CN106810655A - A kind of phenol formaldehyde foam for carrying 3 aminopropyl pentamethyl disiloxanes and preparation method thereof - Google Patents
A kind of phenol formaldehyde foam for carrying 3 aminopropyl pentamethyl disiloxanes and preparation method thereof Download PDFInfo
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- CN106810655A CN106810655A CN201611205366.8A CN201611205366A CN106810655A CN 106810655 A CN106810655 A CN 106810655A CN 201611205366 A CN201611205366 A CN 201611205366A CN 106810655 A CN106810655 A CN 106810655A
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- 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
- C08G8/28—Chemically modified polycondensates
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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
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- 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
- C08L61/14—Modified phenol-aldehyde condensates
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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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
- 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
- C08J2361/14—Modified phenol-aldehyde condensates
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
A kind of phenol formaldehyde foam for carrying 3 aminopropyl pentamethyl disiloxanes and preparation method thereof, is related to a kind of phenol formaldehyde foam and preparation method thereof, and the present invention is made up of following part:Phenolic compound, aldehyde compound, catalyst, modifying agent, surfactant, foaming agent, curing agent.After by phenolic compound, catalyst, aldehyde compound reaction, the aminopropyl pentamethyl disiloxane of modifying agent 3 is added, obtain thick liquid, the phenolic foam resin with 3 aminopropyl pentamethyl disiloxanes;Phenol-formaldehyde resin modified is placed in stand-by in container, in surfactant, foaming agent are weighed successively, adding container, then load weighted curing agent is poured into container, after the completion of shaping to be foamed, mould taken out, form removal, that is, obtain phenolic foam board.The present invention provide phenol formaldehyde foam heat resistance and dimensional stability be improved significantly, with good pliability and combination property.
Description
Technical field
It is more particularly to a kind of to carry 3- aminopropyl pentamethyls the present invention relates to a kind of phenol formaldehyde foam and preparation method thereof
Phenol formaldehyde foam of disiloxane and preparation method thereof.
Background technology
The aspect such as low smokiness, hypotoxicity and dimensional stability when phenolic foam is with its thermal insulation, flame retardancy, burning
Excellent characteristic is taken seriously again, and its technical research and application and development are active again, and oneself is through turning into " insulation material
New candidate ".But phenol formaldehyde foam fragility is big, easy efflorescence, hinders its application development.Therefore traditional phenol formaldehyde foam can not be fitted
The need for Vehicles Collected from Market is answered to high-performance toughness foam, the toughness and heat resistance of foam are improved, be phenolic resin foam thermal insulating material
The current primary study direction of material.
The patent of invention of Publication No. CN 104151556A discloses a kind of preparation of polyborosiloxane and to phenolic resin
Heat resistance modified method, obtain resistant to elevated temperatures phenoweld, polycondensation is carried out by terminal hydroxy group and phenolic resin
Reaction, improves its heat endurance and adhesion strength, but although the introducing of phenyl ring improves heat resistance, but fragility can be made further to become
Greatly, the use scope of phenolic resin is limited.
The content of the invention
It is an object of the invention to provide a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes and its system
Preparation Method, the present invention is to carry out chemical modification to phenolic resin as modifying agent using 3- aminopropyls pentamethyl disiloxane,
Terminal hydroxy group in 3- aminopropyl pentamethyl disiloxanes can carry out polycondensation reaction with the phenolic hydroxyl group in phenolic resin, serve
The effect of intrinsic toughening, introduces siloxanes in traditional phenolic resin, and system heat resistance is greatly enhanced, while increasing master
Chain, improves the fragility of phenolic resin, and the phenol formaldehyde foam obtained by foamed solidification has excellent heat resistance and mechanical property.
The purpose of the present invention is achieved through the following technical solutions:
A kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, with following structure:
。
A kind of described phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, resins synthesis stage each component is pressed
Weight meter, by phenolic compound, 100 parts, aldehyde compound 45-85 parts, catalyst 1-6 parts, modifying agent 8-20 parts constitute;Resin
Foaming stages, each component by weight, by 100 parts of modified phenolic resin, surfactant 2-15 parts, foaming agent 8-16 parts,
Curing agent 10-20 parts of composition.
A kind of described phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, the phenolic compound is benzene
One or more in phenol, cresols, dimethyl phenol, nonyl phenol, bisphenol-A, resorcinol, propylphenol and ethyl -phenol, it is excellent
Elect phenol as.
A kind of described phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, the aldehyde compound is selected from first
One or more in aldehyde, acetaldehyde, butyraldehyde, polyformaldehyde and furfural.
A kind of described phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, the catalyst is hydroxide
One or more in the strong base substances such as sodium, potassium hydroxide.
A kind of described phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, described surfactant is to tell
At least one in temperature -80, Span, silicone oil.
A kind of described phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, described foaming agent is positive penta
At least one in alkane, isopentane.
A kind of described phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, described curing agent is to toluene
One or more in one or more sulfuric acid in sulfonic acid, xylene monosulfonic acid, phenolsulfonic acid, benzene sulfonic acid.
A kind of phenol formaldehyde foam preparation method with 3- aminopropyl pentamethyl disiloxanes, the preparation method includes following step
Suddenly:
Phenolic compound, catalyst, aldehyde compound are sequentially added in the reactor of about 60 ~ 80 DEG C of temperature, after reaction, are added
Modifying agent 3- aminopropyl pentamethyl disiloxanes, lead to N2Protection, 150 are to slowly warm up to the programming rate of 1~5 DEG C/min ~
180 DEG C, room temperature is cooled to after constant temperature stirring 1.5-2.5h;In system in acetic acid and resin liquid is neutral, is then removed under reduced pressure
Small molecule is until no liquid discharge, obtains thick liquid, the phenolic foam resin with 3- aminopropyl pentamethyl disiloxanes;
Phenol-formaldehyde resin modified is placed in it is stand-by in container, successively weigh surfactant, foaming agent, add container in, quickly stir
Mix, stir 1-3 minutes, then load weighted curing agent is poured into container, stir 1-2 minutes, the liquid that then will be stirred falls
In entering mould, mould is put into 60-80 DEG C of baking oven carries out foaming, after the completion of shaping to be foamed, mould is taken out, is torn open
Mould, that is, obtaining phenolic foam board carries out performance test.
Advantages of the present invention is with effect:
1. the present invention is to carry out chemical modification, 3- to phenolic resin as modifying agent using 3- aminopropyls pentamethyl disiloxane
Terminal hydroxy group in aminopropyl pentamethyl disiloxane can carry out polycondensation reaction with the phenolic hydroxyl group in phenolic resin, serve interior
The effect of toughness reinforcing, introduces siloxanes in traditional phenolic resin, and system heat resistance is greatly enhanced, while increasing master
Chain, improves the fragility of phenolic resin, and the phenol formaldehyde foam obtained by foamed solidification has excellent heat resistance and mechanical property.
2. preparation process is simple of the invention, reaction time be short, raw material is easy to get.
3. the present invention is for fields such as adiabatic heat-insulation and sound insulations.Especially as heat-insulating material, it is in building, oil
The fields such as chemical industry, medical and health and Shipping.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
With reference to specific implementation example, the present invention will be further described, not limiting of its scope.Simultaneously
Experimental technique described in following embodiments, unless otherwise specified, is conventional method;The reagent and material, such as without special
Illustrate, commercially obtain.
Embodiment is raw materials used as follows:
Paraformaldehyde
NaOH
3- aminopropyl pentamethyl disiloxanes
Acetic acid
Tween-80
Pentane
Benzene sulfonic acid
Embodiment 1
The present invention is a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, is comprised the following steps:
65g phenol solutions, 0.65g NaOH, 35g paraformaldehydes are sequentially added in the reactor of about 60 ~ 80 DEG C of temperature, instead
After answering 1h, 5.2g 3- aminopropyl pentamethyl disiloxanes are added, lead to N2Protection, is slowly heated up with the programming rate of 3 DEG C/min
To 150 ~ 180 DEG C, room temperature is cooled to after constant temperature stirring 1.5-2.5h.With neutral with resin liquid in acetic acid, body is then removed under reduced pressure
Small molecule in system is until no liquid discharge, obtains thick liquid, a kind of phenolic aldehyde with 3- aminopropyl pentamethyl disiloxanes
Foamex.
By phenolic foam resin, Tween-80, pentane:Benzene sulfonic acid is by proportioning 100:12:10:12 ratio is carried out fully
Uniform mixing, quickly stirs 1min, and then mixed material is transferred in mould, is reacted 10 minutes at 70 DEG C, and the demoulding is
Obtaining phenolic foam board carries out performance test.
Embodiment 2
The present invention is a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, is comprised the following steps:
65g phenol solutions, 0.65g NaOH, 35g paraformaldehydes are sequentially added in the reactor of about 60 ~ 80 DEG C of temperature, instead
After answering 1h, 6.5g 3- aminopropyl pentamethyl disiloxanes are added, lead to N2Protection, is slowly heated up with the programming rate of 3 DEG C/min
To 150 ~ 180 DEG C, room temperature is cooled to after constant temperature stirring 1.5-2.5h.With neutral with resin liquid in acetic acid, body is then removed under reduced pressure
Small molecule in system is until no liquid discharge, obtains thick liquid, a kind of phenolic aldehyde with 3- aminopropyl pentamethyl disiloxanes
Foamex.
By phenolic foam resin, Tween-80, pentane:Benzene sulfonic acid is by proportioning 100:12:10:12 ratio is carried out fully
Uniform mixing, quickly stirs 1min, and then mixed material is transferred in mould, is reacted 10 minutes at 70 DEG C, and the demoulding is
Obtaining phenolic foam board carries out performance test.
Embodiment 3
The present invention is a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, is comprised the following steps:
65g phenol solutions, 0.65g NaOH, 35g paraformaldehydes are sequentially added in the reactor of about 60 ~ 80 DEG C of temperature, instead
After answering 1h, 9.8g 3- aminopropyl pentamethyl disiloxanes are added, lead to N2Protection, is slowly heated up with the programming rate of 3 DEG C/min
To 150 ~ 180 DEG C, room temperature is cooled to after constant temperature stirring 1.5-2.5h.With neutral with resin liquid in acetic acid, body is then removed under reduced pressure
Small molecule in system is until no liquid discharge, obtains thick liquid, a kind of phenolic aldehyde with 3- aminopropyl pentamethyl disiloxanes
Foamex.
By phenolic foam resin, Tween-80, pentane:Benzene sulfonic acid is by proportioning 100:12:10:12 ratio is carried out fully
Uniform mixing, quickly stirs 1min, and then mixed material is transferred in mould, is reacted 10 minutes at 70 DEG C, and the demoulding is
Obtaining phenolic foam board carries out performance test.
Comparative example
65g phenol solutions, 0.65g NaOH, 35g paraformaldehydes are sequentially added in the reactor of about 60 ~ 80 DEG C of temperature, instead
After answering 1h, 150 ~ 180 DEG C are to slowly warm up to the programming rate of 3 DEG C/min, room temperature is cooled to after constant temperature stirring 1.5-2.5h.With
It is neutral with resin liquid in acetic acid, the small molecule in system is then removed under reduced pressure until no liquid discharge, obtains basic expandability phenolic aldehyde
Resin.
By phenolic foam resin, Tween-80, pentane:Benzene sulfonic acid is by proportioning 100:12:10:12 ratio is carried out fully
Uniform mixing, quickly stirs 1min, and then mixed material is transferred in mould, is reacted 10 minutes at 70 DEG C, and the demoulding is
Obtaining phenolic foam board carries out performance test.
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 to phenolic resin using 3- aminopropyl pentamethyl disiloxanes as modifying agent
Learn modified, it is anti-that the terminal hydroxy group in 3- aminopropyl pentamethyl disiloxanes can carry out polycondensation with the phenolic hydroxyl group in phenolic resin
Should, the effect of intrinsic toughening is served, siloxanes is introduced in traditional phenolic resin, system heat resistance is greatly enhanced, together
When increase main chain, improve the fragility of phenolic resin, the modified phenolic foam rate of closed hole obtained by foamed solidification is shown
Writing improves, and carbon yield is high, shock resistance is good, hardness is suitable, has widened the range of application of phenolic resin.
Exemplary 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 that method of the present invention design and technical scheme are carried out are employed, or not improved general
Design of the invention and technical scheme directly apply to other occasions, within the scope of the present invention.
Claims (9)
1. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes, it is characterised in that with following structure:
。
2. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes according to claim 1, its feature exists
In, resins synthesis stage each component by weight, by 100 parts of phenolic compound, aldehyde compound 45-85 parts, catalyst 1-6
Part, modifying agent 8-20 parts of composition;Resin expanded stage, each component by weight, is lived by 100 parts of modified phenolic resin, surface
Property 2-15 parts of agent, foaming agent 8-16 parts, curing agent 10-20 parts composition.
3. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes according to claim 2, its feature exists
In the phenolic compound is phenol, cresols, dimethyl phenol, nonyl phenol, bisphenol-A, resorcinol, propylphenol and ethyl
One or more in phenol, preferably phenol.
4. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes according to claim 2, its feature exists
In the aldehyde compound is selected from one or more in formaldehyde, acetaldehyde, butyraldehyde, polyformaldehyde and furfural.
5. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes according to claim 2, its feature exists
In the catalyst is one or more in the strong base substances such as NaOH, potassium hydroxide.
6. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes according to claim 2, its feature exists
In described surfactant is at least one in Tween-80, Span, silicone oil.
7. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes according to claim 2, its feature exists
In described foaming agent is at least one in pentane, isopentane.
8. a kind of phenol formaldehyde foam with 3- aminopropyl pentamethyl disiloxanes according to claim 2, its feature exists
In described curing agent is in one or more sulfuric acid in p-methyl benzenesulfonic acid, xylene monosulfonic acid, phenolsulfonic acid, benzene sulfonic acid
One or more.
9. a kind of phenol formaldehyde foam preparation method with 3- aminopropyl pentamethyl disiloxanes, it is characterised in that the preparation
Method is comprised the following steps:
Phenolic compound, catalyst, aldehyde compound are sequentially added in the reactor of about 60 ~ 80 DEG C of temperature, after reaction, are added
Modifying agent 3- aminopropyl pentamethyl disiloxanes, lead to N2Protection, 150 are to slowly warm up to the programming rate of 1~5 DEG C/min ~
180 DEG C, room temperature is cooled to after constant temperature stirring 1.5-2.5h;In system in acetic acid and resin liquid is neutral, is then removed under reduced pressure
Small molecule is until no liquid discharge, obtains thick liquid, the phenolic foam resin with 3- aminopropyl pentamethyl disiloxanes;
Phenol-formaldehyde resin modified is placed in it is stand-by in container, successively weigh surfactant, foaming agent, add container in, quickly stir
Mix, stir 1-3 minutes, then load weighted curing agent is poured into container, stir 1-2 minutes, the liquid that then will be stirred falls
In entering mould, mould is put into 60-80 DEG C of baking oven carries out foaming, after the completion of shaping to be foamed, mould is taken out, is torn open
Mould, that is, obtaining phenolic foam board carries out performance test.
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Cited By (1)
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---|---|---|---|---|
WO2023060153A1 (en) * | 2021-10-06 | 2023-04-13 | Dow Global Technologies Llc | Preparation of amino-functional organosilicon compounds |
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