CN107266855A - Based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material and preparation method thereof - Google Patents

Based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material and preparation method thereof Download PDF

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Publication number
CN107266855A
CN107266855A CN201710690535.XA CN201710690535A CN107266855A CN 107266855 A CN107266855 A CN 107266855A CN 201710690535 A CN201710690535 A CN 201710690535A CN 107266855 A CN107266855 A CN 107266855A
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weight
parts
consumption
preparation
retardant
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卢国孝
王斌
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Wuhu Kai Kai Mstar Technology Ltd
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Wuhu Kai Kai Mstar Technology Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/04Condensation polymers of aldehydes or ketones with phenols only
    • C08L61/06Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/14Applications used for foams
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Fireproofing Substances (AREA)

Abstract

The invention discloses a kind of based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material and preparation method thereof, the preparation method includes:Nano silicon and titanate coupling agent are mixed, mixed liquor M is obtained after ultrasonic disperse;Mixed liquor M, phenolic resin, triglycerides, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and acetone are mixed, foamed technique obtains the environment-friendlyflame-retardant flame-retardant material;Solve that existing inorganic material is although heat-resisting, good flame retardation effect, but there is tiny fiber, not only polluted air but also easy breed bacteria, it has also become the problem of the hidden danger of harm health of people.

Description

Based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material and preparation method thereof
Technical field
The present invention relates to environment-friendly materials, in particular it relates to a kind of based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material And preparation method thereof.
Background technology
Caused in recent years because fire disaster accident caused by architecture exterior wall insulating materials burning is continuous serious Casualties and property loss, build inflammable flammable external-wall heat-insulation material has turned into the new disaster hidden-trouble of a class.And existing nothing Machine material is although heat-resisting, good flame retardation effect, but there is tiny fiber, 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 nano silicon is based on to Health Impact is less The problem of modified environment-friendlyflame-retardant flame-retardant material and preparation method thereof is 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 based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material and preparation method thereof, Solve that existing inorganic material is although heat-resisting, good flame retardation effect, but there is tiny fiber, not only polluted air but also easily grown thin Bacterium, it has also become the problem of endangering the hidden danger of health of people.
To achieve these goals, the invention provides a kind of based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material Preparation method, the preparation method includes:
(1)Nano silicon and titanate coupling agent are mixed, mixed liquor M is obtained after ultrasonic disperse;
(2)By mixed liquor M, phenolic resin, triglycerides, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and Acetone is mixed, and foamed technique obtains the environment-friendlyflame-retardant flame-retardant material;
Wherein, relative to the nano silicon of 100 parts by weight, the consumption of titanate coupling agent is 300-400 parts by weight;
Relative to the mixed liquor M of 100 parts by weight, the consumption of phenolic resin is 20-40 parts by weight, and the consumption of triglycerides is 5-10 Parts by weight, the consumption of inorfil is 5-12 parts by weight, and the consumption of diethylenetriamine is 2-8 parts by weight, and the consumption of carbon material is 10-20 parts by weight, the consumption of dispersant is 1-2 parts by weight, and the consumption of bonding agent is 1-2 parts by weight, and the consumption of acetone is 40-80 Parts by weight.
It is described to be based on nano-silica present invention also offers a kind of based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material The environment-friendlyflame-retardant flame-retardant material that SiClx is modified is made by above-mentioned preparation method.
By above-mentioned technical proposal, the invention provides a kind of based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material Preparation method, the preparation method includes:Nano silicon and titanate coupling agent are mixed, mixed after ultrasonic disperse Liquid M;By mixed liquor M, phenolic resin, triglycerides, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and third Ketone is mixed, and foamed technique obtains the environment-friendlyflame-retardant flame-retardant material;Pass through the synergy between each raw material so that obtained environmental protection Fire proofing possesses excellent fire resistance and heat-proof quality, at the same it is simple for the method for preparing the environment-friendlyflame-retardant flame-retardant material, it is former Material is easy to get.
Other features and advantages of the present invention will be described in detail in subsequent embodiment part.
Embodiment
The embodiment to the present invention is described in detail below.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 and any value of disclosed scope 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 based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material, the preparation Method includes:
(1)Nano silicon and titanate coupling agent are mixed, mixed liquor M is obtained after ultrasonic disperse;
(2)By mixed liquor M, phenolic resin, triglycerides, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and Acetone is mixed, and foamed technique obtains the environment-friendlyflame-retardant flame-retardant material;
Wherein, relative to the nano silicon of 100 parts by weight, the consumption of titanate coupling agent is 300-400 parts by weight;
Relative to the mixed liquor M of 100 parts by weight, the consumption of phenolic resin is 20-40 parts by weight, and the consumption of triglycerides is 5-10 Parts by weight, the consumption of inorfil is 5-12 parts by weight, and the consumption of diethylenetriamine is 2-8 parts by weight, and the consumption of carbon material is 10-20 parts by weight, the consumption of dispersant is 1-2 parts by weight, and the consumption of bonding agent is 1-2 parts by weight, and the consumption of acetone is 40-80 Parts by weight.
The present invention it is a kind of preferred embodiment in, in order to further improve obtained material fire resistance and every Hot property, relative to the nano silicon of 100 parts by weight, the consumption of titanate coupling agent is 350-380 parts by weight;
Relative to the mixed liquor M of 100 parts by weight, the consumption of phenolic resin is 25-35 parts by weight, and the consumption of triglycerides is 7-8 Parts by weight, the consumption of inorfil is 8-10 parts by weight, and the consumption of diethylenetriamine is 4-6 parts by weight, and the consumption of carbon material is 13-17 parts by weight, the consumption of dispersant is 1.3-1.6 parts by weight, and the consumption of bonding agent is 1.3-1.6 parts by weight, the use of acetone Measure as 50-70 parts by weight.
The present invention it is a kind of preferred embodiment in, in order to further improve obtained material fire resistance and every Hot property, one or more of the inorfil in glass fibre, aluminium silicate fiber peacekeeping rock mineral wool fiber.
The present invention it is a kind of preferred embodiment in, in order to further improve obtained material fire resistance and every Hot property, one or more of the carbon material in graphite, activated carbon and charcoal powder.
The present invention it is a kind of preferred embodiment in, in order to further improve obtained material fire resistance and every Hot property, the dispersant is selected from triglycerides triethanolamine, coconut oil diethanol amide and detergent alkylate APEO In one or more.
The present invention it is a kind of preferred embodiment in, in order to further improve obtained material fire resistance and every Hot property, one or more of the bonding agent in vinyl acetate emulsion, silicone acrylic emulsion and styrene-acrylic emulsion.
The present invention it is a kind of preferred embodiment in, in order to further improve obtained material fire resistance 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.
The present invention it is a kind of preferred embodiment in, in order to further improve obtained material fire resistance 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.
It is described to be based on nano-silica present invention also offers a kind of based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material The environment-friendlyflame-retardant flame-retardant material that SiClx is modified is made by above-mentioned preparation method.
The present invention will be described in detail by way of examples below.
Embodiment 1
100g nano silicons and 350g titanate coupling agents are mixed, ultrasonic disperse(The frequency of ultrasonic disperse is 5kHz, is surpassed The sound scattered time is 5min)After obtain mixed liquor M;By 100g mixed liquor M, 25g phenolic resin, 7g triglycerides, 8g glass Fiber, 4g diethylenetriamines, 13g graphite, 1.3g triglycerides triethanolamine, 1.3g vinyl acetate emulsions and 50g acetone are mixed Close, foamed technique(The temperature of foaming is 300 DEG C, and the time of foaming is 1h)Obtain the environment-friendlyflame-retardant flame-retardant material A1.
Embodiment 2
100g nano silicons and 380g titanate coupling agents are mixed, ultrasonic disperse(The frequency of ultrasonic disperse is 10kHz, The time of ultrasonic disperse is 10min)After obtain mixed liquor M;By 100g mixed liquor M, 35g phenolic resin, 8g triglycerides, 10g Alumina silicate fibre, 6g diethylenetriamines, 17g activated carbons, 1.6g coconut oil diethanol amides, 1.6g silicone acrylic emulsions and 70g acetone Mixing, foamed technique(The temperature of foaming is 500 DEG C, and the time of foaming is 2h)Obtain the environment-friendlyflame-retardant flame-retardant material A2.
Embodiment 3
100g nano silicons and 365g titanate coupling agents are mixed, ultrasonic disperse(The frequency of ultrasonic disperse is 8kHz, is surpassed The sound scattered time is 7min)After obtain mixed liquor M;By 100g mixed liquor M, 30g phenolic resin, 7.5g triglycerides, 9g rocks Mineral wool fiber, 5g diethylenetriamines, 15g charcoal powders, 1.4g detergent alkylates APEO, 1.4g styrene-acrylic emulsions and 60g third Ketone is mixed, foamed technique(The temperature of foaming is 400 DEG C, and the time of foaming is 1.5h)Obtain the environment-friendlyflame-retardant flame-retardant material A3.
Embodiment 4
It is prepared by the method according to embodiment 3, unlike, the nano silicon relative to 100g, titanate coupling agent Consumption be 350g;Mixed liquor M relative to 100g, the consumption of phenolic resin is 25g, and the consumption of triglycerides is 7g, inorganic The consumption of fiber is 8g, and the consumption of diethylenetriamine is 4g, and the consumption of carbon material is 13g, and the consumption of dispersant is 1.3g, bonding The consumption of agent is 1.3g, and the consumption of acetone is 50g, obtains environment-friendlyflame-retardant flame-retardant material A4.
Embodiment 5
It is prepared by the method according to embodiment 3, unlike, the nano silicon relative to 100g, titanate coupling agent Consumption be 380g;Mixed liquor M relative to 100g, the consumption of phenolic resin is 35g, and the consumption of triglycerides is 8g, inorganic The consumption of fiber is 10g, and the consumption of diethylenetriamine is 6g, and the consumption of carbon material is 17g, and the consumption of dispersant is 1.6g, is glued The consumption for connecing agent is 1.6g, and the consumption of acetone is 70g, obtains environment-friendlyflame-retardant flame-retardant material A5.
Comparative example 1
It is prepared by the method according to embodiment 3, unlike, the nano silicon relative to 100g, titanate coupling agent Consumption be 320g;Mixed liquor M relative to 100g, the consumption of phenolic resin is 20g, and the consumption of triglycerides is 5g, inorganic The consumption of fiber is 5g, and the consumption of diethylenetriamine is 2g, and the consumption of carbon material is 10g, and the consumption of dispersant is 1.1g, bonding The consumption of agent is 1.1g, and the consumption of acetone is 40g, obtains environment-friendlyflame-retardant flame-retardant material D1.
Comparative example 2
It is prepared by the method according to embodiment 3, unlike, the nano silicon relative to 100g, titanate coupling agent Consumption be 400g;Mixed liquor M relative to 100g, the consumption of phenolic resin is 38g, and the consumption of triglycerides is 10g, inorganic The consumption of fiber is 12g, and the consumption of diethylenetriamine is 8g, and the consumption of carbon material is 20g, and the consumption of dispersant is 1.8g, is glued The consumption for connecing agent is 1.8g, and the consumption of acetone is 80g, obtains environment-friendlyflame-retardant flame-retardant material D2.
Test case
Obtained environment-friendlyflame-retardant flame-retardant material A1-A5, D1 and D2 are carried out into compression strength, thermal conductivity factor and burning velocity to determine.
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, can carry out a variety of simple variants, these letters to technical scheme 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 based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material, it is characterised in that the preparation side Method includes:
(1)Nano silicon and titanate coupling agent are mixed, mixed liquor M is obtained after ultrasonic disperse;
(2)By mixed liquor M, phenolic resin, triglycerides, inorfil, diethylenetriamine, carbon material, dispersant, bonding agent and Acetone is mixed, and foamed technique obtains the environment-friendlyflame-retardant flame-retardant material;
Wherein, relative to the nano silicon of 100 parts by weight, the consumption of titanate coupling agent is 300-400 parts by weight;
Relative to the mixed liquor M of 100 parts by weight, the consumption of phenolic resin is 20-40 parts by weight, and the consumption of triglycerides is 5-10 Parts by weight, the consumption of inorfil is 5-12 parts by weight, and the consumption of diethylenetriamine is 2-8 parts by weight, and the consumption of carbon material is 10-20 parts by weight, the consumption of dispersant is 1-2 parts by weight, and the consumption of bonding agent is 1-2 parts by weight, and the consumption of acetone is 40-80 Parts by weight.
2. preparation method according to claim 1, wherein, relative to the nano silicon of 100 parts by weight, titanate esters are even The consumption for joining agent is 350-380 parts by weight;
Relative to the mixed liquor M of 100 parts by weight, the consumption of phenolic resin is 25-35 parts by weight, and the consumption of triglycerides is 7-8 Parts by weight, the consumption of inorfil is 8-10 parts by weight, and the consumption of diethylenetriamine is 4-6 parts by weight, and the consumption of carbon material is 13-17 parts by weight, the consumption of dispersant is 1.3-1.6 parts by weight, and the consumption of bonding agent is 1.3-1.6 parts by weight, the use of acetone Measure as 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 triglycerides triethanolamine, coconut One or more in oily diglycollic 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, time of foaming is 1-2h.
9. it is a kind of based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material, it is characterised in that described to be based on nano silicon Modified environment-friendlyflame-retardant flame-retardant material is made as the preparation method described in any one in claim 1-8.
CN201710690535.XA 2017-08-14 2017-08-14 Based on nano-silicon dioxide modified environment-friendlyflame-retardant flame-retardant material and preparation method thereof Pending CN107266855A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107840605A (en) * 2017-11-09 2018-03-27 安徽艾米伦特建材科技有限公司 Anticracking motar and preparation method thereof

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DE10007977B4 (en) * 2000-02-22 2004-07-29 Hilti Ag Additive mixture to increase the fire resistance of plastic moldings, plastic moldings and a two-component system for their manufacture
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CN104194257A (en) * 2014-07-11 2014-12-10 蚌埠市天宇高温树脂材料有限公司 Glass-fiber reinforced molded plastic of heat-resistant environment-friendly phenolic resin
CN104744881A (en) * 2015-03-13 2015-07-01 芜湖航天特种电缆厂 Warping tape surface adhesion material and preparation method thereof as well as warping tape and preparation method thereof
CN106280231A (en) * 2016-08-12 2017-01-04 河南科技大学 A kind of sports equipment toughening modifying phenolic foam and preparation method thereof
CN106893259A (en) * 2015-12-17 2017-06-27 广东生益科技股份有限公司 A kind of compositions of thermosetting resin and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10007977B4 (en) * 2000-02-22 2004-07-29 Hilti Ag Additive mixture to increase the fire resistance of plastic moldings, plastic moldings and a two-component system for their manufacture
CN1390884A (en) * 2001-06-12 2003-01-15 中国科学院化学研究所 Process for preparing nano-class phenolic resin/day composition
CN102924870A (en) * 2012-11-28 2013-02-13 广东裕丰威禾电子科技股份有限公司 Low-density halogen-free flame retardant type high-strength composite material as well as preparation method and use thereof
CN104194257A (en) * 2014-07-11 2014-12-10 蚌埠市天宇高温树脂材料有限公司 Glass-fiber reinforced molded plastic of heat-resistant environment-friendly phenolic resin
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Application publication date: 20171020