CN106496470B - A kind of phenol formaldehyde foam and preparation method thereof of 3- nitros -4- hydroxyethylaminophenol formaldehyde - Google Patents
A kind of phenol formaldehyde foam and preparation method thereof of 3- nitros -4- hydroxyethylaminophenol formaldehyde Download PDFInfo
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- CN106496470B CN106496470B CN201610837500.XA CN201610837500A CN106496470B CN 106496470 B CN106496470 B CN 106496470B CN 201610837500 A CN201610837500 A CN 201610837500A CN 106496470 B CN106496470 B CN 106496470B
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- formaldehyde
- hydroxyethylaminophenol
- foam
- nitros
- phenol
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000006260 foam Substances 0.000 claims abstract description 23
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 22
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- -1 aldehyde compound Chemical class 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000004088 foaming agent Substances 0.000 claims abstract description 7
- 150000002989 phenols Chemical class 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000005187 foaming Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 19
- 239000005011 phenolic resin Substances 0.000 claims description 15
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- UXKLYBMQAHYULT-UHFFFAOYSA-N 4-(2-hydroxyethylamino)-3-nitrophenol Chemical class OCCNC1=CC=C(O)C=C1[N+]([O-])=O UXKLYBMQAHYULT-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 6
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 6
- 229920000053 polysorbate 80 Polymers 0.000 claims description 6
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 4
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 150000003384 small molecules Chemical class 0.000 claims description 3
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 229940044654 phenolsulfonic acid Drugs 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 3
- 238000001802 infusion Methods 0.000 claims 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 5
- 239000011810 insulating material Substances 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Natural products O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract 2
- XMVJITFPVVRMHC-UHFFFAOYSA-N roxarsone Chemical group OC1=CC=C([As](O)(O)=O)C=C1[N+]([O-])=O XMVJITFPVVRMHC-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 8
- 229920002866 paraformaldehyde Polymers 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229930040373 Paraformaldehyde Natural products 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- JOLVYUIAMRUBRK-UHFFFAOYSA-N 11',12',14',15'-Tetradehydro(Z,Z-)-3-(8-Pentadecenyl)phenol Natural products OC1=CC=CC(CCCCCCCC=CCC=CCC=C)=C1 JOLVYUIAMRUBRK-UHFFFAOYSA-N 0.000 description 1
- YLKVIMNNMLKUGJ-UHFFFAOYSA-N 3-Delta8-pentadecenylphenol Natural products CCCCCCC=CCCCCCCCC1=CC=CC(O)=C1 YLKVIMNNMLKUGJ-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JOLVYUIAMRUBRK-UTOQUPLUSA-N Cardanol Chemical compound OC1=CC=CC(CCCCCCC\C=C/C\C=C/CC=C)=C1 JOLVYUIAMRUBRK-UTOQUPLUSA-N 0.000 description 1
- FAYVLNWNMNHXGA-UHFFFAOYSA-N Cardanoldiene Natural products CCCC=CCC=CCCCCCCCC1=CC=CC(O)=C1 FAYVLNWNMNHXGA-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- BKUYVGOACRJHQO-UHFFFAOYSA-N benzenesulfonic acid;sulfuric acid Chemical compound OS(O)(=O)=O.OS(=O)(=O)C1=CC=CC=C1 BKUYVGOACRJHQO-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- PTFIPECGHSYQNR-UHFFFAOYSA-N cardanol Natural products CCCCCCCCCCCCCCCC1=CC=CC(O)=C1 PTFIPECGHSYQNR-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/16—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with amino- or nitrophenols
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Abstract
A kind of phenol formaldehyde foam and preparation method thereof of 3 nitro, 4 hydroxyethylaminophenol formaldehyde is related to a kind of phenol formaldehyde foam and preparation method thereof, present invention composition：Phenolic compound, aldehyde compound, catalyst, surfactant, foaming agent, curing agent.The modified phenolic foam of gained is by phenol-formaldehyde resin modified, surfactant, and foaming agent is uniformly mixed by certain proportioning, adds curing agent and is uniformly mixed, pours into mold, and certain temperature foaming, demoulding obtains target phenol formaldehyde foam.Phenol formaldehyde foam heat resistance and dimensional stability provided by the invention be improved significantly, have good mechanical property and comprehensive performance.It is mainly used for the fields such as adiabatic heat-insulation and sound insulation.Especially as heat-insulating material, in fields such as building, petrochemical industry, medical and health and Shippings.
Description
Technical field
The present invention relates to a kind of phenol formaldehyde foams and preparation method thereof, more particularly to a kind of 3- nitros -4- hydroxyethylaminos
Phenol formaldehyde foam of phenol formaldehyde (PF) and preparation method thereof.
Background technology
Phenolic foam is with low smokiness, hypotoxicity and dimensional stability when its thermal insulation, flame retardancy, burning etc.
Excellent characteristic is taken seriously again, and technical research and application and development are active again, oneself is through becoming " thermal insulation material
New candidate ".But the release of the small molecules such as water or ammonia is had in phenol formaldehyde foam solidification process, when curing molding generally require plus
Pressure leads to the big brittleness of foam, easy dusting, has hole, therefore hinders its application development.Current existing technology is all in toughening
While lead to the decline of fire protecting performance, or increase cost.Therefore traditional phenol formaldehyde foam does not adapt to Vehicles Collected from Market to height
The needs of performance toughness foam improve the toughness and heat resistance of foam, are that the current emphasis of phenolic resin foam thermal insulation material is ground
Study carefully direction.
Patent 103923285A provides a kind of nitrogenous phenolic resin of modified by cardanol, the phenolic aldehyde which provides
Not only included anacardol side group in the structure of resin, but also has contained N element, it is brittle existing for prior art phenolic resin overcoming
While defect, the high temperature resistance of phenolic resin is improved, but this method reaction time is long, it is less efficient.
Invention content
The purpose of the present invention is to provide a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde and its preparations
Method, the present invention are the phenol replaced using 3- nitro -4- hydroxyethylaminophenols in traditional phenolic resin, with paraformaldehyde into
Row addition and polycondensation introduce nitro in traditional phenolic resin, and system heat resistance is greatly enhanced, while reducing phenolic aldehyde
The brittleness of foam has excellent heat resistance and mechanical property by the phenol formaldehyde foam that foamed solidification obtains.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, monomer have the following structure：
。
A kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, resins synthesis stage each component are pressed
Weight meter by 100 parts of phenolic compound, 45-85 parts of aldehyde compound, 1-6 parts of catalyst, forms；Resin expanded stage, each group
Divide by weight, by 100 parts of modified phenolic resin, 2-15 parts of surfactant, 8-16 parts of foaming agent, 10-20 parts of curing agent
Composition.
A kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, the phenolic compound are 3- nitre
Base -4- hydroxyethylaminophenols.
A kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, the aldehyde compound are selected from first
It is one or more in aldehyde, acetaldehyde, butyraldehyde, polyformaldehyde and furfural.
A kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, the catalyst are sodium hydroxide, hydrogen
It is one or more in the strong base substances such as potassium oxide.
A kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, the surfactant are to spit
At least one of temperature -80, Span, silicone oil.
A kind of phenol formaldehyde foam of the 3- nitros -4- hydroxyethylaminophenol formaldehyde, the foaming agent be pentane,
At least one of isopentane.
A kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, the curing agent are to toluene
It is one or more in one or more of sulfonic acid, xylene monosulfonic acid, phenolsulfonic acid, benzene sulfonic acid sulfuric acid.
A kind of phenol formaldehyde foam preparation method of 3- nitros -4- hydroxyethylaminophenol formaldehyde, the preparation method include with
Lower step：
Quantitative phenolic compound, catalyst, aldehyde compound are sequentially added in the reaction kettle of about 60 ~ 80 DEG C of temperature,
After reacting a period of time, 150 ~ 180 DEG C are to slowly warm up to the heating rate of 1~5 DEG C/min, constant temperature stirs cold after 1.5-2.5h
But to room temperature；With in acetic acid and resin liquid is neutral, the small molecule in system is then removed under reduced pressure until no liquid is discharged, obtain sticky
Liquid, a kind of phenolic resin of 3- nitros -4- hydroxyethylaminophenol formaldehyde；
Phenol-formaldehyde resin modified is placed in container for use, surfactant is weighed successively, foaming agent, is added to the container, soon
Speed stirring, is stirred 1-3 minutes, then load weighted curing agent is poured into container, is stirred 1-2 minutes, the liquid that then will be stirred
Body pours into mold, mold is put into 60-80 DEG C of baking oven and carries out foaming, and after the completion of molding to be foamed, mold is taken
Go out, form removal is tested for the property to get to phenolic foam board.
Advantages of the present invention is with effect：
Present invention is mainly used for the fields such as adiabatic heat-insulation and sound insulation.Especially as heat-insulating material, in building, stone
The fields such as oiling work, medical and health and Shipping.
The present invention is the phenol replaced using 3- nitro -4- hydroxyethylaminophenols in traditional phenolic resin, with poly first
Aldehyde carries out addition and polycondensation, nitro is introduced in traditional phenolic resin, system heat resistance is greatly enhanced, reduces simultaneously
The brittleness of phenol formaldehyde foam has excellent heat resistance and mechanical property by the phenol formaldehyde foam that foamed solidification obtains.
The preparation process of the present invention is simple, reaction time is short, raw material is easy to get.
Specific implementation mode
The following describes the present invention in detail with reference to examples.
With reference to specific implementation example, the present invention will be further described, not limiting of its scope.Simultaneously
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as without special
Illustrate, commercially obtains.
Embodiment is raw materials used as follows：
3- nitro -4- hydroxyethylaminophenols
Paraformaldehyde
Sodium hydroxide
Acetic acid
Tween-80
Pentane
Benzene sulfonic acid
Embodiment 1
The present invention is a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, is included the following steps：
65g 3- nitro -4- hydroxyethylaminophenols solution, the sodium hydroxide solution 0.65g that mass fraction is 50% are added
Enter into 60 DEG C of three-necked flask, after mixing, react 5min, then weighs 35g paraformaldehydes in flask, react 1h
Afterwards, 150 DEG C are to slowly warm up to the heating rate of 3 DEG C/min, constant temperature stirs 1.5 postcoolings to room temperature.With in acetic acid and resin
For neutrality, target phenolic foam resin is obtained.
By phenolic foam resin, Tween-80, pentane：Benzene sulfonic acid according to the ratio 100：12：10：12 ratio carries out abundant
Uniformly mixing, quickly stirs 1min, then mixed material is transferred in mold, reacted 10 minutes at 70 DEG C, demoulding is
Phenolic foam board is obtained to be tested for the property.
Embodiment 2
The present invention is a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, is included the following steps：
65g 3- nitro -4- hydroxyethylaminophenols solution, the sodium hydroxide solution 0.65g that mass fraction is 50% are added
Enter into 60 DEG C of three-necked flask, after mixing, react 5min, then weighs 40g paraformaldehydes in flask, react 1h
Afterwards, 150 DEG C are to slowly warm up to the heating rate of 3 DEG C/min, constant temperature stirs 1.5 postcoolings to room temperature.With in acetic acid and resin
For neutrality, target phenolic foam resin is obtained.
By phenolic foam resin, Tween-80, pentane：Benzene sulfonic acid according to the ratio 100：12：10：12 ratio carries out abundant
Uniformly mixing, quickly stirs 1min, then mixed material is transferred in mold, reacted 10 minutes at 70 DEG C, demoulding is
Phenolic foam board is obtained to be tested for the property.
Embodiment 3
The present invention is a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, is included the following steps：
65g 3- nitro -4- hydroxyethylaminophenols solution, the sodium hydroxide solution 0.65g that mass fraction is 50% are added
Enter into 60 DEG C of three-necked flask, after mixing, react 5min, then weighs 45g paraformaldehydes in flask, react 1h
Afterwards, 150 DEG C are to slowly warm up to the heating rate of 3 DEG C/min, constant temperature stirs 1.5 postcoolings to room temperature.With in acetic acid and resin
For neutrality, target phenolic foam resin is obtained.
By phenolic foam resin, Tween-80, pentane：Benzene sulfonic acid according to the ratio 100：12：10：12 ratio carries out abundant
Uniformly mixing, quickly stirs 1min, then mixed material is transferred in mold, reacted 10 minutes at 70 DEG C, demoulding is
Phenolic foam board is obtained to be tested for the property.
Comparative example
65g phenol solutions, the sodium hydroxide solution 0.65g that mass fraction is 50% are added in 60 DEG C of three-necked flask,
After mixing, 5min is reacted, 35g paraformaldehydes are then weighed in flask, after reacting 1h, with the heating rate of 3 DEG C/min
90 DEG C are to slowly warm up to, constant temperature stirs 1.5 postcoolings to room temperature.With in acetic acid and resin is neutral, basic phenolic foam is obtained
Resin.
By phenolic foam resin, Tween-80, pentane：Benzene sulfonic acid according to the ratio 100：12：10：12 ratio carries out abundant
Uniformly mixing, quickly stirs 1min, then mixed material is transferred in mold, reacted 10 minutes at 70 DEG C, demoulding is
Phenolic foam board is obtained to be tested for the property.
The performance comparison such as following table of phenol-formaldehyde resin modified and phenolic resin prepared by the embodiment of the present invention：
。
As seen from the above table, the present invention is the benzene replaced using 3- nitro -4- hydroxyethylaminophenols in traditional phenolic resin
Phenol carries out addition and polycondensation with paraformaldehyde, nitro is introduced in traditional phenolic resin, system heat resistance is carried significantly
Height, while the brittleness of phenol formaldehyde foam is reduced, and the toughness of phenolic resin is improved, the modified phenolic obtained by foamed solidification
Foam carbon yield is high, shock resistance is good, hardness is suitable, has widened the application range of phenolic resin.
Illustrative description is carried out to the present invention above in conjunction with specific embodiment, it is clear that realization of the invention is not by upper
The limitation of mode is stated, if the various improvement of inventive concept and technical scheme of the present invention progress are used, or not improved general
The design and technical solution of the present invention directly applies to other occasions, is within the scope of the invention.
Claims (9)
1. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde, which is characterized in that monomer has following knot
Structure：
。
2. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde according to claim 1, feature exist
By weight in, resins synthesis stage each component, by 100 parts of phenolic compound, 45-85 parts of aldehyde compound, catalyst 1-6
Part, composition；Resin expanded stage, each component by weight, by 100 parts of modified phenolic resin, 2-15 parts of surfactant, are sent out
10-20 parts of 8-16 parts of infusion, curing agent compositions.
3. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde according to claim 2, feature exist
In the phenolic compound is 3- nitro -4- hydroxyethylaminophenols.
4. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde according to claim 2, feature exist
In the aldehyde compound is one or more in formaldehyde, acetaldehyde, butyraldehyde, furfural.
5. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde according to claim 2, which is characterized in that
The catalyst is one or more in sodium hydroxide, potassium hydroxide strong base substance.
6. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde according to claim 2, feature exist
In the surfactant is at least one of Tween-80, Span, silicone oil.
7. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde according to claim 2, feature exist
In the foaming agent is at least one of pentane, isopentane.
8. a kind of phenol formaldehyde foam of 3- nitros -4- hydroxyethylaminophenol formaldehyde according to claim 2, feature exist
In the curing agent is one or more of p-methyl benzenesulfonic acid, xylene monosulfonic acid, phenolsulfonic acid, benzene sulfonic acid.
9. a kind of phenol formaldehyde foam preparation method of 3- nitros -4- hydroxyethylaminophenol formaldehyde, which is characterized in that the preparation side
Method includes the following steps：
Quantitative phenolic compound, catalyst, aldehyde compound are sequentially added in the reaction kettle of 60 ~ 80 DEG C of temperature, reaction one
After the section time, 150 ~ 180 DEG C are to slowly warm up to the heating rate of 1~5 DEG C/min, constant temperature stirs 1.5-2.5h postcoolings to room
Temperature；It is discharged up to no liquid with resin liquid neutrality, the small molecule being then evaporated under reduced pressure in the system of removing in acetic acid, obtained 3- nitre
The phenolic resin of base -4- hydroxyethylaminophenol formaldehyde；
Phenol-formaldehyde resin modified is placed in container for use, surfactant is weighed successively, foaming agent, is added to the container, quickly stir
It mixes, stirs 1-3 minutes, then load weighted curing agent is poured into container, stir 1-2 minutes, then fall the liquid being stirred
Enter in mold, mold is put into 60-80 DEG C of baking oven and carries out foaming, after the completion of molding to be foamed, mold is taken out, is torn open
Mould is tested for the property to get to phenolic foam board.
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| CN1955206A (en) * | 2005-10-28 | 2007-05-02 | 上海尖端工程材料有限公司 | Synthesing of low normal temp foamable phenolic resin and method for preparing phenolic foam |
| CN101768326A (en) * | 2010-01-15 | 2010-07-07 | 上海虞城新型建材有限公司 | Preparation method of modified phenolic resin and application thereof |
| CN102532799A (en) * | 2011-12-30 | 2012-07-04 | 华东理工大学华昌聚合物有限公司 | Temperature-resistant high-strength expandable phenolic resin and foam preparation method thereof |
| CN103013038A (en) * | 2012-12-27 | 2013-04-03 | 北京莱恩斯高新技术有限公司 | Cardanol modified phenolic aldehyde foam and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1955206A (en) * | 2005-10-28 | 2007-05-02 | 上海尖端工程材料有限公司 | Synthesing of low normal temp foamable phenolic resin and method for preparing phenolic foam |
| CN101768326A (en) * | 2010-01-15 | 2010-07-07 | 上海虞城新型建材有限公司 | Preparation method of modified phenolic resin and application thereof |
| CN102532799A (en) * | 2011-12-30 | 2012-07-04 | 华东理工大学华昌聚合物有限公司 | Temperature-resistant high-strength expandable phenolic resin and foam preparation method thereof |
| CN103013038A (en) * | 2012-12-27 | 2013-04-03 | 北京莱恩斯高新技术有限公司 | Cardanol modified phenolic aldehyde foam and preparation method thereof |
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Application publication date: 20170315 Assignee: SHENYANG XINFEIYU RUBBER PRODUCTS CO.,LTD. Assignor: SHENYANG University OF CHEMICAL TECHNOLOGY Contract record no.: X2023210000283 Denomination of invention: Phenolic foam of 3-nitro-4-hydroxyethylaminophenol formaldehyde and its preparation method Granted publication date: 20180807 License type: Common License Record date: 20231205 |