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WO2021144708A1 - A phenolic resole resin based closed cell rigid foam insulation panel - Google Patents

A phenolic resole resin based closed cell rigid foam insulation panel Download PDF

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Publication number
WO2021144708A1
WO2021144708A1 PCT/IB2021/050219 IB2021050219W WO2021144708A1 WO 2021144708 A1 WO2021144708 A1 WO 2021144708A1 IB 2021050219 W IB2021050219 W IB 2021050219W WO 2021144708 A1 WO2021144708 A1 WO 2021144708A1
Authority
WO
WIPO (PCT)
Prior art keywords
resole resin
aluminium foil
phenolic resole
closed cell
rigid foam
Prior art date
Application number
PCT/IB2021/050219
Other languages
French (fr)
Inventor
Palanisamy MOHANA KRISHNAN
Original Assignee
Alpha Ducts Llc,
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Alpha Ducts Llc, filed Critical Alpha Ducts Llc,
Publication of WO2021144708A1 publication Critical patent/WO2021144708A1/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/141—Hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/046—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of foam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/028—Net structure, e.g. spaced apart filaments bonded at the crossing points
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
    • B32B5/20—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material foamed in situ
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/245—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it being a foam layer
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014—Use of organic additives
    • C08J9/0033—Use of organic additives containing sulfur
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/03—3 layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/05—5 or more layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/101—Glass fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
    • B32B2264/10—Inorganic particles
    • B32B2264/102—Oxide or hydroxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2266/00—Composition of foam
    • B32B2266/02—Organic
    • B32B2266/0214—Materials belonging to B32B27/00
    • B32B2266/0285—Condensation resins of aldehydes, e.g. with phenols, ureas, melamines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2266/00—Composition of foam
    • B32B2266/08—Closed cell foam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/546—Flexural strength; Flexion stiffness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/72—Density
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2419/00—Buildings or parts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
    • C08J2201/026—Crosslinking before of after foaming
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00—Foams characterised by their properties
    • C08J2205/04—Foams characterised by their properties characterised by the foam pores
    • C08J2205/052—Closed cells, i.e. more than 50% of the pores are closed
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00—Foams characterised by their properties
    • C08J2205/10—Rigid foams
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • C08J2361/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols with monohydric phenols
    • C08J2361/10—Phenol-formaldehyde condensates

Definitions

  • TITLE A PHENOLIC RESOLE RESIN BASED CLOSED CELL RIGID FOAM INSULATIONPANEL
  • This invention is related to an insulation material particularly phenolic resole resin-based foam material formation and process of making thereof.
  • Phenolic resole resin-based foam is a very old technology. Phenolic resole resin-based rigid foam is well known for its noble properties like better fire, low smoke, low thermal conductivity. It is widely used in building material applications. Especially as insulation products like HVAC ducts, Duct Insulation, Wall insulation and roof insulation.
  • a phenolic resin foam which includes a phenolic resin and a blowing agent including at least one type of halogenated unsaturated hydrocarbon, and has an average cell diameter of 120 mm or less, a thermal conductivity of 0.019 W/mK or less, and a limiting oxygen index of 28 % or more.
  • the resulting molded product was taken out from the mold and placed in a dryer heated to 85 °C where the molded product was cured for 5 hours, thereby preparing phenolic resin foam.
  • a polysiloxane copolymer composition comprises: a polysiloxane unit comprising 4 to 50 siloxane units, and a polyester- polycarbonate unit consisting of 50 to 100-molepercent of acrylate ester units, less than 50-molepercent aromatic carbonate units, less than 30-molepercent resorcinol carbonate units, and less than 35-molepercentbisphenol carbonate units, wherein the siloxane units are present in the polysiloxane unit in an amount of 0.2 to 10 wt % of the total weight of the polysiloxane copolymer composition, and wherein the polysiloxane copolymer composition has a 2 minute integrated heat release rate of less than or equal to 65 kilowatt-minutes per square meter (kW-min/m 2 ) and a peak heat release rate of less than 65 kilowatts per square meter (kW/m 2 ) as measured using the method of FAR
  • Silicone-based surfactant gives poor closed cell content.
  • Sulphuric acid is one of the precursor chemicals. Maintaining the stock and dealing with the legal authorities are difficult to manage.
  • Phosphoric acid is increasing the hardness of the cell wall. It reduces the flexibility of the wall. It generates hard foam with a maximum percentage of open cells.
  • Curing temperature is around 90 to 95 deg C. High temperature reduces the uniform reaction and cell formation. It reduces the uniform cell structure as well as damages the cells too.
  • Curing time is 9 to 10 minutes. Lesser curing time reduces the cell wall strength. Lesser curing time prevents the further continuation of the reaction. So the cell wall becomes weak. It generates a lot of open cells
  • the main objective of the invention is to provide an insulation material particularly phenolic resole resin-based foam material formation.
  • the other objective of the invention is to provide an insulation material particularly phenolic resole resin-based foam material composition
  • Yet the other objective of the present invention is to provide a process for forming an insulation material particularly phenolic resole resin-based foam material.
  • This invention is related to an insulation material particularly phenolic resole resin- based foam material formation and process of making wherein the phenolic resole resin making process, modifying the parameters, by introducing /eliminating the below listed raw materials also the material ratios of the components resole resin mixture, blowing agent, curing agent are mixed and sandwiched between aluminium foil / glass mesh coated aluminium foil / fibber glass cloth reinforced aluminium foil with set temperature and after cooling the mix resulting Phenolic resole resin-based closed-cell rigid foam insulation panel and the method of manufacturing a Phenolic resole resin-based closed-cell rigid foam comprising of - Adding the components a) resole resin mixture-122.0 parts, b) blowing agent-7 parts, c) curing agent-30.0 parts and mixed with high speed mixture, - Pouring the mixed material on the bottom facing Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced aluminium foil which is kept on the preheated mold.
  • Fig 1 illustrates the top facing of the phenolic resole resin based foam panel
  • Fig 2 illustrates the increase in foam bending
  • Fig 3 illustrates the phenolic resole resin foam
  • in one embodiment in this invention is mainly targeting to achieve all above the market requirements by modifying the phenolic resole resin making process, modifying the parameters, by introducing /eliminating the below listed raw materials also the material ratios
  • This particular product consists of two major components which are
  • facing materials for this particular product are aluminium foil, glass mesh coated aluminium foil and fibber glass cloth reinforced aluminium foil and etc.
  • the main embodiments in the components are required for making this foam core. a) Phenolic resole resin b) Solvent/ plasticizer for resin c) Surfactant d) Filler e) Blowing agent f) Curing agent
  • the raw materials taken for preparing the resole resin are 1) Liquid phenol, 2) Formaldehyde 3) sodium hydroxide, 4) urea, 5) Poly ethylene Glycol ,6) Polyoxyethylene (20) sorbitanmonolaurate, 7) Silica powder.
  • component A Polyoxyethylene(20) sorbitanmonolaurate of resin was added and mixed well for another 10 min. 0.1 to 5 % of silica powder of resin was added and mixed well for 10 min. This mixture will be stored in cold storage. This is called component A.
  • the composition for blowing agent is Cyclo pentane (85%) + Iso Pentane (15 %) mixture or Cyclo pentane (80%) + Iso Pentane (20 %) mixture.
  • Cyclo pentane (85%) + Iso Pentane (15 %) mixture is used as a blowing agent.
  • Blowing agent quantity would be around 4 to 7 % of Component A.
  • Component A 122.0 parts
  • Component B 7.0 parts
  • the above components are mixed with the high-speed mixture and the mixed material is poured on the bottom facing (Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced Aluminium foil) which is kept on the preheated mold. After pouring the mixed material, place another facing (Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced Aluminium foil) on top of the material and close the mold. Maintain the temperature initially around 70 to 75 deg C for 9 to 10 min, then reducing the temperature to 65 to 70 deg C for 2 to 4 hrs. After that, open the mold and remove the foam panel and slice it in required size and pack the panel and store it in cool-dry place. Avoid direct sunlight.
  • Poly ethylene glycol with average molecular weight is 400. It is a low toxic material. It is used as a solvent / plasticizer to reduce the viscosity of the resin. Handling of the resin is easy if resin viscosity becomes low. It increases the closed-cell content of the foam also.
  • Silica powder is just an inorganic filler to increase the mechanical strength of the foam. It prevents the foam shrinkage also. Shrinkage of the foam is a major problem after the production, especially for the closed-cell foam panel. But more quantity will affect the closed cell content. More quantity will generate more open cells.
  • Cyclo pentane or cyclopentane (85%) + lsopentane(15%) mixture can be used as a blowing agent. It is CFC & HCFC free blowing agent.
  • Curing time is 9 to 10 minutes. Lesser curing time reduces the cell wall strength. Lesser curing time prevents the further continuation of the reaction. So the cell wall becomes weak. It generates a lot of open cells. So, curing time has been increased to 3 to 4 hrs.
  • Foam density is 55 to 65 Kgs / m3
  • Achieved Compressive strength @ 10% deformation value is 187.4 kPa
  • FIG 2 shows the increase in foam bending
  • Fig 1 , 3 illustrate phenolic resole resin-based foam panel.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

This invention is related to an insulation material particularly phenolic resole resin-based foam material formation by modifying the phenolic resole resin making process, modifying the parameters, by introducing/eliminating some raw materials also the material ratios to achieve low thermal conductivity, better mechanical strength, better closed-cell value, better bending property, eco-friendly blowing agent, low smoke value and better fire property.

Description

TITLE: A PHENOLIC RESOLE RESIN BASED CLOSED CELL RIGID FOAM INSULATIONPANEL
FIELD OF INVENTION
This invention is related to an insulation material particularly phenolic resole resin-based foam material formation and process of making thereof.
BACKGROUND OF THE INVENTION
Phenolic resole resin-based foam is a very old technology. Phenolic resole resin- based rigid foam is well known for its noble properties like better fire, low smoke, low thermal conductivity. It is widely used in building material applications. Especially as insulation products like HVAC ducts, Duct Insulation, Wall insulation and roof insulation.
There are many inventions forming resin foams, like in EP3275927A1 , where a phenolic resin foam which includes a phenolic resin and a blowing agent including at least one type of halogenated unsaturated hydrocarbon, and has an average cell diameter of 120 mm or less, a thermal conductivity of 0.019 W/mK or less, and a limiting oxygen index of 28 % or more. The resulting molded product was taken out from the mold and placed in a dryer heated to 85 °C where the molded product was cured for 5 hours, thereby preparing phenolic resin foam.
In US 7,790,292 B2, A polysiloxane copolymer composition comprises: a polysiloxane unit comprising 4 to 50 siloxane units, and a polyester- polycarbonate unit consisting of 50 to 100-molepercent of acrylate ester units, less than 50-molepercent aromatic carbonate units, less than 30-molepercent resorcinol carbonate units, and less than 35-molepercentbisphenol carbonate units, wherein the siloxane units are present in the polysiloxane unit in an amount of 0.2 to 10 wt % of the total weight of the polysiloxane copolymer composition, and wherein the polysiloxane copolymer composition has a 2 minute integrated heat release rate of less than or equal to 65 kilowatt-minutes per square meter (kW-min/m2) and a peak heat release rate of less than 65 kilowatts per square meter (kW/m2) as measured using the method of FAR F25.4, in accordance with Federal Aviation Regulation FAR 25.853 (d). A window article for an aircraft, comprising the polysiloxane copolymer composition, is also disclosed.
Many problems are being faced with our old resole resin as well as a foam panel making process. These problems are directly affecting the product quality, such as in
RESIN MAKING PROCESS:
1) The barium hydroxide based resin process is a time-consuming process. It delays the overall reaction period around 2 to 3 hrs.
2) Excess quantity of formaldehyde reduces the formation of closed-cell as well as increase the free formaldehyde content in the resin as well as in foam.
3) Handling the high viscous resin is too difficult. Draining the resin from the reactor as well as from the containers after cooling.
SURFACTANT:
1 ) Silicone-based surfactant gives poor closed cell content.
BLOWING AGENT:
1 ) CFC / FICFC based blowing agents create lot of environmental impacts.
2) FICFC 141 b blowing agent is already limited to use by UAE law
3) It is also very difficult to procure the material from other countries as well as from the local market because of the restrictions by the government.
CURING AGENT:
1 ) Sulphuric acid is one of the precursor chemicals. Maintaining the stock and dealing with the legal authorities are difficult to manage. 2) Phosphoric acid is increasing the hardness of the cell wall. It reduces the flexibility of the wall. It generates hard foam with a maximum percentage of open cells.
FOAM MAKING PROCESS:
A) CURING TEMPERATURE:
Curing temperature is around 90 to 95 deg C. High temperature reduces the uniform reaction and cell formation. It reduces the uniform cell structure as well as damages the cells too.
B) CURING TIME:
Curing time is 9 to 10 minutes. Lesser curing time reduces the cell wall strength. Lesser curing time prevents the further continuation of the reaction. So the cell wall becomes weak. It generates a lot of open cells
Hence, the modifications are required to sort out all the above mentioned problems which were faced during the production time for decade as well as based on the feedback from the customers about the product quality and also based on the market requirements which are given below.
1) Low thermal conductivity ( less than 0.025 W/m K as per ASTM C 518 - 15)
2) Compressive strength (more than 150 kPa as per BS EN 826 :2013)
3) Better closed-cell value (more than 90 % as per EN ISO 4590:2017)
4) Better bending property ( panel should get bend without any rupture)
5) Eco-friendly blowing agent (CFC & HCFC free)
6) Low smoke value ( less than or equal to 50 as per ASTM E 84)
7) Better fire property ( less than or equal to 25 as per ASTM E 84)
Therefore there is a need for modifying the phenolic resole resin making process, foam panel making process, modifying the parameters, material ratios and etc. OBJECT OF THE PRESENT INVENTION
The main objective of the invention is to provide an insulation material particularly phenolic resole resin-based foam material formation.
The other objective of the invention is to provide an insulation material particularly phenolic resole resin-based foam material composition
Yet the other objective of the present invention is to provide a process for forming an insulation material particularly phenolic resole resin-based foam material.
SUMMARY
This invention is related to an insulation material particularly phenolic resole resin- based foam material formation and process of making wherein the phenolic resole resin making process, modifying the parameters, by introducing /eliminating the below listed raw materials also the material ratios of the components resole resin mixture, blowing agent, curing agent are mixed and sandwiched between aluminium foil / glass mesh coated aluminium foil / fibber glass cloth reinforced aluminium foil with set temperature and after cooling the mix resulting Phenolic resole resin-based closed-cell rigid foam insulation panel and the method of manufacturing a Phenolic resole resin-based closed-cell rigid foam comprising of - Adding the components a) resole resin mixture-122.0 parts, b) blowing agent-7 parts, c) curing agent-30.0 parts and mixed with high speed mixture, - Pouring the mixed material on the bottom facing Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced aluminium foil which is kept on the preheated mold. -Placing another facing on Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced aluminium foil top of the material and close the mold. -Maintaining the temperature initially around 70 to 75 deg C for 9 to 10 min and then reducing the temperature to 65 to 70 deg C for 2 to 4 hrs -removing from the mold and slice it as per the requirement and pack it and keep it in cool and dry places. DETAILED DESCRIPTION OF THE DRAWING
Fig 1 illustrates the top facing of the phenolic resole resin based foam panel Fig 2 illustrates the increase in foam bending Fig 3 illustrates the phenolic resole resin foam
DETAILED DESCRIPTION OF THE INVENTION
In one embodiment in this invention is mainly targeting to achieve all above the market requirements by modifying the phenolic resole resin making process, modifying the parameters, by introducing /eliminating the below listed raw materials also the material ratios
1) Addition of Polyethylene glycol
2) Addition of Silica powder
3) Addition of Sodium hydroxide
4) Addition of Polyoxyethylene (20) sorbitanmonolaurate
5) Addition of Pentane
6) Removal of sulphuric acid
7) Removal of phosphoric acid
8) Removal of a silicone-based surfactant
9) Removal of barium hydroxide
10) Removal of HCFC 141 b
In one embodiment in the invention modifying the ratio of a parameter such as
1) Curing time
2) Curing temperature
3) Material ratios (the resin & foam panel making process)
This particular product consists of two major components which are
1) Facing materials
2) Phenolic foam core 1. Facing materials :
Commercially available facing materials for this particular product are aluminium foil, glass mesh coated aluminium foil and fibber glass cloth reinforced aluminium foil and etc.
2. Phenolic foam core
This is phenolic-formaldehyde resole resin-based foam core. As per this invention, the main embodiments in the components are required for making this foam core. a) Phenolic resole resin b) Solvent/ plasticizer for resin c) Surfactant d) Filler e) Blowing agent f) Curing agent
3. It is one of the main embodimentin the invention that the raw materials taken for preparing the resole resin, the materials are 1) Liquid phenol, 2) Formaldehyde 3) sodium hydroxide, 4) urea, 5) Poly ethylene Glycol ,6) Polyoxyethylene (20) sorbitanmonolaurate, 7) Silica powder.
4.
RESOLE RESIN and MIXTURE (Component A)
495 g of liquid phenol is added with 580 g of formaldehyde and then 13 g of sodium hydroxide solution is added and mixed well for 5 min. Then the mixture is heated slowly to reach the temperature of 95 deg C and maintained at the same temperature around 120 to 180 min. After completion of the reflux time, 25 g urea added and mixed well for 5 min then dehydration process was started until getting the viscosity around 20000 to 40000 cPs at 25 deg C. Then the mixture was cooled to 60 to 65 deg C, and then 1 to 12 % of polyethylene glycol-400 of resin was added and mixed well for 10 min. Then 1 to 12 % of Polyoxyethylene(20) sorbitanmonolaurate of resin was added and mixed well for another 10 min. 0.1 to 5 % of silica powder of resin was added and mixed well for 10 min. This mixture will be stored in cold storage. This is called component A.
BLOWING AGENT (Component B):
In one embodiment the composition for blowing agent is Cyclo pentane (85%) + Iso Pentane (15 %) mixture or Cyclo pentane (80%) + Iso Pentane (20 %) mixture. In this case, particularly, preferably Cyclo pentane (85%) + Iso Pentane (15 %) mixture is used as a blowing agent. Blowing agent quantity would be around 4 to 7 % of Component A.
CURING AGENT (Component C):
In this case, only para toluene sulphonic acid is used as a curing agent. Quantity would be around 20 to 30 % of addition of component A and Component B FOAM PANEL MAKING PROCESS:
EXAMPLES
Component A = 122.0 parts Component B = 7.0 parts
Component C = 30.0 parts
Total = 159.0 parts
It is the main embodiment in the invention that the above components are mixed with the high-speed mixture and the mixed material is poured on the bottom facing (Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced Aluminium foil) which is kept on the preheated mold. After pouring the mixed material, place another facing (Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced Aluminium foil) on top of the material and close the mold. Maintain the temperature initially around 70 to 75 deg C for 9 to 10 min, then reducing the temperature to 65 to 70 deg C for 2 to 4 hrs. After that, open the mold and remove the foam panel and slice it in required size and pack the panel and store it in cool-dry place. Avoid direct sunlight.
The main embodiment in the invention is to use new combinational materials and modified parameters
1) Polyethylene glycol
It is a polyether component. Preferably Poly ethylene glycol with average molecular weight is 400. It is a low toxic material. It is used as a solvent / plasticizer to reduce the viscosity of the resin. Handling of the resin is easy if resin viscosity becomes low. It increases the closed-cell content of the foam also.
2) Silica powder
Silica powder is just an inorganic filler to increase the mechanical strength of the foam. It prevents the foam shrinkage also. Shrinkage of the foam is a major problem after the production, especially for the closed-cell foam panel. But more quantity will affect the closed cell content. More quantity will generate more open cells.
3) Sodium hydroxide
Replacing barium hydroxide by sodium hydroxide in order to decrease the overall reaction time.
4) Polyoxyethylene (20) sorbitanmonolaurate
It is a non-ionic surfactant. It gives better structural properties as well as the closed-cell content than the silicone-based surfactant.
5) Pentane
Cyclo pentane or cyclopentane (85%) + lsopentane(15%) mixture can be used as a blowing agent. It is CFC & HCFC free blowing agent.
6) Curing temperature:
High temperature reduces the uniform reaction and cell formation. It reduces the uniform cell structure as well as damages the cells too. So, the temperature has been reduced to 70 to 75 deg C
7) Curing time: Curing time is 9 to 10 minutes. Lesser curing time reduces the cell wall strength. Lesser curing time prevents the further continuation of the reaction. So the cell wall becomes weak. It generates a lot of open cells. So, curing time has been increased to 3 to 4 hrs.
It is the main embodiment in the invention that the following properties are observed in the foam which is arrived in the novel process as above explained.
1) Foam density .
Foam density is 55 to 65 Kgs / m3
2) Closed-cell content (as per EN ISO 4590:2017)
Achieved Closed-cell content value is 97%
3) Thermal conductivity ( as per ASTM C 518 -15)
Achieved values are
A) Thermal conductivity @ 35 deg C= 0.023 W/mK
B) Thermal conductivity @ 10 deg C=0.0229 W/mK
4) Compressive strength @ 10% deformation( BS EN 826 :2013)
Achieved Compressive strength @ 10% deformation value is 187.4 kPa
5) Bending test ( in house test)
Refer Fig 2 shows the increase in foam bending and Fig 1 , 3 illustrate phenolic resole resin-based foam panel.
6) Low smoke value (as per ASTM E 84)
Achieved Smoke developed index is 10
7) Better fire property (as per ASTM E 84)
Achieved Flame Spread Index is 25
While typical embodiments have been set forth for the purpose of illustration, the foregoing descriptions should not be deemed to be a limitation on the scope herein. Accordingly, various modifications, adaptations, and alternatives may occur to one skilled in the art without departing from the spirit and scope herein.

Claims

1 . A Phenolic resole resin based closed cell rigid foam consisting of a) Resole resin mixture (resole resin along with surfactants, solvents & fillers) b) Blowing agent c) Curing agent
Wherein the components resole resin mixture, blowing agent, curing agent are mixed and sandwiched between aluminium foil / glass mesh coated aluminium foil / fibber glass cloth reinforced aluminium foil with set temperature and after cooling the mix resulting Phenolic resole resin based closed cell rigid foam insulation panel.
2. The Phenolic resole resin based closed cell rigid foam as claimed in claim 1 , wherein the resole resin is composition of liquid phenol, formaldehyde, sodium hydroxide, urea, poly ethylene glycol (average molecular weight
400),polyoxyethelene(20)sorbitanmonolarate, and silica powder.
3. The Phenolic resole resin based closed cell rigid foam as claimed in claim 1 , wherein the said blowing agent is the composition of Cyclo pentane (85%) and Iso Pentane (15 %) mixture or Cyclo pentane (80%) and Iso Pentane (20 %) mixture.
4. The Phenolic resole resin based closed cell rigid foam as claimed in claim 1 , wherein the said curing agent is the composition of Para toluene sulphonic acid.
5. A method of manufacturing a Phenolic resole resin based closed cell rigid foam comprising of
- Adding the components a) resole resin-122.0 parts, b) blowing agent-7 parts, c) curing agent-30.0 parts and mixed with high speed mixture,
- Pouring the mixed material on the bottom facing Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced aluminium foil which is kept on the preheated mold.
-Placing another facing on Aluminium foil or glass mesh coated aluminium foil or Fibber glass cloth reinforced aluminium foil top of the material and close the mold. -Maintaining the temperature initially around 70 to 75 deg C for 9 to 10 min and then reducing the temperature to 65 to 70 deg C for 2 to 4 hrs
-removing from the mold and slice it as per the requirement and pack it and keep it in cool and dry palces.
6. The Phenolic resole resin based closed cell rigid foam as claimed in claim 1 , wherein the said set temperature is 70 to 75°C.
PCT/IB2021/050219 2020-01-14 2021-01-13 A phenolic resole resin based closed cell rigid foam insulation panel WO2021144708A1 (en)

Applications Claiming Priority (2)

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IN202041001670 2020-01-14

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114987001A (en) * 2022-07-14 2022-09-02 福建天利高新材料有限公司 Hard open-cell foam sound insulation board and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3282863A (en) * 1961-12-01 1966-11-01 Shell Oil Co Resin foams
EP1583794B1 (en) * 2003-01-13 2007-05-09 Kingspan Holdings (IRL) Limited A phenolic foam
EP2898005B1 (en) * 2012-09-18 2017-11-01 Kingspan Holdings (IRL) Limited Phenolic foam

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3282863A (en) * 1961-12-01 1966-11-01 Shell Oil Co Resin foams
EP1583794B1 (en) * 2003-01-13 2007-05-09 Kingspan Holdings (IRL) Limited A phenolic foam
EP2898005B1 (en) * 2012-09-18 2017-11-01 Kingspan Holdings (IRL) Limited Phenolic foam

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114987001A (en) * 2022-07-14 2022-09-02 福建天利高新材料有限公司 Hard open-cell foam sound insulation board and preparation method and application thereof

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