US3607811A - Stable phenol formaldehyde resin solution for preparation of fire-resistant laminates - Google Patents
Stable phenol formaldehyde resin solution for preparation of fire-resistant laminates Download PDFInfo
- Publication number
- US3607811A US3607811A US781962A US3607811DA US3607811A US 3607811 A US3607811 A US 3607811A US 781962 A US781962 A US 781962A US 3607811D A US3607811D A US 3607811DA US 3607811 A US3607811 A US 3607811A
- Authority
- US
- United States
- Prior art keywords
- fire
- phosphates
- preparation
- resin solution
- phenol formaldehyde
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Lifetime
Links
- 229920001568 phenolic resin Polymers 0.000 title abstract description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 230000009970 fire resistant effect Effects 0.000 title abstract description 7
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 20
- 235000021317 phosphate Nutrition 0.000 claims abstract description 20
- 229920005989 resin Polymers 0.000 claims description 17
- 239000011347 resin Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- DTOMFYCTRINWHW-UHFFFAOYSA-N diazanium;methyl phosphate Chemical class [NH4+].[NH4+].COP([O-])([O-])=O DTOMFYCTRINWHW-UHFFFAOYSA-N 0.000 claims description 11
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 5
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 abstract description 13
- -1 alkyl phosphates Chemical class 0.000 abstract description 8
- 238000005470 impregnation Methods 0.000 abstract description 8
- 239000002655 kraft paper Substances 0.000 abstract description 6
- 150000003839 salts Chemical class 0.000 abstract description 5
- 230000001476 alcoholic effect Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 8
- 239000010452 phosphate Substances 0.000 description 8
- 239000000779 smoke Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000011161 development Methods 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 230000002349 favourable effect Effects 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000002301 combined effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052816 inorganic phosphate Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical class [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
-
- 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
Definitions
- the invention relates to an aqueous alcoholic phenol formaldehyde resin solution suitable for one-step impregnation of kraft paper for the preparation of fire-resistant laminates, containing alkyl phosphates and/or salts thereof and ammonium bromide.
- the invention relates to phenol formaldehyde resin solutions being particularly suitable for the preparation of fire-resistant laminates and having good storage stability.
- the kraft paper is first impregnated with an aqueous solution of one or more fire-preventing agents, usually inorganic salts, whereafter the paper is dried and then impregnated with a solution of phenol formaldehyde resin in aqueous alcohol.
- fire-preventing agents usually inorganic salts
- ammonium bromide had a better inhibiting effect on the smoke temperature (which is an indication of fire-preventing effect) than ammonium methyl phosphates, while the opposite was the case for the smoke development.
- ammonium bromide alone makes it necessary to use unreasonably large amounts to obtain a satisfactory low smoke development
- ammonium methyl phosphates (or other inorganic or organic phosphates) alone makes it necessary to use unreasonably large amounts to obtain a satisfactory fire-preventing effect.
- This also confirms the necessity of using the large amounts of phosphate used according to the above mentioned British Patent, since in the fire-preventing phosphate used it is only the phosphate group itself which exerts any fire-preventing efiect.
- a fire-preventing, storage stable phenol formaldehyde resin solution being particularly suitable for one-step impregnation of kraft paper for the preparation of laminates
- the resin solution is characterized in that it contains from 1 to 10 percent by weight of C alkyl phosphates and/or ammonium salts thereof and from 2 to 10 percent by weight of ammonium bromide, and in that it contains a C alkanol and water in a ratio by weight of alkanol/water of at least 0.60, preferably between 0.85 and 2.
- the percentages by weight stated are calculated as anhydrous substance relative to the total solution of resin and fire-preventing compounds in alcohol and water.
- the resin content (dry weight) in the resin solution will normally be from 35 to 50 percent by weight. If more than 50 percent by weight is used the stability of the resin solution will not be satisfactory for prolonged storage, and if less than 35 percent by weight is used the solution will contain insufiicient resin to give a satisfactory laminate.
- EXAMPLE A solution A was prepared from 450 grams of a phenol formaldehyde resin solution and grams of ethanol.
- the phenol formaldehyde resin solution consists of about 65 percent by weight. of alkali catalyzed phenol fonnaldehyde resin having a molar ratio of formaldehyde/phenol of 1.44, about 17 percent by weight of water, about 11 percent by weight of ethanol and about 7 percent by weight of free formaldehyde and phenol, so that 450 grams thereof contains about 295 grams of resin, 75 grams of water, 50 grams of ethanol and 30 grams of unreacted formaldehyde and phenol.
- a solution B was prepared from 44 grams of ammonium bromide, 4i grams of aqueous ammonium methyl phosphates (consisting of about 65 percent by weight of ammonium methyl phosphates and 35 percent by weight of water, i.e. about 27 and 14 grams respectively) and 60 grams of water.
- the two solutions A and B were thoroughly mixed and adjusted to a pH of about 5.2 by means of 25 percent ammonia.
- the resulting mixture had a content of ammonium methyl phosphates of about 3.5 percent and of ammonium bromide of about 6 percent by weight, and an ethanol/water ratio of about 1.3.
- the mixture was homogeneous and remained completely clear for more than 4 months at room temperature. Laminates prepared with this mixture fulfilled with good margin the requirements with respect to flame spread and smoke development set up by the Norwegian Veritas for surface materials for use in corridors and stairs.
- ammonium methyl phosphates it is also possible to employ ammonium ethyl-, -propyland -butyl phosphates, however, since ammonium methyl phosphates contain most of the active phosphate group per unit weight and also give the most stable solutions they are preferred.
- the pure C alkyl phosphates may also be employed, although the stability of the solutions containing these will not be as good as for solutions containing ammonium methyl phosphates;
- a phenol-formaldehyde solution suitable for one-step impregnation of kraft paper for the preparation of fire-resistant laminates and having excellent storage stability comprising from 35 to 50 percent by weight of phenol formaldehyde resin, from 1 to 10 percent by weight of a phosphate selected from the group of C alkyl phosphates, and C alkyl ammonium phosphates, and from 2 to 10 percent by weight of ammonium bromide, and a solvent which is a mixture of C alkanol and water in a ratio by weight of alkanol to water between about 0.60 and about 2.0.
- Resin solution according to claim 1, wherein the phosphates are ammonium methyl phosphates.
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Reinforced Plastic Materials (AREA)
- Fireproofing Substances (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NO170967A NO118878B (enrdf_load_stackoverflow) | 1967-12-13 | 1967-12-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3607811A true US3607811A (en) | 1971-09-21 |
Family
ID=19910355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US781962A Expired - Lifetime US3607811A (en) | 1967-12-13 | 1968-12-06 | Stable phenol formaldehyde resin solution for preparation of fire-resistant laminates |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US3607811A (enrdf_load_stackoverflow) |
| DE (1) | DE1814137A1 (enrdf_load_stackoverflow) |
| GB (1) | GB1188219A (enrdf_load_stackoverflow) |
| NO (1) | NO118878B (enrdf_load_stackoverflow) |
| SE (1) | SE334030B (enrdf_load_stackoverflow) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10260232B1 (en) | 2017-12-02 | 2019-04-16 | M-Fire Supression, Inc. | Methods of designing and constructing Class-A fire-protected multi-story wood-framed buildings |
| US10290004B1 (en) | 2017-12-02 | 2019-05-14 | M-Fire Suppression, Inc. | Supply chain management system for supplying clean fire inhibiting chemical (CFIC) totes to a network of wood-treating lumber and prefabrication panel factories and wood-framed building construction job sites |
| US10311444B1 (en) | 2017-12-02 | 2019-06-04 | M-Fire Suppression, Inc. | Method of providing class-A fire-protection to wood-framed buildings using on-site spraying of clean fire inhibiting chemical liquid on exposed interior wood surfaces of the wood-framed buildings, and mobile computing systems for uploading fire-protection certifications and status information to a central database and remote access thereof by firefighters on job site locations during fire outbreaks on construction sites |
| US10332222B1 (en) | 2017-12-02 | 2019-06-25 | M-Fire Supression, Inc. | Just-in-time factory methods, system and network for prefabricating class-A fire-protected wood-framed buildings and components used to construct the same |
| US10430757B2 (en) | 2017-12-02 | 2019-10-01 | N-Fire Suppression, Inc. | Mass timber building factory system for producing prefabricated class-A fire-protected mass timber building components for use in constructing prefabricated class-A fire-protected mass timber buildings |
| US10653904B2 (en) | 2017-12-02 | 2020-05-19 | M-Fire Holdings, Llc | Methods of suppressing wild fires raging across regions of land in the direction of prevailing winds by forming anti-fire (AF) chemical fire-breaking systems using environmentally clean anti-fire (AF) liquid spray applied using GPS-tracking techniques |
| US10814150B2 (en) | 2017-12-02 | 2020-10-27 | M-Fire Holdings Llc | Methods of and system networks for wireless management of GPS-tracked spraying systems deployed to spray property and ground surfaces with environmentally-clean wildfire inhibitor to protect and defend against wildfires |
| US11395931B2 (en) | 2017-12-02 | 2022-07-26 | Mighty Fire Breaker Llc | Method of and system network for managing the application of fire and smoke inhibiting compositions on ground surfaces before the incidence of wild-fires, and also thereafter, upon smoldering ambers and ashes to reduce smoke and suppress fire re-ignition |
| US11826592B2 (en) | 2018-01-09 | 2023-11-28 | Mighty Fire Breaker Llc | Process of forming strategic chemical-type wildfire breaks on ground surfaces to proactively prevent fire ignition and flame spread, and reduce the production of smoke in the presence of a wild fire |
| US11836807B2 (en) | 2017-12-02 | 2023-12-05 | Mighty Fire Breaker Llc | System, network and methods for estimating and recording quantities of carbon securely stored in class-A fire-protected wood-framed and mass-timber buildings on construction job-sites, and class-A fire-protected wood-framed and mass timber components in factory environments |
| US11865394B2 (en) | 2017-12-03 | 2024-01-09 | Mighty Fire Breaker Llc | Environmentally-clean biodegradable water-based concentrates for producing fire inhibiting and fire extinguishing liquids for fighting class A and class B fires |
| US11865390B2 (en) | 2017-12-03 | 2024-01-09 | Mighty Fire Breaker Llc | Environmentally-clean water-based fire inhibiting biochemical compositions, and methods of and apparatus for applying the same to protect property against wildfire |
| US11911643B2 (en) | 2021-02-04 | 2024-02-27 | Mighty Fire Breaker Llc | Environmentally-clean fire inhibiting and extinguishing compositions and products for sorbing flammable liquids while inhibiting ignition and extinguishing fire |
| US12168152B2 (en) | 2021-02-04 | 2024-12-17 | Mighty Fire Breaker Llc | Remotely-triggered wildfire defense system for automatically spraying environmentally-clean water-based liquid fire inhibitor to proactively form thin fire-inhibiting alkali metal salt crystalline coatings on sprayed combustible surfaces prior to wildfire |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2807697A1 (de) * | 1978-02-23 | 1979-09-06 | Basf Ag | Feuerschutzmasse |
| DE3032156A1 (de) * | 1980-08-26 | 1982-04-08 | Odenwald-Chemie GmbH, 6901 Schönau | Waermedaemmendes und feuerhemmendes, fuer den schutz von konstruktionsteilen aus holz, beton, stahl o.dgl. dienendes abdeckelement sowie verfahren und vorrichtung zu dessen herstellung |
-
1967
- 1967-12-13 NO NO170967A patent/NO118878B/no unknown
-
1968
- 1968-12-06 US US781962A patent/US3607811A/en not_active Expired - Lifetime
- 1968-12-11 GB GB58911/68A patent/GB1188219A/en not_active Expired
- 1968-12-12 DE DE19681814137 patent/DE1814137A1/de active Pending
- 1968-12-12 SE SE17020/68A patent/SE334030B/xx unknown
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| US10290004B1 (en) | 2017-12-02 | 2019-05-14 | M-Fire Suppression, Inc. | Supply chain management system for supplying clean fire inhibiting chemical (CFIC) totes to a network of wood-treating lumber and prefabrication panel factories and wood-framed building construction job sites |
| US10311444B1 (en) | 2017-12-02 | 2019-06-04 | M-Fire Suppression, Inc. | Method of providing class-A fire-protection to wood-framed buildings using on-site spraying of clean fire inhibiting chemical liquid on exposed interior wood surfaces of the wood-framed buildings, and mobile computing systems for uploading fire-protection certifications and status information to a central database and remote access thereof by firefighters on job site locations during fire outbreaks on construction sites |
| US10332222B1 (en) | 2017-12-02 | 2019-06-25 | M-Fire Supression, Inc. | Just-in-time factory methods, system and network for prefabricating class-A fire-protected wood-framed buildings and components used to construct the same |
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Also Published As
| Publication number | Publication date |
|---|---|
| SE334030B (enrdf_load_stackoverflow) | 1971-04-05 |
| DE1814137A1 (de) | 1969-06-19 |
| NO118878B (enrdf_load_stackoverflow) | 1970-02-23 |
| GB1188219A (en) | 1970-04-15 |
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