Title of Invention	"A PROCESS FOR THE PREPARATION OF A RESIN FOR USE IN THE MANUFACTURE OF THE COMPOSITE PARTICLES BOARDS"
Abstract	A process for preparation of a resin for use in the manufacture of composite particle boards comprising the steps of: (a) mixing 20 to 90% by weight of a resin material with 5-40% by weight of phenol wherein resin material is selected from cashew nut shell liquid (CNSL), cardanol and a mixture of CSNL and cardanol; (b) adding 0.5-3% by weight of an alkaline catalyst such as herein described to the mixture obtained by step (a) and 0.4 to 0.7 mole of para- formaldehyde wherein the alkaline catalyst is dissolved in 1 to 5 times its weight in water; (c) heating the reaction mixture obtained by step (b) to a temperature of 55 to 95°C for a period of 25 min to 45 minutes; (d) adding 1 to 1,6 mole of para-formaldehyde in divided equal quantities at a fixed time intervals with continued heating; (e) adding further quantity of 5 to 40% by weight of phenol, 0.5 to 2% by weight of sodium hydroxide dissolved in 1 to 5 times its weight in water; (f) heating the mixture obtained by step (e) to a temperature range of 55 to 95°C for a period of 30 to 45 minutes followed by cooling to obtain the desired resin.

Title of Invention

"A PROCESS FOR THE PREPARATION OF A RESIN FOR USE IN THE MANUFACTURE OF THE COMPOSITE PARTICLES BOARDS"

Abstract

A process for preparation of a resin for use in the manufacture of composite particle boards comprising the steps of: (a) mixing 20 to 90% by weight of a resin material with 5-40% by weight of phenol wherein resin material is selected from cashew nut shell liquid (CNSL), cardanol and a mixture of CSNL and cardanol; (b) adding 0.5-3% by weight of an alkaline catalyst such as herein described to the mixture obtained by step (a) and 0.4 to 0.7 mole of para- formaldehyde wherein the alkaline catalyst is dissolved in 1 to 5 times its weight in water; (c) heating the reaction mixture obtained by step (b) to a temperature of 55 to 95°C for a period of 25 min to 45 minutes; (d) adding 1 to 1,6 mole of para-formaldehyde in divided equal quantities at a fixed time intervals with continued heating; (e) adding further quantity of 5 to 40% by weight of phenol, 0.5 to 2% by weight of sodium hydroxide dissolved in 1 to 5 times its weight in water; (f) heating the mixture obtained by step (e) to a temperature range of 55 to 95°C for a period of 30 to 45 minutes followed by cooling to obtain the desired resin.

Full Text	This invention relates to a process for the preparation of a resin for use in the manufacture of the composite particle boards. This is a divisional patent application to 281/DEL/94. It is known in the 'art to produce particle board from agro-wastes using phenolic resins. Such a known process envisages the step of blending rice husk iwht a phenolic resin containing a substantial quantity of water. Due to the presence of water, the blend is subjected to the step of drying for removal of the excess moisture content during or after the resin is coated on the rice husk or furnish. The furnish is then hot pressed to form particle boards. Several disadvantages are associated with the use of such a known phenolic resin. One such disadvantage is that a drying operation results in a precuring of the resin, thereby diminishing its adhesive strength and resulting in poor quality particle boards. Moreover, since rice husk is a material of low bulk density, handling of the resin coated husk or furnish for drying is not convenient. Another disadvantage is that of the control of the moisture content of the furnish. It is generally known that the furnish should have a moisture content, but which simultaneously should not be substantial in quantity as an excess of moisture could result in the formation of blisters or steam pockets in the formed boards. Thus, as rice husk itself contains moisture, the use of the known resin containing substantial quantities of water results in a furnish having a high moisture content, which is detrimental to the formation of the board. Furthermore, even if the furnish is subjected to the step of drying, it is difficult to control the correct content of moisture in the furnish. An object of this invention is to propose a process for the production of a resin for use in the manufacture of the composite boards from rice husk. One of the concepts of the present invention resides in the use of a substantially moisture free resin so that, firstly, the moisture content of the furnish can be controlled and. secondly, the step of drying of the furnish is avoided. The step of control on the moisture content of the furnish is important, as the presence of a correct moisture content provides a board without blisters and steam pockets. According to this invention there is provided a process for preparation of a resin for use in the manufacture of composite particle boards comprising the steps of: (a) mixing 20 to 90% by weight of a resin material with 5-40% by weight of phenol wherein resin material is selected from cashew nut shell liquid (CNSL), cardanol and a mixture of CSNL and cardanol; (b) adding 0.5-3% by weight of an alkaline catalyst such as herein described to the mixture obtained by step (a) and 0.4 to 0.7 mole of para- formaldehyde wherein the alkaline catalyst is dissolved in 1 to 5 times its weight in water; (c) heating the reaction mixture obtained by step (b) to a temperature of 55 to 95°C for a period of 25 min to 45 minutes; (d) adding 1 to 1.6 mole of para-formaldehyde in divided equal quantities at a fixed time intervals with continued heating; (e) adding further quantity of 5 to 40% by weight of phenol, 0.5 to 2% by weight of sodium hydroxide dissolved in 3 to 5 times its weight in water; (f) heating the mixture obtained by step (e) to a temperature range of 55 to 95°C for a period of 30 to 45 minutes followed by cooling to obtain the desired resin. In accordance with this invention an adhesive resin suitable for bonding rice husk is prepared by admixing 20-90% by weight of cashewnut shell liquid and/or cardabol with 10-80% by weight of phenol. The mixture is then heated at a temperature of 50 to 55°C for a period of 20-30 minutes in the presence of 1-50% by weight of an alkaline catalyst. 1.4 to 2 moles of par-formaldehyde is added to athe reaction mixture while the heating is continued to complete the condensatio reaction and thereafter cooling the reacito product. A process for the preparation of a resin according to the process of this invention is herein described in detail. According to the process the reactants are taken in the proportion set forth below - CNSL/Cardanol , 20% to 90% by weight Phenol • ] 0% to 80% by weight These reactants are mixed together and are heated in the presence of a catalyst. Paraformaldehyde equivalent to 1.4 to 2 moles of formaldehyde based on the CNSL and phenol used is then mixed. Alkaline catalyst used in the process is in the range of 1 to 5% by .weight of the CNSL/Cardanol and phenol used. The catah/st is dissolved in 2 to 10 times its weight of water before adding to the condensation mixture The condensation takes place at the temperature ranye of 50 to 95°C The heating is generally continued for a period of 25 to 45 minutes initially. The second stage of condensation after the addition of a further quantity of phenol is carried out at the temperature range of 55 to 95°C for a period of 30 to-45 minutes to complete (he condensation reaction The following examples are only illustrative and not limited to the scope of this invention. EXAMPLE1 5.45 kg, phenol, 0 31 kg sodium hydroxide dissolved in 2.35 kq water, 26 5 kg CNSL and 1.56 kg paraformaldehyde are mixed together and heated to 50 to 55°C Tn about 25 minules, 8,15 kg of paraformaldehyde are added to the above reaction mixture in 12 approximately equal quantities at about 4 mins intervals each. The heating is continued during the addition of paraformaldehyde, 5.9 kg phenol and 0 15 kg of sodium hydroxide dissolved in 0.75 kg water are added to the reaction of mixture, while continuinq the heating. The temperature is then raised to around 65 to 70°C, and the mixture is heated for around 40 minutes to complete the condensation. The resinous product is then cooled 7.5 kg. phenol, 0 37 kg sodium hydroxide dissolved in 2.7 kg water, 13 4 kg cardanol and. 1.5 kq paraformaldehyde are mixed together and heated to 50 to 55°C. To this I 1.0 kg of paraformaldehyde are added in approximately 12 equal quantities at 4 mins. intervals while continuing the heating Subsequently a further quantity of 12.6 kg phenol and 0.22 kg sodium hydroxide dissolved in 1 23 kg water is added to the mixture, and the temperature raised to 65 to 70°C. The heating is continued for 30 minutes to complete the condensation reaction. The product is thereafter cooled. WE CLAIM: 1. A process for preparation of a resin for use in the manufacture of composite particle boards comprising the steps of: (a) mixing 20 to 90% by weight of a resin material with 5-40% by weight of phenol wherein resin material is selected from cashew nut shell liquid (CNSL), cardanol and a mixture of CSNL and cardanol; (b) adding 0.5-3% by weight of an alkaline catalyst such as herein described to the mixture obtained by step (a) and 0.4 to 0.7 mole of para- formaldehyde wherein the alkaline catalyst is dissolved in 1 to 5 times its weight in water; (c) heating the reaction mixture obtained by step (b) to a temperature of 55 to 95°C for a period of 25 min to 45 minutes; (d) adding 1 to 1.6 mole of para-formaldehyde in divided equal quantities at a fixed time intervals with continued heating; (e) adding further quantity of 5 to 40% by weight of phenol, 0.5 to 2% by weight of sodium hydroxide dissolved in 1 to 5 times its weight in water; (f) heating the mixture obtained by step (e) to a temperature range of 55 to 95°C for a period of 30 to 45 minutes followed by cooling to obtain the desired resin. 2. A process as claimed in claim 1 wherein said alkaline catalyst is sodium hydroxide. 3. A process as claimed in claim 1 wherein said para-formaldehyde is added in twelve equal quantities at 4 minutes time interval. 4. A process for preparation of a resin for use for manufacture of composite boards substantially as herein described and illustrated.

Full Text

This invention relates to a process for the preparation of a resin for use in the manufacture of the composite particle boards. This is a divisional patent application to 281/DEL/94.
It is known in the 'art to produce particle board from agro-wastes using phenolic resins. Such a known process envisages the step of blending rice husk iwht a phenolic resin containing a substantial quantity of water. Due to the presence of water, the blend is subjected to the step of drying for removal of the excess moisture content during or after the resin is coated on the rice husk or furnish. The furnish is then hot pressed to form particle boards.
Several disadvantages are associated with the use of such a known phenolic resin. One such disadvantage is that a drying operation results in a precuring of the resin, thereby diminishing its adhesive strength and resulting in poor quality particle boards. Moreover, since rice husk is a material of low bulk density, handling of the resin coated husk or furnish for drying is not convenient.
Another disadvantage is that of the control of the moisture content of the furnish. It is generally known that the furnish should have a moisture content, but which simultaneously should not be substantial in quantity as an excess of moisture could result in the formation of blisters or steam pockets in the formed boards. Thus, as rice husk itself contains moisture, the use of the known resin containing substantial quantities of water results in a furnish having a high moisture content, which is detrimental to the formation of the board. Furthermore, even if the furnish is subjected to the step of drying, it is difficult to control the correct content of moisture in the furnish.
An object of this invention is to propose a process for the production of a resin for use in the manufacture of the composite boards from rice husk.
One of the concepts of the present invention resides in the use of a substantially moisture free resin so that, firstly, the moisture content of the furnish can be controlled and. secondly, the step of drying of the furnish is avoided. The step of control on the moisture

content of the furnish is important, as the presence of a correct moisture content provides a board without blisters and steam pockets.
According to this invention there is provided a process for preparation of a resin for use in the manufacture of composite particle boards comprising the steps of:
(a) mixing 20 to 90% by weight of a resin material with 5-40% by weight of
phenol wherein resin material is selected from cashew nut shell liquid
(CNSL), cardanol and a mixture of CSNL and cardanol;
(b) adding 0.5-3% by weight of an alkaline catalyst such as herein described
to the mixture obtained by step (a) and 0.4 to 0.7 mole of para-
formaldehyde wherein the alkaline catalyst is dissolved in 1 to 5 times its
weight in water;
(c) heating the reaction mixture obtained by step (b) to a temperature of 55 to
95°C for a period of 25 min to 45 minutes;
(d) adding 1 to 1.6 mole of para-formaldehyde in divided equal quantities at a
fixed time intervals with continued heating;
(e) adding further quantity of 5 to 40% by weight of phenol, 0.5 to 2% by
weight of sodium hydroxide dissolved in 3 to 5 times its weight in water;
(f) heating the mixture obtained by step (e) to a temperature range of 55 to
95°C for a period of 30 to 45 minutes followed by cooling to obtain the
desired resin.
In accordance with this invention an adhesive resin suitable for bonding rice husk is prepared by admixing 20-90% by weight of cashewnut shell liquid and/or cardabol with 10-80% by weight of phenol. The mixture is then heated at a temperature of 50 to 55°C for a period of 20-30 minutes in the presence of 1-50% by weight of an alkaline catalyst. 1.4 to 2 moles of par-formaldehyde is added to athe reaction mixture while the heating is continued to complete the condensatio reaction and thereafter cooling the reacito product.
A process for the preparation of a resin according to the process of this invention is herein described in detail.

According to the process the reactants are taken in the proportion set forth below -
CNSL/Cardanol , 20% to 90% by weight
Phenol • ] 0% to 80% by weight
These reactants are mixed together and are heated in the presence of a catalyst. Paraformaldehyde equivalent to 1.4 to 2 moles of formaldehyde based on the CNSL and phenol used is then mixed.
Alkaline catalyst used in the process is in the range of 1 to 5% by .weight of the CNSL/Cardanol and phenol used. The catah/st is dissolved in 2 to 10 times its weight of water before adding to the condensation mixture The condensation takes place at the temperature ranye of 50 to 95°C The heating is generally continued for a period of 25 to 45 minutes initially.
The second stage of condensation after the addition of a further quantity of phenol is
carried out at the temperature range of 55 to 95°C for a period of 30 to-45 minutes to
complete (he condensation reaction
The following examples are only illustrative and not limited to the scope of this invention.

EXAMPLE1
5.45 kg, phenol, 0 31 kg sodium hydroxide dissolved in 2.35 kq water, 26 5 kg CNSL and 1.56 kg paraformaldehyde are mixed together and heated to 50 to 55°C Tn about 25 minules, 8,15 kg of paraformaldehyde are added to the above reaction mixture in 12 approximately equal quantities at about 4 mins intervals each. The heating is continued during the addition of paraformaldehyde, 5.9 kg phenol and 0 15 kg of sodium hydroxide dissolved in 0.75 kg water are added to the reaction of mixture, while continuinq the heating. The temperature is then raised to around 65 to 70°C, and the mixture is heated for around 40 minutes to complete the condensation. The resinous product is then cooled
7.5 kg. phenol, 0 37 kg sodium hydroxide dissolved in 2.7 kg water, 13 4 kg cardanol and. 1.5 kq paraformaldehyde are mixed together and heated to 50 to 55°C. To this I 1.0 kg of paraformaldehyde are added in approximately 12 equal quantities at 4 mins. intervals while continuing the heating Subsequently a further quantity of 12.6 kg phenol and 0.22 kg sodium hydroxide dissolved in 1 23 kg water is added to the mixture, and the temperature raised to 65 to 70°C. The heating is continued for 30 minutes to complete the condensation reaction. The product is thereafter cooled.

WE CLAIM:
1. A process for preparation of a resin for use in the manufacture of composite
particle boards comprising the steps of:
(a) mixing 20 to 90% by weight of a resin material with 5-40% by weight of
phenol wherein resin material is selected from cashew nut shell liquid
(CNSL), cardanol and a mixture of CSNL and cardanol;
(b) adding 0.5-3% by weight of an alkaline catalyst such as herein described
to the mixture obtained by step (a) and 0.4 to 0.7 mole of para-
formaldehyde wherein the alkaline catalyst is dissolved in 1 to 5 times its
weight in water;
(c) heating the reaction mixture obtained by step (b) to a temperature of 55 to
95°C for a period of 25 min to 45 minutes;
(d) adding 1 to 1.6 mole of para-formaldehyde in divided equal quantities at a
fixed time intervals with continued heating;
(e) adding further quantity of 5 to 40% by weight of phenol, 0.5 to 2% by
weight of sodium hydroxide dissolved in 1 to 5 times its weight in water;
(f) heating the mixture obtained by step (e) to a temperature range of 55 to
95°C for a period of 30 to 45 minutes followed by cooling to obtain the
desired resin.

2. A process as claimed in claim 1 wherein said alkaline catalyst is sodium
hydroxide.
3. A process as claimed in claim 1 wherein said para-formaldehyde is added in
twelve equal quantities at 4 minutes time interval.

4. A process for preparation of a resin for use for manufacture of composite boards substantially as herein described and illustrated.

Documents:

584-del-2002-abstract.pdf

584-del-2002-claims.pdf

584-del-2002-correspondence-otheres.pdf

584-del-2002-correspondence-po.pdf

584-del-2002-description (complete).pdf

584-del-2002-form-1.pdf

584-del-2002-form-2.pdf

584-del-2002-gpa.pdf

584-del-2002-petition-138.pdf

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Patent Number

199701

Indian Patent Application Number

584/DEL/2002

PG Journal Number

38/2008

Publication Date

19-Sep-2008

Grant Date

21-Aug-2007

Date of Filing

24-May-2002

Name of Patentee

NATIONAL RESEARCH DEVELOPMENT CORPORATION,a Govt. of India Enterprises, India

Applicant Address

ANUSANDHAN VIKAS, 20-22, ZAMROODPUR COMMUNITY CENTREM KAILASH COLONY EXTENSION, NEW DELHI-110 048, INDIA.

Inventors:

#	Inventor's Name	Inventor's Address
1	JOSEPH GEORGE	226/243/64, 18TH CROSS (BEHIND MARUTI MANDIR), MRCR EXTENSION, MAGADI CHORID ROAD, BANGALORE-560 040, KARNATAKA.

PCT International Classification Number

B2 7N 3/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA