CN107474539A - Environmental protection flame retardant heat-barrier material and preparation method thereof - Google Patents
Environmental protection flame retardant heat-barrier material and preparation method thereof Download PDFInfo
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- CN107474539A CN107474539A CN201710690523.7A CN201710690523A CN107474539A CN 107474539 A CN107474539 A CN 107474539A CN 201710690523 A CN201710690523 A CN 201710690523A CN 107474539 A CN107474539 A CN 107474539A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/0023—Use of organic additives containing oxygen
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- 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
- C08J9/0028—Use of organic additives containing nitrogen
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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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
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
- C08J9/008—Nanoparticles
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- 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
- C08J9/0085—Use of fibrous compounding ingredients
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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
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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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
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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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
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Polymers & Plastics (AREA)
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- Paints Or Removers (AREA)
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Abstract
The invention discloses a kind of environmental protection flame retardant heat-barrier material and preparation method thereof, the preparation method includes：Nano silicon and silane coupler are mixed, mixed liquor M is obtained after ultrasonic disperse；Mixed liquor M, epoxy resin, oleic acid, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and ethylene glycol are mixed, foamed technique obtains the environmental protection flame retardant heat-barrier material；Solve that existing inorganic material is although heat-resisting, good flame retardation effect, but tiny fiber be present, not only polluted air but also easy breed bacteria, it has also become the problem of endangering the hidden danger of health of people.
Description
Technical field
The present invention relates to environment-friendly materials, in particular it relates to a kind of environmental protection flame retardant heat-barrier material and preparation method thereof.
Background technology
The fire disaster accident caused by architecture exterior wall insulating materials are burnt constantly causes serious in recent years
Casualties and property loss, build inflammable flammable external-wall heat-insulation material has turned into a kind of new disaster hidden-trouble.And existing nothing
Machine material is although heat-resisting, good flame retardation effect, but tiny fiber be present, has not only polluted air but also easy breed bacteria, it has also become harm
The hidden danger of health of people.
Therefore it provides a kind of have splendid fire protecting performance, and to the less environmental protection flame retardant heat-barrier material of Health Impact
And preparation method thereof the problem of being urgent need to resolve of the present invention.
The content of the invention
It is an object of the invention to provide a kind of environmental protection flame retardant heat-barrier material and preparation method thereof, solves existing inorganic material
Although expecting heat-resisting, good flame retardation effect, tiny fiber be present, not only polluted air but also easy breed bacteria, it has also become endanger people
The problem of hidden danger of health.
To achieve these goals, the invention provides a kind of preparation method of environmental protection flame retardant heat-barrier material, the preparation
Method includes：
（1）Nano silicon and silane coupler are mixed, mixed liquor M is obtained after ultrasonic disperse；
（2）By mixed liquor M, epoxy resin, oleic acid, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and second two
Alcohol mixes, and foamed technique obtains the environmental protection flame retardant heat-barrier material；
Wherein, relative to the nano silicon of 100 parts by weight, the dosage of silane coupler is 300-400 parts by weight；
Relative to the mixed liquor M of 100 parts by weight, the dosage of epoxy resin is 20-40 parts by weight, and the dosage of oleic acid is 5-10 weight
Part, the dosage of inorfil is 5-12 parts by weight, and the dosage of diethylenetriamine is 2-8 parts by weight, and the dosage of carbon material is 10-20
Parts by weight, the dosage of dispersant is 1-2 parts by weight, and the dosage of bonding agent is 1-2 parts by weight, and the dosage of ethylene glycol is 40-80 weights
Measure part.
Present invention also offers a kind of environmental protection flame retardant heat-barrier material, the environmental protection flame retardant heat-barrier material is by above-mentioned preparation side
Method is made.
Pass through above-mentioned technical proposal, the invention provides a kind of preparation method of environmental protection flame retardant heat-barrier material, the preparation
Method includes：Nano silicon and silane coupler are mixed, mixed liquor M is obtained after ultrasonic disperse；By mixed liquor M, epoxy
Resin, oleic acid, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and ethylene glycol mixing, foamed technique obtain
The environmental protection flame retardant heat-barrier material；Pass through the synergy between each raw material so that obtained environmental protection flame retardant heat-barrier material possesses
Excellent fire resistance and heat-proof quality, while the method for preparing the environmental protection flame retardant heat-barrier material is simple, raw material is easy to get.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The end points of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
The invention provides a kind of preparation method of environmental protection flame retardant heat-barrier material, the preparation method includes：
（1）Nano silicon and silane coupler are mixed, mixed liquor M is obtained after ultrasonic disperse；
（2）By mixed liquor M, epoxy resin, oleic acid, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and second two
Alcohol mixes, and foamed technique obtains the environmental protection flame retardant heat-barrier material；
Wherein, relative to the nano silicon of 100 parts by weight, the dosage of silane coupler is 300-400 parts by weight；
Relative to the mixed liquor M of 100 parts by weight, the dosage of epoxy resin is 20-40 parts by weight, and the dosage of oleic acid is 5-10 weight
Part, the dosage of inorfil is 5-12 parts by weight, and the dosage of diethylenetriamine is 2-8 parts by weight, and the dosage of carbon material is 10-20
Parts by weight, the dosage of dispersant is 1-2 parts by weight, and the dosage of bonding agent is 1-2 parts by weight, and the dosage of ethylene glycol is 40-80 weights
Measure part.
In a kind of preferred embodiment of the present invention, in order to further improve the fire resistance of obtained material and every
Hot property, relative to the nano silicon of 100 parts by weight, the dosage of silane coupler is 350-380 parts by weight；
Relative to the mixed liquor M of 100 parts by weight, the dosage of epoxy resin is 25-35 parts by weight, and the dosage of oleic acid is 7-8 weight
Part, the dosage of inorfil is 8-10 parts by weight, and the dosage of diethylenetriamine is 4-6 parts by weight, and the dosage of carbon material is 13-17
Parts by weight, the dosage of dispersant is 1.3-1.6 parts by weight, and the dosage of bonding agent is 1.3-1.6 parts by weight, and the dosage of ethylene glycol is
50-70 parts by weight.
In a kind of preferred embodiment of the present invention, in order to further improve the fire resistance of obtained material and every
Hot property, one or more of the inorfil in glass fibre, aluminium silicate fiber peacekeeping rock mineral wool fiber.
In a kind of preferred embodiment of the present invention, in order to further improve the fire resistance of obtained material and every
Hot property, one or more of the carbon material in graphite, activated carbon and charcoal powder.
In a kind of preferred embodiment of the present invention, in order to further improve the fire resistance of obtained material and every
Hot property, the dispersant is in triethanolamine oleate, coconut oil diethanol amide and detergent alkylate APEO
It is one or more.
In a kind of preferred embodiment of the present invention, in order to further improve the fire resistance of obtained material and every
Hot property, one or more of the bonding agent in vinyl acetate emulsion, silicone acrylic emulsion and styrene-acrylic emulsion.
In a kind of preferred embodiment of the present invention, in order to further improve the fire resistance of obtained material and every
Hot property, in step（1）In, the condition of ultrasonic disperse includes：The frequency of ultrasonic disperse is 5-10kHz, the time of ultrasonic disperse
For 5-10min.
In a kind of preferred embodiment of the present invention, in order to further improve the fire resistance of obtained material and every
Hot property, in step（2）In, the condition of foam process includes：The temperature of foaming is 300-500 DEG C, and the time of foaming is 1-2h.
Present invention also offers a kind of environmental protection flame retardant heat-barrier material, the environmental protection flame retardant heat-barrier material is by above-mentioned preparation side
Method is made.
The present invention will be described in detail by way of examples below.
Embodiment 1
100g nano silicons and 350g silane couplers are mixed, ultrasonic disperse（The frequency of ultrasonic disperse is 5kHz, ultrasound
The scattered time is 5min）After obtain mixed liquor M；By 100g mixed liquor M, 25g epoxy resin, 7g oleic acid, 8g glass fibres, 4g
Diethylenetriamine, 13g graphite, 1.3g triethanolamine oleates, 1.3g vinyl acetate emulsions and the mixing of 50g ethylene glycol, it is foamed
Technique（The temperature of foaming is 300 DEG C, and the time of foaming is 1h）Obtain the environmental protection flame retardant heat-barrier material A1.
Embodiment 2
100g nano silicons and 380g silane couplers are mixed, ultrasonic disperse（The frequency of ultrasonic disperse is 10kHz, is surpassed
The sound scattered time is 10min）After obtain mixed liquor M；By 100g mixed liquor M, 35g epoxy resin, 8g oleic acid, 10g alumina silicate
Fiber, 6g diethylenetriamines, 17g activated carbons, 1.6g coconut oil diethanol amides, 1.6g silicone acrylic emulsions and the mixing of 70g ethylene glycol,
Foamed technique（The temperature of foaming is 500 DEG C, and the time of foaming is 2h）Obtain the environmental protection flame retardant heat-barrier material A2.
Embodiment 3
100g nano silicons and 365g silane couplers are mixed, ultrasonic disperse（The frequency of ultrasonic disperse is 8kHz, ultrasound
The scattered time is 7min）After obtain mixed liquor M；100g mixed liquor M, 30g epoxy resin, 7.5g oleic acid, 9g rocks mineral wool is fine
Dimension, 5g diethylenetriamines, 15g charcoal powders, 1.4g detergent alkylates APEO, 1.4g styrene-acrylic emulsions and 60g ethylene glycol mix
Close, foamed technique（The temperature of foaming is 400 DEG C, and the time of foaming is 1.5h）Obtain the environmental protection flame retardant heat-barrier material A3.
Embodiment 4
It is prepared by the method according to embodiment 3, unlike, relative to 100g nano silicon, silane coupler
Dosage is 350g；Relative to 100g mixed liquor M, the dosage of epoxy resin is 25g, and the dosage of oleic acid is 7g, inorfil
Dosage is 8g, and the dosage of diethylenetriamine is 4g, and the dosage of carbon material is 13g, and the dosage of dispersant is 1.3g, the use of bonding agent
Measure as 1.3g, the dosage of ethylene glycol is 50g, obtains environmental protection flame retardant heat-barrier material A4.
Embodiment 5
It is prepared by the method according to embodiment 3, unlike, relative to 100g nano silicon, silane coupler
Dosage is 380g；Relative to 100g mixed liquor M, the dosage of epoxy resin is 35g, and the dosage of oleic acid is 8g, inorfil
Dosage is 10g, and the dosage of diethylenetriamine is 6g, and the dosage of carbon material is 17g, and the dosage of dispersant is 1.6g, bonding agent
Dosage is 1.6g, and the dosage of ethylene glycol is 70g, obtains environmental protection flame retardant heat-barrier material A5.
Comparative example 1
It is prepared by the method according to embodiment 3, unlike, relative to 100g nano silicon, silane coupler
Dosage is 320g；Relative to 100g mixed liquor M, the dosage of epoxy resin is 20g, and the dosage of oleic acid is 5g, inorfil
Dosage is 5g, and the dosage of diethylenetriamine is 2g, and the dosage of carbon material is 10g, and the dosage of dispersant is 1.1g, the use of bonding agent
Measure as 1.1g, the dosage of ethylene glycol is 40g, obtains environmental protection flame retardant heat-barrier material D1.
Comparative example 2
It is prepared by the method according to embodiment 3, unlike, relative to 100g nano silicon, silane coupler
Dosage is 400g；Relative to 100g mixed liquor M, the dosage of epoxy resin is 38g, and the dosage of oleic acid is 10g, inorfil
Dosage is 12g, and the dosage of diethylenetriamine is 8g, and the dosage of carbon material is 20g, and the dosage of dispersant is 1.8g, bonding agent
Dosage is 1.8g, and the dosage of ethylene glycol is 80g, obtains environmental protection flame retardant heat-barrier material D2.
Test case
Obtained environmental protection flame retardant heat-barrier material A1-A5, D1 and D2 are carried out into compression strength, thermal conductivity factor and burning velocity to survey
It is fixed.
Table 1
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited to the tool in above-mentioned embodiment
Body details, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, these letters
Monotropic type belongs to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (9)
1. a kind of preparation method of environmental protection flame retardant heat-barrier material, it is characterised in that the preparation method includes：
（1）Nano silicon and silane coupler are mixed, mixed liquor M is obtained after ultrasonic disperse；
（2）By mixed liquor M, epoxy resin, oleic acid, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and second two
Alcohol mixes, and foamed technique obtains the environmental protection flame retardant heat-barrier material；
Wherein, relative to the nano silicon of 100 parts by weight, the dosage of silane coupler is 300-400 parts by weight；
Relative to the mixed liquor M of 100 parts by weight, the dosage of epoxy resin is 20-40 parts by weight, and the dosage of oleic acid is 5-10 weight
Part, the dosage of inorfil is 5-12 parts by weight, and the dosage of diethylenetriamine is 2-8 parts by weight, and the dosage of carbon material is 10-20
Parts by weight, the dosage of dispersant is 1-2 parts by weight, and the dosage of bonding agent is 1-2 parts by weight, and the dosage of ethylene glycol is 40-80 weights
Measure part.
2. preparation method according to claim 1, wherein, it is silane coupled relative to the nano silicon of 100 parts by weight
The dosage of agent is 350-380 parts by weight；
Relative to the mixed liquor M of 100 parts by weight, the dosage of epoxy resin is 25-35 parts by weight, and the dosage of oleic acid is 7-8 weight
Part, the dosage of inorfil is 8-10 parts by weight, and the dosage of diethylenetriamine is 4-6 parts by weight, and the dosage of carbon material is 13-17
Parts by weight, the dosage of dispersant is 1.3-1.6 parts by weight, and the dosage of bonding agent is 1.3-1.6 parts by weight, and the dosage of ethylene glycol is
50-70 parts by weight.
3. preparation method according to claim 1 or 2, wherein, the inorfil is selected from glass fibre, alumina silicate fibre
With the one or more in rock mineral wool fiber.
4. preparation method according to claim 1 or 2, wherein, the carbon material is in graphite, activated carbon and charcoal powder
One or more.
5. preparation method according to claim 1 or 2, wherein, the dispersant is selected from triethanolamine oleate, coconut oil two
One or more in glycollic amide and detergent alkylate APEO.
6. preparation method according to claim 1 or 2, wherein, the bonding agent is selected from vinyl acetate emulsion, the breast of silicon third
One or more in liquid and styrene-acrylic emulsion.
7. preparation method according to claim 1 or 2, wherein, in step（1）In, the condition of ultrasonic disperse includes：Ultrasound
Scattered frequency is 5-10kHz, and the time of ultrasonic disperse is 5-10min.
8. preparation method according to claim 1 or 2, wherein, in step（2）In, the condition of foam process includes：Foaming
Temperature be 300-500 DEG C, the time of foaming is 1-2h.
9. a kind of environmental protection flame retardant heat-barrier material, it is characterised in that the environmental protection flame retardant heat-barrier material is by any in claim 1-8
Preparation method described in one is made.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710690523.7A CN107474539A (en) | 2017-08-14 | 2017-08-14 | Environmental protection flame retardant heat-barrier material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710690523.7A CN107474539A (en) | 2017-08-14 | 2017-08-14 | Environmental protection flame retardant heat-barrier material and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001048067A2 (en) * | 1999-11-09 | 2001-07-05 | Jiffy Foam, Incorporated | Novolac-epoxy resin foam |
| CN105001600A (en) * | 2014-04-24 | 2015-10-28 | 沈阳航空航天大学 | Preparation method of flame-retardant epoxy foamed material |
| CN106699225A (en) * | 2016-12-12 | 2017-05-24 | 天津红光京建科技有限公司 | Flame-retardant heat-retaining board and production method thereof |
-
2017
- 2017-08-14 CN CN201710690523.7A patent/CN107474539A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001048067A2 (en) * | 1999-11-09 | 2001-07-05 | Jiffy Foam, Incorporated | Novolac-epoxy resin foam |
| CN105001600A (en) * | 2014-04-24 | 2015-10-28 | 沈阳航空航天大学 | Preparation method of flame-retardant epoxy foamed material |
| CN106699225A (en) * | 2016-12-12 | 2017-05-24 | 天津红光京建科技有限公司 | Flame-retardant heat-retaining board and production method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 宋波: "《塑料改性技术》", 30 October 2016, 中国纺织出版社 * |
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Application publication date: 20171215 |