CN107022182A - A kind of inorganic nano flame-retardance unsaturated resin composite and preparation method thereof - Google Patents
A kind of inorganic nano flame-retardance unsaturated resin composite and preparation method thereof Download PDFInfo
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- CN107022182A CN107022182A CN201710346768.8A CN201710346768A CN107022182A CN 107022182 A CN107022182 A CN 107022182A CN 201710346768 A CN201710346768 A CN 201710346768A CN 107022182 A CN107022182 A CN 107022182A
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/06—Unsaturated polyesters
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/91—Polymers modified by chemical after-treatment
- C08G63/914—Polymers modified by chemical after-treatment derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/918—Polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- General Chemical & Material Sciences (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The present invention relates to a kind of inorganic nano flame-retardance unsaturated resin composite and preparation method thereof, described unsaturated-resin composite is made by the following method：3 15 parts of 30 60 parts of unsaturated polyester resin, 40 70 parts of inorganic nanometer powder fire retardant and end phosphoric acid polyester hyper-dispersant are weighed in proportion, stirring mixing, add 1.5 2.0 parts of 0.6 1.2 parts of cobalt naphthenate accelerator and initiator methyl ethyl ketone peroxide, blended under agitation is uniform, pour into again in mould, curing molding is to obtain purpose product unsaturated-resin composite.Compared with prior art, the present invention can using the end phosphoric acid polyester hyper-dispersant reduction inorganic nanometer powder fire retardant surface of certain molecular chain length, improve it dispersed in unsaturated-resin, so as to reduce compound system viscosity, improve processing and the mechanical property of compound system, in addition, end phosphoric acid polyester also has the effect of cooperative flame retardant, its addition makes the fire-retardant performance of composite be further improved.
Description
Technical field
It is multiple more particularly, to a kind of inorganic nano flame-retardance unsaturated resin the present invention relates to Polymer Synthesizing and blending field
Condensation material and preparation method thereof.
Background technology
In many high polymer materials, unsaturated-resin (UPR) is due to its easily fabrication process condition and cheap valency
Lattice and as the class thermosetting resin that is widely used, it can be by being heating and curing or a variety of types are made in the method for normal temperature cure
Material (mainly fiberglass), but this kind of material easily burns, when be often accompanied by fire, caused not to human life and property
Appreciable loss, therefore the fire resistance of raising unsaturated-resin seems more urgent.
Addition fire retardant is most directly effective method, and with the raising of mankind's environmental consciousness, the exploitation of fire retardant is not only
Need performance more excellent, at the same the environmental issue during fire retardant itself and use it is also proposed it is more strict will
Ask.Composite, non-halogen, suppression fuming, the flame-retardant system of low toxicity have become the trend of 21 century fire retardant overall development, and
Inorganic combustion inhibitor because with combustion products toxicity is small, low cigarette or it is smokeless, do not ooze out, do not migrate, permanent fire retardant, it is free from environmental pollution,
With low cost the features such as, meet the main trend that fire retardant develops to environment-friendly type, it has also become the Main way of flame-retarded technology development.But
It is that compatibility of the inorganic based flame retardant when in use with high polymer is poor, it is difficult to dispersed in high polymer, and only exists
Addition could have good flame retardant effect when larger, but adding too much can make system have higher viscosity, influence material
The processing characteristics of material simultaneously makes its mechanical performance significantly decline.The key for solving this problem is the fineness for improving fire retardant with this
Increase the adhesion and the dispersiveness in high polymer of its effective menu area and enhancing fire retardant and high polymer.Enhancing
The method of adhesion and dispersiveness mainly carries out surface modification to fire retardant, to improve the physicochemical characteristics on its surface, increases
It is strong its with matrix be organic polymer compatibility and its dispersiveness in organic substrate, and then the processability of raising material
Energy.The modification to inorganic combustion inhibitor mainly passes through the surface modifiers such as coupling agent, surfactant, unsaturated organic acid at present
In the absorption of particle surface, cladding, react with film forming etc. and realize.Chinese patent ZL201310211136.2 discloses a kind of nothing
Machine flame-retardance unsaturated resin, by the material composition of following weight percentage：Nanometer inorganic flame retardant 40-50%, viscosity reduction disperses
Auxiliary agent 1-5%, surplus is unsaturated-resin.Above-mentioned viscosity reducing dispersing auxiliary by following weight percentage material composition：Propylene
Acid esters 60-83%, acrylic acid 1-5%, initiator 6-15%, chain-transferring agent 10-20%.The patent uses esters of acrylic acid viscosity reduction
Dispersing aid is combined unsaturated-resin matrix, and serving certain improve compound system processing mechanical property and improve fire resistance
Effect, but be not still particularly pertinent.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of inorganic nano is fire-retardant
Unsaturated-resin composite and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of inorganic nano flame-retardance unsaturated resin composite, includes the component of following parts by weight：Inorganic nanometer-powder
40-70 parts of body fire retardant, 3-15 parts of end phosphoric acid polyester hyper-dispersant, 30-60 parts of unsaturated-resin.
It is preferred that, the particle diameter of described inorganic nanometer powder fire retardant is 80nm~800nm, and described end phosphoric acid polyester surpasses
The molecular weight of dispersant is 600-3000.
It is preferred that, the particle diameter of described inorganic nanometer powder fire retardant is corresponding with holding the molecular weight of phosphoric acid polyester hyper-dispersant
It is applicable.Wherein, when the particle diameter of inorganic nanometer powder fire retardant is 80nm~250nm, the molecular weight of phosphoric acid polyester hyper-dispersant is held
Correspondence uses 600-1000；When the particle diameter of inorganic nanometer powder fire retardant is 250nm~500nm, phosphoric acid polyester hyper-dispersant is held
Molecular weight correspondence use 1000-2000；When the particle diameter of inorganic nanometer powder fire retardant is 500nm~800nm, phosphoric acid polyester is held
The molecular weight correspondence of hyper-dispersant uses 2000-3000.(molecular weight of the invention refers to number-average molecular weight)
The molecular weight of end phosphoric acid polyester hyper-dispersant determines the length of solvent chain, the main function of solvent chain be
Nano-meter flame retardantses powder granule surface forms certain thickness protective layer, and it is the main part in hyper-dispersant molecular structure,
The adsorbent layer thickness that hyper-dispersant is formed on nano-meter flame retardantses surface is determined, thus largely determines its scattered effect
Really.If hyper-dispersant molecular weight is too small, solvent chain is too short, and not enough, its corresponding steric barrier is not enough to adsorbent layer thickness
Attracting each other between particle is overcome, so that the flocculation between particle can not effectively be hindered.But solvent chain is oversize,
Solvent chain can be produced to fold in particle surface, compression stroke steric hindrance layer；The entanglement of solvent chain occurs between particle, leads
Cause particle flocculation；Solvation of the unsaturated-resin to solvent chain is larger, and larger to anchoring group generation pulls away power, draws
Play the harmful effects such as anchoring group desorption.
Needed for the stabilized protection course that end phosphoric acid polyester hyper-dispersant is formed on the nano-meter flame retardantses powder of different-grain diameter
The length of solvent chain is that molecular weight is different, and the present invention verifies the corresponding pass for drawing the above by theoretical calculation Binding experiment
System.
It is preferred that, described inorganic nanometer powder fire retardant is aluminium hydroxide, magnesium hydroxide；
Described unsaturated-resin is unsaturated polyester resin.
It is preferred that, described end phosphoric acid polyester hyper-dispersant is monoester type end monoesters, diester-type or mixing ester type end phosphoric acid
Polyester hyper-dispersant, it is made up of following steps：
(1) (0.1-0.6) mol is pressed：(1-2)mol：1g takes caproic acid, maleic anhydride and catalyst benzyl triethyl ammonium chlorine
Change ammonium mixing, be heated to 120 DEG C, then expoxy propane 1.5-2.5mol is added dropwise, react 2h, obtain solvent chain terminal hydroxy group and gather
(maleic anhydride-expoxy propane) ester；
(2) at 70 DEG C, poly- (maleic anhydride-expoxy propane) ester of solvent chain terminal hydroxy group made from step (1) is taken
With phosphorus pentoxide 2-4 in molar ratio:1 mixing, is warming up to 90 DEG C, reacts 6h, that is, obtains purpose product end monoesters end monoesters, end
Dibasic acid esters or mixed ester end phosphoric acid polyester hyper-dispersant.
The consumption of initiator acetic acid determines hyper-dispersant in the synthesis technique of above-mentioned end phosphoric acid polyester hyper-dispersant
Molecular weight, poly- (maleic anhydride-expoxy propane) ester of solvent chain terminal hydroxy group determines super in molar ratio with phosphorus pentoxide
The quantity of the anchoring group of dispersant., can be according to poly- to acetic acid, and solvent chain terminal hydroxy group in specific experiment preparation
(maleic anhydride-expoxy propane) ester and phosphorus pentoxide control the molecular weight and kind of hyper-dispersant respectively in molar ratio
Class.
The preparation method of inorganic nano flame-retardance unsaturated resin composite, comprises the following steps：
30-60 parts of unsaturated polyester resin, 40-70 parts of inorganic nanometer powder fire retardant and end phosphoric acid polyester are weighed in proportion
3-15 parts of hyper-dispersant, stirring mixing, adds 0.6-1.2 parts of cobalt naphthenate accelerator and initiator methyl ethyl ketone peroxide 1.5-
2.0 parts, blended under agitation is uniform, then pours into mould, and curing molding is to obtain purpose product unsaturated-resin composite.Promote
Agent and initiator are the basic recipe of the universal unsaturated-resin solidification of normal temperature.
Existing surface modifier uses small molecule, there is cladding not exclusively, adsorbs not firm enough defect.This hair
Two parts that bright hyper-dispersant is completely dispensed with by function：Anchoring group and solvent chain composition.Anchoring group can be with particle
The highly polar group on surface is combined in the form of ion pair, is firmly adsorbed with nano-meter flame retardantses particle surface, of the invention
End phosphate has stronger anchorage effect to nano-aluminum hydroxide and nano-sized magnesium hydroxide；Solvent chain can be in unsaturated polyester (UP) tree
There is good compatibility, the present invention have selected poly- (maleic anhydride-expoxy propane) ester of terminal hydroxy group for solvation in fat
Chain, its structure and unsaturated polyester resin (UPR) are very much like, thus have good compatibility with unsaturated-resin, and are formed
Certain thickness protective layer, effectively prevents the reunion of nano flame retardant powder granule, plays scattered effect.
Compared with prior art, the present invention reduces inorganic receive using the end phosphoric acid polyester hyper-dispersant of certain molecular chain length
Ground rice body fire retardant surface energy, improves its dispersiveness in unsaturated-resin and is filled so as to reduce the height by matrix of unsaturated-resin
Inorganic nanometer powder fire retardant compound system viscosity, improves processing and the mechanical property of compound system.In addition, end phosphoric acid polyester
Also there is the effect of cooperative flame retardant, its addition makes the inorganic fire-retarded fire-retardant performance of unsaturated-resin composite further be carried
It is high.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Raw material in following embodiment and comparative example, unless otherwise noted, using conventional commercial product.
Monoester type end monoesters, diester-type or mixing ester type end phosphoric acid polyester hyper-dispersant employed in following each embodiments
It is made up of following steps：
(1) (0.1-0.6) mol is pressed：(1-2)mol：1g takes caproic acid, maleic anhydride and catalyst benzyl triethyl ammonium chlorine
Change ammonium mixing, be heated to 120 DEG C, then expoxy propane 1.5-2.5mol is added dropwise, react 2h, obtain solvent chain terminal hydroxy group and gather
(maleic anhydride-expoxy propane) ester；
(2) at 70 DEG C, poly- (maleic anhydride-expoxy propane) ester of solvent chain terminal hydroxy group made from step (1) is taken
With phosphorus pentoxide in molar ratio 2:1-4:1 mixing, is warming up to 90 DEG C, reacts 6h, that is, obtain purpose product end monoesters end monoesters,
Hold dibasic acid esters or mixed ester end phosphoric acid polyester hyper-dispersant.
Embodiment 1
The material that the present embodiment is provided is formulated by weight proportion by following raw material：
It is by raw material proportioning that unsaturated polyester resin (UPR), nano-meter flame retardantses aluminium hydroxide and end phosphoric acid polyester is ultra-dispersed
Agent is mixed, and 5min is stirred with reinforcement agitator, and system is triggered using normal temperature, is added cobalt naphthenate accelerator by raw material proportioning and is drawn
Agent methyl ethyl ketone peroxide is sent out, the blend stirred is poured into preprepared sample mould, curing molding.
Comparative example 1-1
A kind of unsaturated-resin composite, is made by the following method：
It is by raw material proportioning that unsaturated polyester resin (UPR), nano-meter flame retardantses aluminium hydroxide and end phosphoric acid polyester is ultra-dispersed
Agent is mixed, and 5min is stirred with reinforcement agitator, and system is triggered using normal temperature, is added cobalt naphthenate accelerator by raw material proportioning and is drawn
Agent methyl ethyl ketone peroxide is sent out, the blend stirred is poured into preprepared sample mould, curing molding.
Comparative example 1-2
A kind of unsaturated-resin composite, is made by the following method：
It is by raw material proportioning that unsaturated polyester resin (UPR), nano-meter flame retardantses aluminium hydroxide and end phosphoric acid polyester is ultra-dispersed
Agent is mixed, and 5min is stirred with reinforcement agitator, adds benzoyl peroxide by raw material proportioning, the blend stirred is poured into
In preprepared sample mould, curing molding.
Embodiment 2
The material that the present embodiment is provided is formulated by weight proportion by following raw material：
It is by raw material proportioning that unsaturated polyester resin (UPR), nano-meter flame retardantses magnesium hydroxide and end phosphoric acid polyester is ultra-dispersed
Agent is mixed, and 5min is stirred with reinforcement agitator, and system is triggered using normal temperature, is added cobalt naphthenate accelerator by raw material proportioning and is drawn
Agent methyl ethyl ketone peroxide is sent out, the blend stirred is poured into preprepared sample mould, curing molding.
Comparative example 2-1
A kind of unsaturated-resin composite, is made by the following method：
It is by raw material proportioning that unsaturated polyester resin (UPR), nano-meter flame retardantses aluminium hydroxide and end phosphoric acid polyester is ultra-dispersed
Agent is mixed, and 5min is stirred with reinforcement agitator, and system is triggered using normal temperature, is added cobalt naphthenate accelerator by raw material proportioning and is drawn
Agent methyl ethyl ketone peroxide is sent out, the blend stirred is poured into preprepared sample mould, curing molding.
Embodiment 3
The material that the present embodiment is provided is formulated by weight proportion by following raw material：
First nano-meter flame retardantses aluminium hydroxide and end phosphoric acid polyester hyper-dispersant are mixed by raw material proportioning, insatiable hunger is then added
In polyester resin (UPR), 5min is stirred with reinforcement agitator, system is triggered using normal temperature, aphthenic acids is added by raw material proportioning
Cobalt accelerator and initiator methyl ethyl ketone peroxide, the blend stirred is poured into preprepared sample mould, Gu
Chemical conversion type.
Embodiment 4
The material that the present embodiment is provided is formulated by weight proportion by following raw material：
First nano-meter flame retardantses magnesium hydroxide and end phosphoric acid polyester hyper-dispersant are mixed by raw material proportioning, insatiable hunger is then added
In polyester resin (UPR), 5min is stirred with reinforcement agitator, system is triggered using normal temperature, aphthenic acids is added by raw material proportioning
Cobalt accelerator and initiator methyl ethyl ketone peroxide, the blend stirred is poured into preprepared sample mould, Gu
Chemical conversion type.
The performance of the embodiment of table 1. and comparative example
Analyze comparative example 1 and comparative example 1-1, comparative example 1-2, embodiment 2 and comparative example 2-1, it is known that, for difference
The inorganic nanometer powder fire retardant of particle diameter, can all have the molecular weight of the end phosphoric acid polyester hyper-dispersant of a most suitable scope right with it
Should, if the molecular weight of end phosphoric acid polyester hyper-dispersant is not in the range of restriction, such as molecular weight is excessive or too small, can cause multiple
The impact strength and system oxygen index (OI) of condensation material system have more obvious decline.Therefore, the fire-retardant unsaturated tree of inorganic nano
The performance of resin composite material system is related to the molecular weight of the particle diameter of nanometer inorganic flame retardant and hyper-dispersant.
Embodiment 5
The material that the present embodiment is provided is formulated by weight proportion by following raw material：
First nano-meter flame retardantses magnesium hydroxide and end phosphoric acid polyester hyper-dispersant are mixed by raw material proportioning, insatiable hunger is then added
In polyester resin (UPR), 5min is stirred with reinforcement agitator, system is triggered using normal temperature, aphthenic acids is added by raw material proportioning
Cobalt accelerator and initiator methyl ethyl ketone peroxide, the blend stirred is poured into preprepared sample mould, Gu
Chemical conversion type.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel are according to the announcement of the present invention, and not departing from improvement and modification that scope made all should be the present invention's
Within protection domain.
Claims (6)
1. a kind of inorganic nano flame-retardance unsaturated resin composite, it is characterised in that include the component of following parts by weight：Nothing
40-70 parts of machine nano-powder fire retardant, 3-15 parts of end phosphoric acid polyester hyper-dispersant, 30-60 parts of unsaturated-resin.
2. a kind of inorganic nano flame-retardance unsaturated resin composite according to claim 1, it is characterised in that described
The particle diameter of inorganic nanometer powder fire retardant is 80nm~800nm, and the molecular weight of described end phosphoric acid polyester hyper-dispersant is 600-
3000。
3. a kind of inorganic nano flame-retardance unsaturated resin composite according to claim 2, it is characterised in that described
The particle diameter of inorganic nano packet fire retardant is corresponding with holding the molecular weight of phosphoric acid polyester hyper-dispersant to be applicable, wherein, work as inorganic nano
The particle diameter of powder fire retardant is 80nm~250nm, and the molecular weight correspondence of end phosphoric acid polyester hyper-dispersant uses 600-1000；Work as nothing
The particle diameter of machine nano-powder fire retardant is 250nm~500nm；The molecular weight correspondence of end phosphoric acid polyester hyper-dispersant uses 1000-
2000；When the particle diameter of inorganic nanometer powder fire retardant is 500nm~800nm, the molecular weight correspondence of end phosphoric acid polyester hyper-dispersant
Using 2000-3000.
4. a kind of inorganic nano flame-retardance unsaturated resin composite according to claim 1, it is characterised in that described
Inorganic nanometer powder fire retardant is aluminium hydroxide, magnesium hydroxide；
Described unsaturated-resin is unsaturated polyester resin.
5. a kind of inorganic nano flame-retardance unsaturated resin composite according to claim 1, it is characterised in that described
It is monoester type end monoesters, diester-type or mixing ester type end phosphoric acid polyester hyper-dispersant to hold phosphoric acid polyester hyper-dispersant, its by with
Lower step is made：
(1) (0.1-0.6) mol is pressed：(1-2)mol：1g takes caproic acid, maleic anhydride and catalyst benzyltriethylammoinium chloride
Mixing, is heated to 120 DEG C, then expoxy propane 1.5-2.5mol is added dropwise, and reacts 2h, obtains solvent chain terminal hydroxy group poly- (suitable
Anhydride maleique-expoxy propane) ester；
(2) at 70 DEG C, poly- (maleic anhydride-expoxy propane) ester and five of solvent chain terminal hydroxy group made from step (1) is taken
Aoxidize two phosphorus 2-4 in molar ratio:1 mixing, is warming up to 90 DEG C, reacts 6h, that is, obtains purpose product end monoesters end monoesters, end dibasic acid esters
Or mixed ester end phosphoric acid polyester hyper-dispersant.
6. the preparation method of the inorganic nano flame-retardance unsaturated resin composite as described in claim 1-5 is any, its feature
It is, comprises the following steps：
30-60 parts of unsaturated polyester resin, 40-70 parts of inorganic nanometer powder fire retardant and end phosphoric acid polyester oversubscription are weighed in proportion
3-15 parts of powder, stirring mixing, adds 0.6-1.2 parts of cobalt naphthenate accelerator and initiator methyl ethyl ketone peroxide 1.5-2.0
Part, blended under agitation is uniform, then pours into mould, and curing molding is to obtain purpose product unsaturated-resin composite.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110643160A (en) * | 2019-09-25 | 2020-01-03 | 徐州吉瑞合金铸造有限公司 | More stable composite die base material |
| CN111378263A (en) * | 2018-12-28 | 2020-07-07 | 浙江荣泰科技企业有限公司 | Single-component halogen-free flame-retardant insulating impregnating resin and preparation method thereof |
| CN116041619A (en) * | 2023-01-28 | 2023-05-02 | 安徽科柏特复合材料科技有限公司 | Unsaturated resin and preparation method and application thereof |
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| CN116041619A (en) * | 2023-01-28 | 2023-05-02 | 安徽科柏特复合材料科技有限公司 | Unsaturated resin and preparation method and application thereof |
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Application publication date: 20170808 |