. Industrial methods have been made available for production of aleuritic acid.
One of the most commonly used method of production of aleuritic, which has replaced many known industrial methods, is by hydrolysis of lac, particularly of seed lac, shellac,kiri lac and other products, which in turn are excreted by insects Laccifera lacca Kerr (family Laccifera cockerel) on certain varieties of trees (called lac hosts) indigenous to India, Thailand and some parts of China.
Such a know method results in generation lac wastes, particularly in seed lac, shellac or kiri lac depending upon the original lac used as a raw material for production of aleuritic acid. Such lac wastes is discharged into the drain after recovery of aleuritic acid.
The development of coatings, polishes, toughening compounds, dressing agents, filters for boots, hardening and water proofing of leather and leather articles has been reported in a number of patents.
Some of these patents referred herein above, refer to the use of lac, particularly shellac as one of the raw materials either in its raw form or its purified form. None of the patents granted or applied for refers to utilize the lac wastes, which at the moment is discharged into the drain after recovery of aleuritic acid, referred herein above.
Therefore, it is obvious from the foregoing description, that there is no method which utilises the lac wastes, particularly seed lac wastes or shellac wastes for development of coatings, polishes, toughening compounds, dressing agents, filters for boots, hardening and water proofing of leather and leather articles, particularly for development of coating for generating the leather, raxine, shoes, upholstery, sports goods, more particularly of an anti-fungal coating for generating the leather gloss on leather articles.
The inventor of the presently disclosed invention has put considerable efforts in to research to develop coating, particularly anti-fungal coating for generating the leather gloss on leather, raxine, shoes, upholstery, sports goods, more particularly of an anti-fungal coating for generating the leather gloss on leather articles, from seed lac, shellac, kirilac and other lac wastes obtained after recovery of aleuritic acid.
NEED OF THE INVENTION:
Therefore, there is a need to have a process for development of anti-fungal coating from lac wastes and product thereof, particularly to have a process for development of anti-fungal coating from seed lac, shellac,kiriiac and other lac wastes and product thereof, even more particularly to have a process for the development of anti-fungal coating from seed lac, shellac, kirilac and other lac wastes obtained after recovery of aleuritic acid, for generating the leather gloss on leather, raxine, shoes, upholstery , sports goods, and product thereof, even more particularly to have a process for development of anti-fungal coating from seed lac,shellac, kirilac and other wastes obtained after recovery of aleuritic acid from such lac, for generating the leather gloss on leather articles and products thereof.
OBJECTS OF THE INVENTION:
This is the main object of the present invention to make a complete disclosure of a process for development of anti-fungal coating from lac wastes, particularly from seed lac, shellac, kirilac and other lac wastes, more particularly from seed lac wastes obtained after recovery of aleuritic acid, for generating the leather gloss on leather, raxine, shoes, upholstery, sports goods, even more particularly to have a process for development of anti-fungal coating from seed lac, wastes obtained after recovery of aleuritic acid from such lac, for generating the leather gloss on leather articles and products thereof.
Alternatively, the object of the present invention is to propose for a method for conversion of lac wastes to anti-fungal coating, more particularly for conversion of seed
lac wastes obtained after recovery of aleuritic acid to anti-fungal coating for generating the leather gloss on leather, raxine, shoes, upholstery, sports good, and products thereof.
Other objects of the present invention will become obvious from the following description.
DESCRIPTION OF THE INVENTION:
Accordingly the present invention makes a complete disclosure of a process for development of anti-fungal coating from lac wastes, particularly from seed lac, shellac, kirilac and other lac wastes, more particularly from seed lac seed lac wastes obtained after recovery of aleuritic acid, for generating the leather gloss on leather, raxine, shoes, upholstery, sports goods, even more particularly to have a process for development of anti-fungal coating from seed lac, wastes obtained after recovery of aleuritic acid from such lac, for generating the leather gloss on leather articles and products thereof, wherein the discharged liquor obtained after filtering the crude aleuritic acid from hydrolysis step is collected in a tank, which is subjected to the steps of presently disclosed method, as described herein below.
In accordance to the preferred embodiment of the presently disclosed process of the present invention, about one liter of the said discharged liquor is taken in a beaker of about 2 liters capacity and cooled to about 10 to 15°C temperature, preferably to about 5 to 10°C to this cooled liquor, an acidic solution preferably of hydrochloric acid (HCI), sulphuric acid (H 2SO4, nitric acid (HNO3) or phosphoric acid (H3PO4), more prefarably of hydrochloric acid (HCI) even more preferably of dilute hydrochloric acid (HCI), still more preferably of HC1:H2O in 1:1 ratio is added in first step.
In accordance to the preferred embodiments of this invention, in the second step of the presently disclosed process the acidified liquor is filtered to remove any solid separated at this stage of acidification. In accordance to one of the preferred embodiments of this invention the filtrate is treated with acid again, preferably with hydrochloric acid (HCI),
sulphuric acid (H2SO4), nitric acid (HNO3) or phosphoric acid (H3PO4), more prefarably of hydrochloric acid (HC1) even more preferably of dilute hydrochloric acid (HC1), still more preferably of HC1 : H2O in 1:1 ratio.
According to the preferred embodiment of this invention the acid in first stage of acidification is added till the pH of the cooled liquor is achieved at about 4 to 6 and at second stage acidification the acid is added till the pH of the filtered liquor is achieved at about 2.5 to 3.5.
In accordance to the process of the present invention, the acidified filtrate having pH of about 2.5 to 3.5 is further treated with common salt solution, preferably with saturated common salt solution and about 1 to 3% of agar-agar or alum or polyaluminium chloride (about 10-14% solution) to salt out the solid material and to coagulate any colloidal matter in the third step.
In accordance to one of the preferred embodiments of the presently disclosed invention the reacted mass from third step is heated, preferably at about 75 to 100°C, more preferably at about 80 to 90°C for a period of about 1 to 4 hrs, preferably for a period of about 2 to 2.5 hrs in the fourth step and maintained at this temperature for additional one hr. At this stage, the material is decanted hot to drain off as much water as possible. The semi-solid product obtained at this stage is first washed with hot water and then with cold water several times till it is free from chloride or sulphate ions, as the case may be, which can be tested by any known method.
According to the present invention, the semi-solid product, as refferd herein above when obtained after fourth step and after washings with hot and cold water, in accordance to the presently disclosed method, is suspended in an alcoholic medium, preferably in aqueous alcoholic medium, more preferably in aqueous method or ethanol or propanol along with about 2 to 5% of the total volume of amylacetate or chloroform or dichloromethane or any other low boiling ester or ketone to counter the smell of the lac
wastes that may persist, and heated to the boling point. The reaction mixture is kept boiling for a period of about one hr.
In accordance to one of the preferred embodiments of the presently disclosed invention the boiling reaction mixture is filtered while hot and the filtrate collected is cooled and treated through with pentachlorophenol and paranitrophenol in the final step of the presently disclosed invention, which results in the desired coating, which in turn can be applied directly or after dilution on to the leather article to give a leather gloss. In accordance to still another preferred embodiment of the present invention, the said filtrate is treated thoroughly with about 2% of pentachlorophenol and about 1% of paranitrophenol in the final step of the presently disclosed invention.
The presently disclosed invention has been described with a set of specific reaction for development of coating from lac wastes, particularly from seed lac wastes for generating leather on any leather article, which is not intended to limit the scope of the present invention. It is obvious that, a minor modification in the reaction conditions of the presently disclosed set of specific reaction is possible without deviating from the scope of the present invention.




We CLAIM:
1. A process for development of protective coating comprising the steps of:
(a) subjecting lac waste to sequential acidification initially at a temperature
ranging from 10 to 25°C so as to achieve pli between 4 & 6, filtering to remove
the solids generated, continuing acidification till pH is further reduced to 2.5 to
3.5, removing the solids generated, followed by cooling to a temperature in the
range of 10 to 15°C and isolating the solids generated, heating the isolated solids
to a temperature ranging from 75°C to 100°C recovering the solid mass by
decantation, then washing with water till the mass is free from chloride or
sulphate ions and suspending in lower aliphatic alcohol with 1 to 3 carbon atoms
optionally along with low boiling ester or ketone, or mixture there of such as
herein described,
(b) salting the suspension obtained in step (a) followed by coagulating the salted
mass and combining with conventional microbicidal agent to get protective
coating.

2. A process as claimed in claim 1 wherein lac waste used is the hydrolyscd discharged
liquor obtained after recovery of aleuritic acid.
3. A process as claimed in claim 1 wherein the sequential acidification in step (a) is
carried out employing acid selected from phosphoric acid nitric acid, sulphuric acid,
or hydrochloric acid preferably hydrochloric acid.
4. A process as claimed in preceding claims wherein the acid used is dilute acid
preferably acid to water in 1:1 ratio.
5. A process as claimed in preceding claims wherein heating in step (a) is effected at a
temperature ranging from 80°C to 90°C for a period of 1 to 4 hours preferably for 2
to 2.5 hours.
6. A process as claimed in claim 1 wherein the alcohol used in step (a) is methanol,
ethanol, propanol preferably in aqueous form optionally with low boiling ester or
ketone such as amylacetate, or chloroform or dichloromethane in an amount of 2 to
5% of the total volume.
7. A process as claimed in preceding claims wherein the salting in step (b) is
conducted by treating the suspension with common salt solution, preferably with
saturated common salt solution and about 1-3% of agar-agar or alum or
polyaluminium chloride.
8. A process as claimed in preceding claims wherein the conventional microbicidal
agents used are fungicides such as pentachlorophenol and paranitrophenol in an
amount of 2 and l%respectively.
9. A process for development of protective coating substantially as herein described.

Dated this 1lm day of May 1999.



Documents:

709-del-1999-abstract.pdf

709-del-1999-claims.pdf

709-del-1999-correspondence-others.pdf

709-del-1999-correspondence-po.pdf

709-del-1999-description (complete).pdf

709-del-1999-form-1.pdf

709-del-1999-form-13.pdf

709-del-1999-form-19.pdf

709-del-1999-form-2.pdf

709-del-1999-form-3.pdf

709-del-1999-form-5.pdf

709-del-1999-gpa.pdf


Patent Number 230547
Indian Patent Application Number 709/DEL/1999
PG Journal Number 11/2009
Publication Date 13-Mar-2009
Grant Date 27-Feb-2009
Date of Filing 11-May-1999
Name of Patentee Dean, Industrial Research And Development (DIRD)
Applicant Address INDIAN INSTITUTE OF TECHNOLOGY, DELHI, HAUZ KHAS, NEW DELHI - 110016, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 DR. RAMESH KUMAR MEHTA INDIAN INSTITUTE OF TECHNOLOGY, HAUS KHAS, NEW DELHI 110016, INDIA.
PCT International Classification Number A23B 7/022
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA