Title of Invention	PROCESS FOR THE PRODUCTION OF LIQUID FUEL FROM WASTE POLYPROPYLENE USING ACID ACTIVATED KAOLIN
Abstract	The present invention discloses a simple method for the conversion of waste polypropylene to fuel oil. A stainless steel reactor is used to convert the waste polypropylene to fuel oil in presence of an acid treated kaoline catalyst. This catalyst improves the yield of oil and increases the rate of reaction. The oil obtained in the optimum condition is a mixture of different fractions in the range of gasoline (30%) and the rest a mixture of diesel and kerosene.

Title of Invention

PROCESS FOR THE PRODUCTION OF LIQUID FUEL FROM WASTE POLYPROPYLENE USING ACID ACTIVATED KAOLIN

Abstract

The present invention discloses a simple method for the conversion of waste polypropylene to fuel oil. A stainless steel reactor is used to convert the waste polypropylene to fuel oil in presence of an acid treated kaoline catalyst. This catalyst improves the yield of oil and increases the rate of reaction. The oil obtained in the optimum condition is a mixture of different fractions in the range of gasoline (30%) and the rest a mixture of diesel and kerosene.

Full Text	STATEMENT OF INVENTION: The present invention discloses a simple method for the conversion of waste polypropylene to fuel oil. A stainless steel reactor is used to convert the waste polypropylene to fuel oil in presence of an acid treated kaoline catalyst. This catalyst improves the yield of oil and increases the rate of reaction. The oil obtained in the optimum condition is a mixture of different fractions in the range of gasoline (30%) and the rest a mixture of diesel and kerosene. BACKGROUND OF INVENTION: Plastics pyrolysis has long been topical in academic circles and also continues to inspire industrial R&D and demonstration projects. Still the pyrolysis of mixed plastics is economically to be proven because of the small scale potential pyrolysis plant and the huge cost expenditure towards collecting, cleaning, and grading considerable tonnages of plastics. In addition, the cost of catalyst, its efficiency to convert the waste plastics to fuel in terms of change of yield and rate of the reaction, and also its reusability contribute to the overall economic and ecological aspects of the process. During the past 40 years, numerous studies have been reported in which a variety of catalysts and reaction conditions have been employed to convert waste polymers into hydrocarbon mixtures. This is also reflected by a number of pilot, demonstration, and commercial plants processing various types of plastic wastes in Germany, Japan, USA, India, and elsewhere. Exhaustive patent search reveals that no patent has been filed in any country in this direction using the waste polypropylene and acid treated kaoline clay as catalyst. OBJECT OF THE INVENTION: The objective of the invention is to develop a process for conversion of waste polypropylene to liquid fuel. The basic purpose of this invention is the development of a suitable acid treated kaoline catalyst to be used to convert the waste polypropylene to enhance the rate of reaction and the oil yield. SUMMARY OF INVENTION: Waste Polypropylenes is subjected to thermal and catalytic cracking, kaoline clay and acid treated kaolines are used as catalysts for conversion of waste polypropylene to liquid fuel. The reaction is carried out in a reactor in the temperature range of 400-600°C with an objective to optimize the oil yield, optimize the amount of catalyst and the reaction time. In the catalytic pyrolysis, a mixture of catalyst and the polypropylene flakes in different proportion were subjected to pyrolysis in the reactor at a desired temperature. The highest yield of liquid product obtained is 82.85% by weight at 500°C in thermal pyrolysis. Use of kaoline as catalyst increased the yield of liquid fraction to 87.5%. Sulphuric acid treated kaoline further increased the oil yield to 93%. Study of FTIR and GC-MS confirmed the presence of different hydrocarbons (mostly alkanes and olefins) in the oil. The composition of the oil significantly narrowed in presence of kaoline catalyst and also in acid treated kaoline as compared to thermal pyrolysis. The fuel properties of the oil was also analysed to find its suitability as a petrochemical fuel substitute. Kaoline is a cheap chemical and acid treatment technique is very simple process. The catalyst used can be regenerated back for further use. So this method is simple, eco-friendly and easy to use. DRAWINGS (if any) DETAILED DESCRIPTION The present invention provides a process for the conversion of waste polypropylene to liquid fuel using suitable kaoline clay based catalyst. The different acid treated kaoline is prepared by treating kaoline with different concentration of sulphuric acid, which is used in the experiment. The kaolin clay used in this experiment is procured commercially from Chemtex Corporation, Kolkata, India. From the proximate analysis and XRD report it could be concluded that the major component of the clay is kaolinite with Hinckley index of 0.4. Some traces of impurities (may be mica, quartz and feldspar which could not be traced in the XRD report) are also present which contribute the components other than SiC^ and AI2O3. The BET surface area of kaoline was found to be 23m2/g. The pore size distributions of kaolinite samples showed a sharp peak at a radius of 3.5nm, thus it is mesoporous. The modification of kaoline using different concentration of sulphuric acid was carried out by adding 50g of the clay to 500ml of sulphuric acid solution- of different concentrations (1M, 3M, 5M) and refluxing at 110 °C under the atmospheric pressure in a round bottomed flask equipped with a reflux condenser for four hours. The resulting clay suspension was then rapidly quenched by adding 500ml ice cold water. The content was then filtered, repeatedly washed with distilled water to remove any unspent acid, dried in an oven, calcined at 500°C for one hour and ground in a mortar pastel to powder form. The untreated sample is referred to as KC and treated samples after calcination at 500°C are referred to as KC1M, KC3M, and KC5M in the subsequent text where the numbers refers to the different concentration of acid used. Another sample named KC5M 750 is obtained by calcining at 750°C after 5M acid treatment in the same process. The clay samples were characterized by using XRD, XRF, TGA, SEM, Nitrogen adsorption desorption isotherm technique, FTIR to understand the affect of acid treatments. The acid treatment of catalyst increases the Si/Al ratio, surface area and pore volume of the clay sample. The composition and properties of the different clay samples are summarised in the Table 1. The pyrolysis reaction is carried out in a stainless reactor set up. The waste polypropylene is pyrolysed in the reactor along with different clay catalyst samples using different catalyst to feed ratio (1:2,1:3,1:4,1:10,1:20,1:40) in the range of temperature of 400-600°C. The oil yield and reaction time for the pyrolysis reaction carried out using different catalysts in optimum condition is summarised in Table 2. Table 2 The'results of the pyrolysis (Temperature=500°C, Catalyst:Feed=l :3) using different types of catalysts The fuel properties of pyrolytic oil and its fractions after distillation are summarised in Table 3. The distillation report of the oil infers that oil is in the boiling range of 59- 346°C, so it is a mixture of different oil fractions in the range of gasoline (30%) and rest 70% a mixture of kerosene and diesel. The present invention is further described in the following examples. EXAMPLE 1 20g waste polypropylene when subjected to thermal pyrolysis at 500°C yield oil of 16.5g (82.5wt.%) in 58 minutes reaction time. EXAMPLE 2 20g waste polypropylene when pyrolysed using kaoline catalyst with 1:3 catalysts to polypropylene ratio at 500°C yield oil of 17.5g (87.5wt.%) in 43 minutes reaction time. EXAMPLE 3 20g waste polypropylene when pyrolysed using kaoline catalyst with 1:10 catalysts to polypropylene ratio at 500°C yield oil of 16.8g (84wt.%) in 53 minutes reaction time. EXAMPLE 4 20g waste polypropylene when pyrolysed using 1MKC catalyst with 1:3 catalysts to polypropylene ratio at 500°C yield oil of 17.5g (87.5wt.%) in 41 minutes reaction time. EXAMPLE 5 20g waste polypropylene when pyrolysed using 3MKC catalyst with 1:3 catalysts to polypropylene ratio at 500°C yield oil of 17.5g (87.5wt.%) in 41 minutes reaction time. EXAMPLE 6 20g waste polypropylene when pyrolysed using 5MKC catalyst with 1:4 catalysts to polypropylene ratio at 500°C yield oil of 18.0g (90wt%) in 42 minutes reaction time. EXAMPLE 7 20g waste polypropylene when pyrolysed using 5MKC catalyst with 1:3 catalysts to polypropylene ratio at 500°C yield oil of 18.2g (91wt%) in 39 minutes reaction time. EXAMPLE 8 The reusability of the catalyst was studied by using the used catalyst. The catalysts give almost same performance up to 4th time reuse. The oil yield decreased to 84wt.% and reaction time increased to 73 minutes with 5th time reused kaoline (at 500°C with 1:3 catalyst to polypropylene ratio). The 5th time reused kaoline is regenerated by calcining at 750°C. The regenerated catalyst yield 88wt.% oil in 45minute reaction time (at 500°C with 1:3 catalyst to polypropylene ratio). CLAIMS We claim: 1. A process for conversion of waste polypropylene to liquid fuel oil using modified kaoline clay catalyst at 400-600°C with 1:3 catalyst to feed ratio. 2. A process according to claim 1, wherein the pyrolysis process is carried out in a reactor made up of stainless steel. 3. A process according to claim 1, wherein the waste polypropylene is pyrolysed using acid treated kaoline to obtain liquid fuel. 4. A process according to claim 1, wherein the reaction time decreased (rate of reaction increased) in presence of acid treated kaoline catalyst. 5. A process according to claim 1, wherein the yield of oil was 93% by weight using 5MKC750 catalyst at 500°C with 1:3 catalyst to feed ratio. 6. A process according to claim 1, acid treated kaoline can be regenerated at 750°C after use and reused with same efficiency. 7. A process according to claim 1, wherein the distillation of the liquid oil obtained is a mixture of gasoline 30% and rest a mixture of kerosene and diesel oil. The present invention discloses a simple method for the conversion of waste polypropylene to fuel oil. A stainless steel reactor is used to convert the waste polypropylene to fuel oil in presence of an acid treated kaoline catalyst. This catalyst improves the yield of oil and increases the rate of reaction. The oil obtained in the optimum condition is a mixture of different fractions in the range of gasoline (30%) and the rest a mixture of diesel and kerosene.

Full Text

STATEMENT OF INVENTION:
The present invention discloses a simple method for the conversion of waste
polypropylene to fuel oil. A stainless steel reactor is used to convert the waste
polypropylene to fuel oil in presence of an acid treated kaoline catalyst. This catalyst
improves the yield of oil and increases the rate of reaction. The oil obtained in the
optimum condition is a mixture of different fractions in the range of gasoline (30%) and
the rest a mixture of diesel and kerosene.
BACKGROUND OF INVENTION:
Plastics pyrolysis has long been topical in academic circles and also continues to inspire
industrial R&D and demonstration projects. Still the pyrolysis of mixed plastics is
economically to be proven because of the small scale potential pyrolysis plant and the
huge cost expenditure towards collecting, cleaning, and grading considerable tonnages of
plastics. In addition, the cost of catalyst, its efficiency to convert the waste plastics to fuel
in terms of change of yield and rate of the reaction, and also its reusability contribute to
the overall economic and ecological aspects of the process. During the past 40 years,
numerous studies have been reported in which a variety of catalysts and reaction
conditions have been employed to convert waste polymers into hydrocarbon mixtures.
This is also reflected by a number of pilot, demonstration, and commercial plants
processing various types of plastic wastes in Germany, Japan, USA, India, and elsewhere.
Exhaustive patent search reveals that no patent has been filed in any country in this
direction using the waste polypropylene and acid treated kaoline clay as catalyst.
OBJECT OF THE INVENTION:
The objective of the invention is to develop a process for conversion of waste
polypropylene to liquid fuel. The basic purpose of this invention is the development of a
suitable acid treated kaoline catalyst to be used to convert the waste polypropylene to
enhance the rate of reaction and the oil yield.
SUMMARY OF INVENTION:
Waste Polypropylenes is subjected to thermal and catalytic cracking, kaoline clay and
acid treated kaolines are used as catalysts for conversion of waste polypropylene to liquid
fuel. The reaction is carried out in a reactor in the temperature range of 400-600°C with
an objective to optimize the oil yield, optimize the amount of catalyst and the reaction
time. In the catalytic pyrolysis, a mixture of catalyst and the polypropylene flakes in
different proportion were subjected to pyrolysis in the reactor at a desired temperature.
The highest yield of liquid product obtained is 82.85% by weight at 500°C in thermal
pyrolysis. Use of kaoline as catalyst increased the yield of liquid fraction to 87.5%.
Sulphuric acid treated kaoline further increased the oil yield to 93%. Study of FTIR and
GC-MS confirmed the presence of different hydrocarbons (mostly alkanes and olefins) in
the oil. The composition of the oil significantly narrowed in presence of kaoline catalyst
and also in acid treated kaoline as compared to thermal pyrolysis. The fuel properties of
the oil was also analysed to find its suitability as a petrochemical fuel substitute. Kaoline
is a cheap chemical and acid treatment technique is very simple process. The catalyst
used can be regenerated back for further use. So this method is simple, eco-friendly and
easy to use.
DRAWINGS (if any)
DETAILED DESCRIPTION
The present invention provides a process for the conversion of waste polypropylene to
liquid fuel using suitable kaoline clay based catalyst. The different acid treated kaoline is
prepared by treating kaoline with different concentration of sulphuric acid, which is used
in the experiment.
The kaolin clay used in this experiment is procured commercially from Chemtex
Corporation, Kolkata, India. From the proximate analysis and XRD report it could be
concluded that the major component of the clay is kaolinite with Hinckley index of 0.4.
Some traces of impurities (may be mica, quartz and feldspar which could not be traced in
the XRD report) are also present which contribute the components other than SiC^ and
AI2O3. The BET surface area of kaoline was found to be 23m2/g. The pore size
distributions of kaolinite samples showed a sharp peak at a radius of 3.5nm, thus it is
mesoporous.
The modification of kaoline using different concentration of sulphuric acid was carried
out by adding 50g of the clay to 500ml of sulphuric acid solution- of different
concentrations (1M, 3M, 5M) and refluxing at 110 °C under the atmospheric pressure in
a round bottomed flask equipped with a reflux condenser for four hours. The resulting
clay suspension was then rapidly quenched by adding 500ml ice cold water. The content
was then filtered, repeatedly washed with distilled water to remove any unspent acid,
dried in an oven, calcined at 500°C for one hour and ground in a mortar pastel to powder
form. The untreated sample is referred to as KC and treated samples after calcination at
500°C are referred to as KC1M, KC3M, and KC5M in the subsequent text where the
numbers refers to the different concentration of acid used. Another sample named KC5M
750 is obtained by calcining at 750°C after 5M acid treatment in the same process. The
clay samples were characterized by using XRD, XRF, TGA, SEM, Nitrogen adsorption
desorption isotherm technique, FTIR to understand the affect of acid treatments.
The acid treatment of catalyst increases the Si/Al ratio, surface area and pore volume of
the clay sample. The composition and properties of the different clay samples are
summarised in the Table 1.
The pyrolysis reaction is carried out in a stainless reactor set up. The waste
polypropylene is pyrolysed in the reactor along with different clay catalyst samples using
different catalyst to feed ratio (1:2,1:3,1:4,1:10,1:20,1:40) in the range of temperature
of 400-600°C. The oil yield and reaction time for the pyrolysis reaction carried out using
different catalysts in optimum condition is summarised in Table 2.
Table 2 The'results of the pyrolysis (Temperature=500°C, Catalyst:Feed=l :3) using
different types of catalysts
The fuel properties of pyrolytic oil and its fractions after distillation are summarised in
Table 3. The distillation report of the oil infers that oil is in the boiling range of 59-
346°C, so it is a mixture of different oil fractions in the range of gasoline (30%) and rest
70% a mixture of kerosene and diesel.
The present invention is further described in the following examples.
EXAMPLE 1
20g waste polypropylene when subjected to thermal pyrolysis at 500°C yield oil of 16.5g
(82.5wt.%) in 58 minutes reaction time.
EXAMPLE 2
20g waste polypropylene when pyrolysed using kaoline catalyst with 1:3 catalysts to
polypropylene ratio at 500°C yield oil of 17.5g (87.5wt.%) in 43 minutes reaction time.
EXAMPLE 3
20g waste polypropylene when pyrolysed using kaoline catalyst with 1:10 catalysts to
polypropylene ratio at 500°C yield oil of 16.8g (84wt.%) in 53 minutes reaction time.
EXAMPLE 4
20g waste polypropylene when pyrolysed using 1MKC catalyst with 1:3 catalysts to
polypropylene ratio at 500°C yield oil of 17.5g (87.5wt.%) in 41 minutes reaction time.
EXAMPLE 5
20g waste polypropylene when pyrolysed using 3MKC catalyst with 1:3 catalysts to
polypropylene ratio at 500°C yield oil of 17.5g (87.5wt.%) in 41 minutes reaction time.
EXAMPLE 6
20g waste polypropylene when pyrolysed using 5MKC catalyst with 1:4 catalysts to
polypropylene ratio at 500°C yield oil of 18.0g (90wt%) in 42 minutes reaction time.
EXAMPLE 7
20g waste polypropylene when pyrolysed using 5MKC catalyst with 1:3 catalysts to
polypropylene ratio at 500°C yield oil of 18.2g (91wt%) in 39 minutes reaction time.
EXAMPLE 8
The reusability of the catalyst was studied by using the used catalyst. The catalysts give
almost same performance up to 4th time reuse. The oil yield decreased to 84wt.% and
reaction time increased to 73 minutes with 5th time reused kaoline (at 500°C with 1:3
catalyst to polypropylene ratio). The 5th time reused kaoline is regenerated by calcining
at 750°C. The regenerated catalyst yield 88wt.% oil in 45minute reaction time (at 500°C
with 1:3 catalyst to polypropylene ratio).
CLAIMS
We claim:
1. A process for conversion of waste polypropylene to liquid fuel oil using
modified kaoline clay catalyst at 400-600°C with 1:3 catalyst to feed ratio.
2. A process according to claim 1, wherein the pyrolysis process is carried out in
a reactor made up of stainless steel.
3. A process according to claim 1, wherein the waste polypropylene is pyrolysed
using acid treated kaoline to obtain liquid fuel.
4. A process according to claim 1, wherein the reaction time decreased (rate of
reaction increased) in presence of acid treated kaoline catalyst.
5. A process according to claim 1, wherein the yield of oil was 93% by weight
using 5MKC750 catalyst at 500°C with 1:3 catalyst to feed ratio.
6. A process according to claim 1, acid treated kaoline can be regenerated at
750°C after use and reused with same efficiency.
7. A process according to claim 1, wherein the distillation of the liquid oil
obtained is a mixture of gasoline 30% and rest a mixture of kerosene and
diesel oil.

The present invention discloses a simple method for the conversion of waste
polypropylene to fuel oil. A stainless steel reactor is used to convert the waste
polypropylene to fuel oil in presence of an acid treated kaoline catalyst. This catalyst
improves the yield of oil and increases the rate of reaction. The oil obtained in the
optimum condition is a mixture of different fractions in the range of gasoline (30%) and
the rest a mixture of diesel and kerosene.

Documents:

http://ipindiaonline.gov.in/patentsearch/GrantedSearch/viewdoc.aspx?id=UwDa+s2zRYsR6NKgdyYjEg==&loc=wDBSZCsAt7zoiVrqcFJsRw==

« Previous Patent

Next Patent »

Patent Number

278742

Indian Patent Application Number

674/KOL/2011

PG Journal Number

54/2016

Publication Date

30-Dec-2016

Grant Date

29-Dec-2016

Date of Filing

16-May-2011

Name of Patentee

NATIONAL INSTITUTE OF TECHNOLOGY

Applicant Address

NATIONAL INSTITUTE OF TECHNOLOGY ROURKELA-769 008 DIST: SUNDARGARH ORISSA INDIA

Inventors:

#	Inventor's Name	Inventor's Address
1	DR. RAGHUBANSH KUMAR SINGH	NATIONAL INSTITUTE OF TECHNOLOGY ROURKELA-769 008 DIST: SUNDARGARH ORISSA INDIA
2	MR. ACHYUT KUMAR PANDA	NATIONAL INSTITUTE OF TECHNOLOGY ROURKELA-769 008 DIST: SUNDARGARH ORISSA INDIA

PCT International Classification Number

C10G1/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA