CN106700440A - Heat-conducting flame-retardant polyester composite material and preparation method thereof - Google Patents
Heat-conducting flame-retardant polyester composite material and preparation method thereof Download PDFInfo
- Publication number
- CN106700440A CN106700440A CN201611175094.1A CN201611175094A CN106700440A CN 106700440 A CN106700440 A CN 106700440A CN 201611175094 A CN201611175094 A CN 201611175094A CN 106700440 A CN106700440 A CN 106700440A
- Authority
- CN
- China
- Prior art keywords
- heat
- polyester composite
- flame
- preparation
- magnesium hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/5205—Salts of P-acids with N-bases
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a heat-conducting flame-retardant polyester composite material and a preparation method thereof. The heat-conducting flame-retardant polyester composite material is characterized by comprising the following components in parts by weight: 100 parts of polyester resins, 100-300 parts of heat treated magnesium hydroxide, 0-50 parts of auxiliary heat conducting agents, 0-30 parts of auxiliary flame retardants, 1-8 parts of a dispersing agent and 1-3 parts of a stabilizer. According to the composite material disclosed by the invention, the heat treated magnesium hydroxide which has more excellent heat-conducting performance than ordinary magnesium hydroxide and also has flame-retardant properties is adopted, and the auxiliary heat conducting agents and flame retardants are used, so that the heat-conducting flame-retardant polyester composite material with excellent performance is prepared, and various application requirements can be met.
Description
Technical field：
A kind of heat conductive flame-retarding polyester composite and preparation method thereof, is related to a kind of side for improving magnesium hydroxide heat conductivility
Method, the magnesium hydroxide prepared by this kind of method can make polyester material while having heat conduction and fire resistance.
Background technology：
Common polyester plastics mainly has PET (PET) and polybutylene terephthalate (PBT),
Because it has excellent mechanical property, heat endurance, electrical insulating property, it is widely used in packing business, electronic apparatus, medical treatment and defends
The field such as life, building, automobile.However, there is inflammable and poor thermal conductivity in itself in polyester plastics, it is difficult to meet high-performance system
The application requirement of product, limit its Contemporary Industrial Design and manufacture in range of application, therefore, research and development have it is fire-retardant and
The polyester composite of the performances such as heat conduction is significant.
Flame retardant polyester is to be blended to plastify compound and prepare by polyester base plastic and fire retardant, and main fire retardant has
Halogen flame retardant system, phosphorus series compound, the metal hydroxides of bromine based compound and antimony oxide composition.Halogen flame is to polyester
With good flame retardant effect, such as Chinese patent 201010612307.9 is hindered using TDE, brominated triazine, phosphorus nitrogen
Two or more in combustion agent, tetrabromobisphenol A are that antimony oxide and/or sodium antimonate are compound with fire retarding synergist, prepare resistance to burning
The PBT of heated filament excellent performance, fire resistance up to UL94 V-0, because in combustion process, bromine antimony based flame retardant can be produced to ring
Border harmful substance, is just limited by more and more policies and regulations.
Phosphorus flame retardant meets environmental requirement, based on phosphate compounds, has the advantages that flame retarding efficiency is high, for example
Chinese patent 201210158866.6 uses tricresyl phosphate, antimony oxide as fire retardant, based on PBT, POM be
It is auxiliary, and with calcium carbonate, silica as filler, be prepared for a kind of enhancing anti-flaming PBT composite, with fire-retardant, high temperature resistant,
It is antistatic, the features such as toughness is high.But there is migration problem in phosphate, this cause the anti-flammability of fire-retardant product and mechanical property with
Time reduces.
Heat conduction polyester composite is to be blended that plasticizing is compound to be obtained by polyester base plastic and conduction powder, insulating properties without
Machine conduction powder mainly includes metal oxide (aluminum oxide, magnesia), nitride (such as boron nitride, aluminium nitride).Such as China
Patent 201510718473.X is prepared for a kind of heat conduction with the mixture of magnesia, aluminum oxide and boron nitride as heat filling
PET alloy material.Metal oxide aluminium, oxidation magnesium hardness are high, big to equipment attrition during extrusion, and easy during filling extrusion high
The problems such as discoloration, limit it and used as main conductive filler powder；Although nitride excellent thermal conductivity, in the polymer
It is difficult to disperse, its addition is difficult to reach the requirement of heat conduction threshold value, and expensive.
Chinese patent CN201610098700.8 by with the heat fillings such as graphene oxide, CNT and aluminium nitride,
Compounding with borate and metal hydroxides is prepared for a kind of heat conduction toughening flame-proof enhancing PBT plastic as fire retardant.But specially
The heat filling aluminium nitride selected in profit is poor with resin compatible, and poor processability is difficult to high heat conduction under low filling；Carbon is received
Although mitron excellent thermal conductivity, can only apply and black products, its range of application is limited from color；Magnesium hydroxide
As a kind of common halogen-free flame retardants, have the advantages that environmentally friendly, cheap, but its flame retarding efficiency is poor, while heat transfer efficiency
It is low.
For the application limitation that heat conductive flame-retarding polyester composite wood prepared by above all kinds of patents is present, this patent provides a kind of
The method for lifting magnesium hydroxide heat conductivility, by magnesium hydroxide heat conductivility obtained in this method than common magnesium hydroxide more
Height, while having fire resistance concurrently, its heat conductive flame-retarding polyester composite excellent performance for preparing can meet various application requirements.
The content of the invention：
The present invention improves its heat conductivility by being heat-treated magnesium hydrate powder, for polyester resin matrix provides a kind of tool
The inorganic heat filling of standby anti-flammability and heat conductivility, so as to prepare a kind of heat conductive flame-retarding polyester composite.
The present invention provides a kind of preparation method of heat conductive flame-retarding polyester composite, it is characterised in that it includes following component
(in terms of mass fraction)：
Polyester resin 100
Heat treatment magnesium hydroxide 100~300
Auxiliary heat conduction agent 0~50
Auxiliary flame retardant 0~30
Dispersant 1~8
Stabilizer 1~3
Mix 5~30 minutes during above-mentioned various raw materials are added into high speed agitator, the compound feeding twin-screw for being obtained
Extruder melt pelletization, the temperature in each area of extruder is：T1=190~200 DEG C, T2=195~205 DEG C, T3=200~210
DEG C, T4=205~215 DEG C, T5=210~220 DEG C, T6=215~225 DEG C, T7=220~230 DEG C, T8=225~235
DEG C, T9=230~240 DEG C, T mould=220~230 DEG C.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that heat treatment magnesium hydroxide leads to
Cross and magnesium hydrate powder is put into Muffle furnace calcining acquisition, its powder meso-position radius is 1~50 μm, preferably 5~30 μm.If in powder
Position footpath is less than 5 μm, then powder is easily reunited, it is difficult to disperseed；If powder meso-position radius are higher than 30 μm, the easy shape in composite system
Into stress concentration point, mechanical properties decrease.
Magnesium hydrate powder is combined with polyester plastics, can assign polyester certain fire-retardant and heat conduction function, its fire retardant mechanism
It is that in combustion, magnesium hydroxide is decomposed and produces magnesia, and is released and combined water, absorbs substantial amounts of latent heat to reduce its institute
Surface temperature of the synthetic material of filling in flame, decomposes with suppression polyester and produced fuel gas is cooled down
Effect, help improves the fire resistance of polyester composite, while the vapor released also can be used as a kind of smoke suppressant.Generally
When magnesium hydrate powder addition about 50% mass fraction, prepared polyester composite can reach the fire-retardant of UL-V0
Rank；The opposing party's aspect, magnesium hydroxide heat conduction is the propagation in the passage of heat that oxygen, magnesium and hydrogen atom are constituted by thermal phonon
Realize, because the atomic weight of hydrogen atom oxygen more therein and magnesium differ greatly, cause the mean free path of its thermal phonon small, thus
Its thermal conductivity is low.
It is heat-treated in advance by magnesium hydrate powder, is carried out partially dehydrated, although reduces its flame retardant effect, but
The hydrogen content of its passage of heat is reduced, the mean free path of thermal phonon can be increased, so as to improve its thermal conductivity.The present invention passes through
The temperature and time of control heat treatment magnesium hydroxide, thus controls the dehydration rate of magnesium hydroxide, so as to realize being heat-treated hydroxide
The regulation of the fire resistance and heat conductivility of magnesium.The present invention is not limited to high temperature furnace, can be conventional Muffle furnace, its temperature
Control at 400~700 DEG C, preferably 500~600 DEG C；1~6h of calcination time, preferably 2~4h.High-temperature calcination is to decompose
Part in magnesium hydroxide combines water, and the decomposition temperature of magnesium hydroxide is 340 DEG C, if temperature is below 400 DEG C, dehydration is carried out very
Slowly, the dehydration rate time for reaching setting is long；If temperature is higher than 700 DEG C, magnesium hydroxide is then dehydrated too soon, is unfavorable for that precise control takes off
Water rate, while being unfavorable for keeping the perfection of lattice of powder, increases thermal resistance.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that polyester base-material is gathered to benzene
Naphthalate (PET) or polybutylene terephthalate (PBT) (PBT), 1~100g/10min of its melt index
(2.16kg, 250 DEG C), preferably 20~60g/10min.If melt index is less than 1g/10min, it is unfavorable for being heat-treated hydroxide
Magnesium powder body is dispersed in base plastic, causes to be difficult to plasticizing extrusion；If melt index is higher than 100g/10min, mechanics
Poor-performing, it is difficult to meet requirement of the application to intensity.
The present invention adds insulating properties high heat conduction powder, such as boron nitride, nitrogen on the basis of magnesium hydroxide conduction powder is heat-treated
Change the compound of aluminium or both, as auxiliary heat conduction agent, further to improve the heat conductivility of prepared polyester composite.
The addition of auxiliary heat conduction powder does not do special limitation, depending on desired value of the prepared material to thermal conductivity.In view of nitrogen
Change boron and aluminium nitride more difficult dispersion in the polyester, its addition is advisable within being maintained at 50phr.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that auxiliary flame retardant is phosphorous
Compound, preferably Melamine Polyphosphate.In view of heat treatment magnesium hydroxide because sloughing part combines water in advance, its resistance
Fuel efficiency fruit can decline, its decline degree regarding dehydration rate depending on, therefore, when be heat-treated magnesium hydroxide addition it is less high or
When person's dehydration rate is higher, the fire resistance of prepared polyester composite may not meet application requirement.Therefore, auxiliary association
The addition for imitating fire retardant it can improve system fire resistance with synergistic.Phosphonium flame retardant has preferably resistance to oxygen-enriched organic compound
Really, wherein Melamine Polyphosphate is wider one kind of range of application in nitrogen phosphorus flame retardant to fuel efficiency, and temperature tolerance is good, decomposes
More than 300 DEG C of temperature, generates source of the gas (melamine) and acid source (phosphoric acid) material after decomposition, have preferably association with magnesium hydroxide
Effect is acted on.In combustion process, the gas and magnesium hydroxide that Melamine Polyphosphate is produced by thermal decomposition receive thermogenetic water
Steam, can dilute the concentration of fuel gas and oxygen；Acid source can be dehydrated into carbon with catalyst, polyester, improve magnesium hydroxide and be heated life
The consistency of magnesia carbon-coating is produced, so as to improve flame retarding efficiency.The addition of auxiliary flame retardant regards prepared composite to resistance
Depending on the requirement of combustion, typically within 30phr.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that dividing using a class is special
Powder, its structure has as follows：
R is the alkane segment that carbon number is 12-18；
M=2 or 4；
N is the integer between 2-30.
Dispersant is used for the surface treatment of inorganic filler, can improve the compatibility of resin and inorganic filler, makes composite
With good mechanical property, and improve processing characteristics.Polyester group in this kind of dispersant has preferable with matrix resin
Compatibility, can play a part of interior lubrication, while avoiding the migration of dispersant；And it is the alkane chain of 12-18 that R is carbon number
Section, plays a part of to powder dispersion and outer lubrication in system.This dispersant is added in system, inorganic filler can be improved and existed
Scattered dispersiveness in polyester, improves the compatibility of powder and resin, and realizes process simultaneously, inside and outside lubricity
Balance, so as to the processing characteristics of system can be improved.The consumption of this dispersant is 3~8phr, and powder addition is higher or powder
Particle diameter is smaller, and its consumption is bigger.
The stabilizer that the present invention is used includes a kind of in antioxidant, hydrolysis-resisting agent, heat stabilizer or theirs is compound.
Because, containing fatty segment and ester group, under melt-processed or higher temperature, oxygen easily makes in polyester resin main chain
There is thermal oxide in it, so as to cause product jaundice, burnt hair, moisture can cause hydrolysis of ester group, so that polyester physical and mechanical properties
Decline and even destroy.Therefore, in polyester composite process, it is usually added into antioxidant, hydrolysis-resisting agent, heat stabilizer
A kind of or they compound, prevent polyester from decomposing or degrading under heat, oxygen, water function.Common antioxidant is divided into be received
Resistance phenols and phosphorous acid lipid, such as antioxidant 1010,168,1076,1098.Heat stabilizer has Ciba companies
IrganoxHP136, Irganox1425, IrganoxB2215 etc..Hydrolysis-resisting agent has Carbodiimides, such as bright Sheng
Stabaxol-1, Stabaxol-P, Stabaxol-P100, Stabaxol-P200 etc., can use, and patent does not do special limit
System, its addition is 1-3 parts.
The present invention is equipped with the powder dispersant of special polyester-type to be heat-treated based on magnesium hydroxide, there is provided a kind of
The approach of the polyester composite with fire-retardant and heat conduction function is prepared, its technical characterstic is：(1) heat treatment magnesium hydroxide is relative
In common magnesium hydroxide, with thermal conductivity higher, therefore prepared polyester composite, better heat transfer is shown
Performance；(2) different from the heat conduction and flame retardant polyester implemented respectively at present, heat treatment magnesium hydroxide is realizing the same of heat conduction function
When, anti-flaming function can be realized, particularly under heat conduction requirement powder higher filling situation high, prepared polyester composite
Still maintain good fire resistance；(3) dispersant comprising polyester oligomer and long chain alkane for using, assigns powder with tree
The more preferable compatibility of fat, and dispersing uniformity of the powder in resin, so that the processing characteristics of composite polyester material is good
Good, the intensity of prepared composite is high.
Specific implementation formula：
The present invention is further described in detail with reference to specific embodiment, the embodiment for being given is only for explaining
The bright present invention, rather than in order to limit the scope of the present invention.
Raw material sources employed in embodiment and comparative example are described as follows：
Polyester resin (PBT：Trade mark B4040G6) purchased from German BASF；Magnesium hydroxide comes from the water Jin Gexin of Foshan City three
Type Materials Co., Ltd；Polyester-type dispersant JZF-1, JZF-2, JZF-3, purchased from Guangzhou Ya Xin Chemical Co., Ltd.s；Antioxidant
1010th, 168 etc. it is purchased from Dongguan City Bao Sheng plastic cement Co., Ltd；IrganoxHP136 is purchased from Ciba；Stabaxol-1 is purchased from
It is bright to contain Co., Ltd in chemistry.
Method of testing employed in embodiment and comparative example is described as follows：
Thermal conductivity：Shone the thermal conductivity of the prepared sample of method conductometer LFA-447 tests using the resistance to laser of speeding of Germany, sample
Size is 1cm*1cm, and thickness is 2mm.
Fire resistance：Fire resistance is tested using vertical combustion analyzer CZF-2 (analytical instrument factory of Jiangsu Jiangning county).
Mechanical property：Tensile strength is tested using HD-B640DB-S computer servo twin columns puller system.
Embodiment 1
It is heat-treated the preparation of magnesium hydroxide：1000g magnesium hydrate powders (10 μm of meso-position radius) are put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 550 DEG C, keeps this temperature 4h, obtains heat
Treatment powder 648.3g, dehydration rate is 35.2%.
The preparation of flame-retarded heat-conducting polyester composite：By formula as below, mixed during various raw materials are added into 5L high speed agitators
Close 3 minutes, the compound for being obtained adds the plasticizing granulation of the double screw extruders of φ 35, the temperature setting in each area of extruder is：T1
=190 DEG C, T2=205 DEG C, T3=210 DEG C, T4=210 DEG C, T5=220 DEG C, T6=225 DEG C, T7=225 DEG C, T8=235
DEG C, T9=235 DEG C, T mould=220 DEG C.The pellet for being obtained is placed 4 hours in 100 DEG C of blast drier, by injection machine
Prepare test sample.The data tested are shown in Table one.
Comparative example 1
Magnesium hydroxide is heat-treated in the polyester composite formula of embodiment 1 and replaces with magnesium hydroxide, other are formulated and technique
It is constant.The data tested are shown in Table one.
Comparative example 2
Dispersant JZF-1 replaces calcium stearate in the polyester composite of embodiment 1 formula, and other formulas and technique are constant.
The data tested are shown in Table one.
Embodiment 2
It is heat-treated the preparation of magnesium hydroxide：1000g magnesium hydrate powders (10 μm of meso-position radius) are put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 500 DEG C, keeps this temperature 4h, obtains heat
Treatment powder 762.5g, dehydration rate is 23.8%.
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 3
It is heat-treated the preparation of magnesium hydroxide：1000g magnesium hydrate powders (10 μm of meso-position radius) are put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 450 DEG C, keeps this temperature 4h, obtains heat
Treatment powder 864.0g, dehydration rate is 13.6%.
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 4
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 5
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 6
It is heat-treated the preparation of magnesium hydroxide：1000g magnesium hydrate powders (5 μm of meso-position radius) are put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 500 DEG C, keeps this temperature 5h, obtains heat
Treatment powder 648.0g, dehydration rate is 28.5%.
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 7
It is heat-treated the preparation of magnesium hydroxide：1000g magnesium hydrate powders (30 μm of meso-position radius) are put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 600 DEG C, keeps this temperature 3.6h, is obtained
Heat treatment powder 648.4g, dehydration rate is 28.6%.
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 8
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 9
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 10
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Embodiment 11
Polyester composite is prepared by formula as below, and its technique is with embodiment 1.The data tested are shown in Table one.
Be can see from the test data of table one：(1) the test data discovery of comparing embodiment 1-3, comparative example 1, made
Standby polyester composite, under identical filling number, magnesium hydroxide dehydration rate is higher, and the fire resistance of composite is poorer,
Thermal conductivity is higher；(2) contrast of embodiment 1 and the database of comparative example 2 shows, using polyester-type dispersant than conventional stearic acid
Polyester composite tensile strength prepared by salt is higher, shows that this dispersant not only has the good dispersion to powder, and
With the excellent compatibility with resin；(3) number of comparing embodiment 1 and embodiment 4,5 is it has been found that in dehydration rate identical situation
Under, the filling number of magnesium hydroxide is higher, then the heat conductivility of polyester composite is higher, and anti-flammability is better；(4) implementation is compared
The number of example 1 and embodiment 6,7 is it has been found that with the reduction of heat treatment magnesium hydrate powder particle diameter, prepared polyester composite wood
The tensile strength increase of material, anti-flammability is unchanged, and heat conductivility decreases；(5) data pair of embodiment 8 and embodiment 3
Than showing, the addition of Melamine Polyphosphate is remarkably improved the fire resistance of polyester composite, shows that it has good
Good flame retardant synergism；(6) number of comparing embodiment 9,10 and embodiment 3 is it has been found that equally under filling number, add nitridation
Boron or boron nitride and aluminium nitride it is compound, be remarkably improved the heat conductivility of prepared polyester composite；Further herein
On the basis of compound Melamine Polyphosphate, its fire resistance is obviously improved.
Table one, polyester composite is fire-retardant with heat conductivility data
Claims (8)
1. a kind of heat conductive flame-retarding polyester composite and preparation method thereof, it is characterised in that polyester composite is by following weight
The component of part is made：
Polyester resin 100
Heat treatment magnesium hydroxide 100~300
Auxiliary heat conduction agent 0~50
Auxiliary flame retardant 0~30
Dispersant 1~8
Stabilizer 1~3
After 5~30min is mixed in the material addition high-speed mixer in above-mentioned formula, melting is squeezed in feeding double screw extruder
Go out, the billot extruded is cooled down through tank, is pulled into pelleter granulation, obtains final product heat conductive flame-retarding polyester composite.Wherein, it is double
The temperature in each area of screw extruder is：T1=190~200 DEG C, T2=195~205 DEG C, T3=200~210 DEG C, T4=205~
215 DEG C, T5=210~220 DEG C, T6=215~225 DEG C, T7=220~230 DEG C, T8=225~235 DEG C, T9=230~
240 DEG C, T mould=220~230 DEG C.
2. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that heat treatment hydrogen
Magnesia enters high temperature furnace calcining acquisition by the way that magnesium hydroxide is put into powder, and its powder meso-position radius is 1~50 μm, preferably 5~30 μm.
3. according to claim 1 and 2, it is characterized in that high temperature furnace temperature control is at 400~700 DEG C, preferably 500~600 DEG C；
1~6h of calcination time, preferably 2~4h.
4. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that polyester base-material
It is polyethylene terephthalate (PET) or polybutylene terephthalate (PBT) (PBT), 1~100g/ of its melt index
10min, preferably 20~60g/10min.
5. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that auxiliary heat conduction
Agent is insulating properties high heat conduction powder, and preferably boron nitride, aluminium nitride, or both is compound.
6. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that assisting flame-resistant
Agent is phosphorus-containing compound, preferably Melamine Polyphosphate.
7. kind of heat conductive flame-retarding polyester composite a kind of according to claim 1 and preparation method thereof, it is characterized in that dispersant
With following structure：
R is the alkane segment that carbon number is 12-18；
M=2 or 4；
N is the integer between 2-30.
8. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that stabilizer is
A kind of in antioxidant, hydrolysis-resisting agent, heat stabilizer or theirs is compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611175094.1A CN106700440B (en) | 2016-12-16 | 2016-12-16 | A kind of heat conductive flame-retarding polyester composite and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611175094.1A CN106700440B (en) | 2016-12-16 | 2016-12-16 | A kind of heat conductive flame-retarding polyester composite and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106700440A true CN106700440A (en) | 2017-05-24 |
| CN106700440B CN106700440B (en) | 2019-02-19 |
Family
ID=58938052
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611175094.1A Active CN106700440B (en) | 2016-12-16 | 2016-12-16 | A kind of heat conductive flame-retarding polyester composite and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106700440B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108676212A (en) * | 2018-05-18 | 2018-10-19 | 深圳市金菱通达电子有限公司 | The non-silicon heat-conducting pad that suitable optical module uses |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899209A (en) * | 2010-03-30 | 2010-12-01 | 金发科技股份有限公司 | Heat conductive insulation material and preparation method thereof |
| CN102558609A (en) * | 2011-12-13 | 2012-07-11 | 金发科技股份有限公司 | Method for improving thermal conductivity of thermal conductive polymer |
| CN104559147A (en) * | 2014-12-16 | 2015-04-29 | 惠州力王佐信科技有限公司 | Anti-dripping smoke-suppression-type environment-friendly heat-conducting material and preparation method thereof |
| CN104861595A (en) * | 2015-06-08 | 2015-08-26 | 江苏理工学院 | Halogen-free flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof |
-
2016
- 2016-12-16 CN CN201611175094.1A patent/CN106700440B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899209A (en) * | 2010-03-30 | 2010-12-01 | 金发科技股份有限公司 | Heat conductive insulation material and preparation method thereof |
| CN102558609A (en) * | 2011-12-13 | 2012-07-11 | 金发科技股份有限公司 | Method for improving thermal conductivity of thermal conductive polymer |
| CN104559147A (en) * | 2014-12-16 | 2015-04-29 | 惠州力王佐信科技有限公司 | Anti-dripping smoke-suppression-type environment-friendly heat-conducting material and preparation method thereof |
| CN104861595A (en) * | 2015-06-08 | 2015-08-26 | 江苏理工学院 | Halogen-free flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘庆丰等: "烷基化聚酯超分散剂改性水滑石的合成及其在PVC中的应用", 《聚氯乙烯》 * |
| 翟学良: "氢氧化镁热分解行为与机理研究", 《矿产综合利用》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108676212A (en) * | 2018-05-18 | 2018-10-19 | 深圳市金菱通达电子有限公司 | The non-silicon heat-conducting pad that suitable optical module uses |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106700440B (en) | 2019-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101717560B (en) | Halogen-free antiflaming polyester molding composition and preparation method thereof | |
| WO2020233028A1 (en) | Flame-retardant and smoke-suppressing soft polyvinyl chloride composite material having good mechanical performance and preparation method therefor | |
| Gallo et al. | Halogen-free flame retarded poly (butylene terephthalate)(PBT) using metal oxides/PBT nanocomposites in combination with aluminium phosphinate | |
| CN108102213B (en) | Flame-retardant polypropylene composition and preparation method and application thereof | |
| CN101280097A (en) | Nanometer flame-proof polyethylene glycol terephthalate engineering plastics and preparation thereof | |
| CN107312298A (en) | A kind of flame retardant type polycarbonate composite material and preparation method thereof | |
| CN112778741B (en) | Flame-retardant polycarbonate composition and preparation method thereof | |
| Thi et al. | Synergistic effects of aluminum hydroxide, red phosphorus, and expandable graphite on the flame retardancy and thermal stability of polyethylene | |
| CN106009585A (en) | Halogen-free flame retardation polycarbonate material and preparation method thereof | |
| KR102501772B1 (en) | Flame-retardant master batch and method for manufacturing the same | |
| CN106496863B (en) | A kind of mildew-proof flame retarded polyvinyl chloride sheath material of novel environment friendly | |
| CN109082093A (en) | Abrasion-resistant clear flame-retardant polycarbonate material and preparation method thereof | |
| DE69709504T2 (en) | Flame retardant polyester composition | |
| CN115322488A (en) | Flame-retardant polypropylene composite material and preparation method and application thereof | |
| CN103740038A (en) | High-glossiness halogen-free flame-retardant ABS material and preparation method thereof | |
| CN108117692A (en) | A kind of composite high-molecular plastic building template and preparation method thereof | |
| CN105111729B (en) | Environmental protection flame retardant carbon fiber reinforced polyamide composite material and its preparation method and application | |
| CN105001561B (en) | Flame retardant polyvinyl chloride composition and preparation method thereof | |
| CN106700440B (en) | A kind of heat conductive flame-retarding polyester composite and preparation method thereof | |
| CN109777049A (en) | Polybutylene terephthalate (PBT) resin combination | |
| CN103694549A (en) | Low-temperature-resistant oil-resistant halogen-free flame-retardant crosslinking cable sheath material and preparation method thereof | |
| CN106633388B (en) | A kind of red phosphorus flame-retardant reinforced polypropylene material and preparation method thereof | |
| CN111690197A (en) | Melamine-containing direct intercalation g-C3N4Flame-retardant cable material and preparation method thereof | |
| CN108570205A (en) | A kind of Flameproof styrenic composition and preparation method thereof | |
| CN110272618A (en) | A kind of high fluidity environmental-friendly fire-retardant PC material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: No.12, Yinzhou Road, Baini Town, Sanshui District, Foshan City, Guangdong Province Patentee after: Foshan Jinge New Material Co.,Ltd. Address before: No.81182, Baishui industrial district, Foshan City, Guangdong Province Patentee before: FOSHAN SANSHUI JINGE NEW MATERIALS Co.,Ltd. |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: No. 12, Yinzhou Road, Zhou Village, Baini Town, Sanshui District, Foshan, Guangdong 528131 Patentee after: Guangdong Jinge New Materials Co.,Ltd. Address before: No.12, Yinzhou Road, Baini Town, Sanshui District, Foshan City, Guangdong Province Patentee before: Foshan Jinge New Material Co.,Ltd. |
|
| CP03 | Change of name, title or address |