Title of Invention

"A METHOD OF PREPARING NOVEL ORGANIC THERMAL STABILIZER"

Abstract A method of preparing novel organic thermal stabilizer comprising the steps of: subjecting the post consumer waste as herein described to the step of aminolysis with organic compound selected from Ethylenediamine and methylamine in the presence of a catalyst selected from Zinc acetate, Zinc stearate, Aluminium stearate, Lead stearate & Magnesium stearate; mixing the reactants in a reaction vessel and sealing for 15 to 20 days at a temperature of 20 to 50°C; filtering and washing the white precipitate; subjecting the said precipitate to the step of washing and drying.
Full Text BRIEF DESCRIPTION OF THE INVENTION:
According, to this invention there is provided a method of preparing novel organic thermal stabilizer comprising the steps of:
subjecting the post consumer waste as herein described to the step of aminolysis with organic compound selected from Ethylenediamine and methylamine in the presence of a catalyst selected from Zinc acetate, Zinc stearate, Aluminium stearate, Lead stearate & Magnesium stearate; mixing the reactants in a reaction vessel and sealing for 15 to 20 days at a temperature of 20 to 50°C; filtering and washing the white precipitate; subjecting the said precipitate to the step of washing and drying.
DETAILED DESCRIPTION OF THE PRESENT INVENTION:
The present work focuses on the synthesis of a novel organic thermal stabilizer from PET waste. PET waste is degraded by aminolysis to work as thermal stabilizer for PVC. The products obtained were characterized and their structure was elucidated using FTIR, NMR, Mass spectroscopy. The PVC sheets were prepared using this organic thermal stabilizer. The organic stabilizer were used either alone or in combination with some metal stearates.
PET waste (post consumer waste) is such as left over remains of the packaging products of beaverages plastic bottles, films made up of polyethylene terephthalate such as water and soft drink plastic bottles, cups containers etc. was collected, cleaned and cut into flakes. PET waste was then reacted with alkylamine (20% to 38% by weight) in the different ratio. Both the reactant were mixed in the reaction vessel and then it was sealed for 15 to 20 days. The reaction was carried out in the temperature range 20°C to 50°C. The white precipitate started appearing. When all the PET flakes were completely degraded, the reaction was filtered and white precipitate was washed with distilled water and dried in oven.
The above reaction was carried out both in the absence and presence of catalyst. Catalysts employed were Zinc acetate, Zinc stearate, Lead stearate, quaternary ammonium salt etc. The product so obtained was then grinded to fine powder. This white powder was used as such in PVC compounding to work as thermal stabilizer. The quantity of thermal stabilizer was varied from 2 phr to 13 phr.
The white precipitate was also used in combination with some metal stearates such as Magnesium stearate, Zinc stearate, Aluminum stearate, calcium stearate etc. to work as Thermal stabilizer. The result obtained using this white precipitate as thermal stabilizer was comparable with that of lead based stabilizer.
1. PET waste was mixed with alkyfamine (25%) at temperature 25*C in a
sealed vessel. The white precipitate was obtained it was filtered and
washed with distilled water and dried in vacuum oven.-Thermal stabilizer I
2. PET waste was mixed with alkylamine in presence of catalyst Zinc
acetate. The precipitate was filtered was washed with distilled water and
dried-Thermal Stabilizer II
3. PET waste was reacted with ammonia in presence of catalyst such as
Zinc stearate, Aluminium stearate. The white precipitate obtained was
filtered and washed and then dried in vacuum oven-Thermal Stabilizer III

(Table Removed) When the novel organic thermal stabilizer was used in PVC compounding the range of properties was observed such as thermal stability was found in the range of 40-90 minutes. The tensile strength was found to be in the range of 700-1700 psi, %elongation was in the range of 200-350% and tensile modulus in the range of 500-15000 psi, which dearly shows that the novel organic thermal stabilizer is compatible with the other compounding ingredients. The electrical properties were also determined and dielectric strength was found to be in the range 9000-14000 v/mm. Volume resistivety was in the range 30x1012 to 70 x 1012 ohm cm.
EXAMPLE 1:
Preparation of Bis-amino ethyl terephthalamide
A very prompt reaction was observed when PET flakes were aminolysed using ethylene diamlne. A series of reaction were investigated in varying ratio of PETwaste to ethylenedJamine such as 1 :1,1 : 5,1 :10. The reaction was carried out at room temperature in a sealed vessel with stirring at room temperature. The white precipitate started appearing within one-two days. After 10 days the reaction was complete and the precipitate was washed with distill water and was dried in oven at 60° C. It was characterized by various spectroscopic properties and used as thermal stabilizer. The reaction scheme is shown in Rg. 1.
EXAMPLE 2:
10g of PET waste flakes were placed in 500ml flask, 100 ml of CH2NH2 was added to the flask and 1 gm of zinc acetate was added as catalyst then the flask was sealed and kept at room temperature. After 3-5 days It was observed that nearly all the PET waste has been degraded. The reaction mixture was filtered and unreacted PET waste was separated from 1, 4 benzene dicarboxymethyl thus obtained as a product and was washed with distilled water and dried ay 60°C in vacuum oven till constant weight.
Example 3:
10g of PET waste flakes were placed in 500ml flask, 100 mi of CH2NH2 was added to the flask and then the flask was sealed and kept at room temperature. After 15-20 days it was observed that nearly all the PET waste has been degraded. The reaction mixture was filtered and unreacted PET waste was separated from 1, 4 benzene dicarboxymethyl thus obtained as a product and was washed with distilled waster and dried ay 60°C in vacuum oven till constant weight.
EXAMPLE 4:
A very prompt reaction was observed when PET flakes were aminolysed using ethytene diamine A series of reaction were investigated in varying ratio of PET waste to ethyienediamfne such as 1:1,1:5, 1:10. The reaction was carried out at room temperature in a sealed vessel with stirring at room temperature. The white precipitate started appearing within one-two days. After 10 days the reaction was complete and the precipitate was washed with distill water and was dried in oven at 60°C. The product thus obtained was Bis-amino ethyl terephthalamide. It was characterize for various spectroscopic properties and used as thermal stabilizer.




WE CLAIM:
1. A method of preparing novel organic thermal stabilizer comprising the steps
of:
subjecting the post consumer waste as herein described to the step of aminolysis with organic compound selected from Ethylenediamine and methylamine in the presence of a catalyst selected from Zinc acetate, Zinc stearate, Aluminium stearate, Lead stearate & Magnesium stearate;
mixing the reactants in a reaction vessel and sealing for 15 to 20 days at a temperature of 20 to 50°C;
filtering and washing the white precipitate;
subjecting the said precipitate to the step of washing and drying.
2. The method as claimed in claim 1, wherein the preferred temperature for aminolysis is 25°C.

Documents:

238-DEL-2007-Abstract-(14-11-2011).pdf

238-DEL-2007-Abstract-(17-01-2012).pdf

238-del-2007-abstract.pdf

238-DEL-2007-Claims-(14-11-2011).pdf

238-DEL-2007-Claims-(17-01-2012).pdf

238-del-2007-claims.pdf

238-DEL-2007-Correspondence Others-(14-11-2011).pdf

238-DEL-2007-Correspondence Others-(17-01-2012).pdf

238-del-2007-correspondence-others.pdf

238-DEL-2007-Description (Complete)-(14-11-2011).pdf

238-DEL-2007-Description (Complete)-(17-01-2012).pdf

238-del-2007-description (complete).pdf

238-DEL-2007-Form-1-(14-11-2011).pdf

238-del-2007-form-1.pdf

238-DEL-2007-Form-13-(17-01-2012).pdf

238-del-2007-form-18.pdf

238-del-2007-form-2.pdf

238-DEL-2007-GPA-(14-11-2011).pdf

abstract.jpg


Patent Number 251416
Indian Patent Application Number 238/DEL/2007
PG Journal Number 11/2012
Publication Date 16-Mar-2012
Grant Date 12-Mar-2012
Date of Filing 06-Feb-2007
Name of Patentee CHAUDHARY CHARAN SINGH UNIVERSITY, MEERUT
Applicant Address UNIVERSITY MEERUT,INDIA
Inventors:
# Inventor's Name Inventor's Address
1 R,K,SONI CHEMISTRY, C.C.S. UNIVERSITY, MEERUT
2 VANDANA YADAV CHEMISTRY, C.C.S.UNIVERSITY, MEERUT.INDIA
PCT International Classification Number C08J11/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA