CN110172236A - A kind of surface modified carbon microballoon/unsaturated polyester (UP) composite flame-proof material preparation method and applications - Google Patents
A kind of surface modified carbon microballoon/unsaturated polyester (UP) composite flame-proof material preparation method and applications Download PDFInfo
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- CN110172236A CN110172236A CN201910010811.2A CN201910010811A CN110172236A CN 110172236 A CN110172236 A CN 110172236A CN 201910010811 A CN201910010811 A CN 201910010811A CN 110172236 A CN110172236 A CN 110172236A
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- 229920006305 unsaturated polyester Polymers 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 150000001721 carbon Chemical class 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims description 11
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 239000003607 modifier Substances 0.000 claims abstract description 9
- 229920006337 unsaturated polyester resin Polymers 0.000 claims abstract description 8
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 6
- 239000010452 phosphate Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000008901 benefit Effects 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 26
- 239000003063 flame retardant Substances 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 7
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229920001661 Chitosan Polymers 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 229920002101 Chitin Polymers 0.000 claims description 2
- 239000004809 Teflon Substances 0.000 claims description 2
- 229920006362 Teflon® Polymers 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001746 injection moulding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000004580 weight loss Effects 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- 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
- C08K9/02—Ingredients treated with inorganic substances
-
- 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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
Landscapes
- 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)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention discloses a kind of modified hydridization carbosphere/unsaturated polyester (UP) composite flame-proof materials in surface.The composite flame-proof material is mainly composed of the following raw materials by weight: 97~100 parts of unsaturated polyester (UP), 1~3 part of carbosphere, 2~6 parts of surface modifier, 1~2 part of phosphate, 2~6 parts of urea, 2 parts of initiator.Appropriate surface modified carbon microballoon, initiator and unsaturated polyester resin are sufficiently mixed rear curing molding to get product.The present invention has the advantages that surface modifying method raw material sources used in (1) are extensive, environmentally protective, cost is relatively low, and process simple process, it is suitble to industrialized production；(2) composite flame-proof material provided solves the problems, such as that compatibility is poor between carbosphere and unsaturated polyester (UP) to a certain extent；(3) composite flame-proof material provided, which is compared pure unsaturated polyester (UP) and compared, has higher thermal stability and oxygen index (OI).
Description
Technical field
The invention belongs to carbon material hydridization flame-retardant high-molecular technical fields, and in particular to and a kind of surface modified carbon microballoon/no
Saturated polyester composite flame-proof material and preparation method thereof.
Background technique
Unsaturated polyester (UP) is extensive due to its excellent mechanical performance, workability, high chemical resistance and corrosion resistance
As automobile, aviation, electronics, building and packaging industry.But unsaturated polyester (UP) itself is inflammable, and generates in combustion a large amount of
Smog and toxic gas, seriously threaten environmental and human health impacts, hinder it and development is widely applied.Therefore, increasingly increased quotient
Industry demand promotes people to develop effective and environmentally friendly fire retardant to enhance the fire protecting performance of unsaturated polyester (UP).
As a kind of emerging carbon material, the outstanding chemical stability of carbosphere and thermal stability make it from numerous novel
Fire proofing in show one's talent.But biggish specific surface area and higher surface energy, lead to carbosphere and unsaturated polyester (UP)
Between compatibility it is poor, seriously compromise the durability of unsaturated polyester (UP) composite flame-proof material.To overcome disadvantage mentioned above, the present invention
Surface modification treatment is carried out to carbosphere, enhances its compatibility between unsaturated polyester (UP), and then it is multiple to improve unsaturated polyester (UP)
Flame retardant property, thermal stability and the durability of condensation material.
Patent CN108752892A and patent CN108752893A discloses a kind of new flame retardant type unsaturated polyester (UP), but
Synthetic route is more complex and cost is excessively high.Patent CN108192307A discloses a kind of system of high-fire resistance unsaturated polyester resin
Preparation Method, but the fire retardant type added is excessive.Surface modified carbon microballoon provided by the invention/unsaturated polyester (UP) composite flame-proof material
Expect that synthetic route is simpler, and fire retardant additive amount and type are less.
Summary of the invention
In order to solve deficiency in the prior art, the object of the present invention is to provide a kind of surface modified carbon microballoon/unsaturations
Polyester composite flame retardant material and preparation method thereof.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of modified hydridization carbosphere/unsaturated polyester (UP) composite flame-proof material in surface, the high flame retardant unsaturated polyester (UP)
Resin is mainly composed of the following raw materials by weight: 97~100 parts of unsaturated polyester (UP), 1~3 part of carbosphere, and surface modifier 2~6
Part, 1~2 part of phosphate, 2~6 parts of urea, 2 parts of initiator.
The surface modifier is that chitin, chitosan and cellulose are any one or more of.
The phosphate is that triethyl phosphate, phosphoric acid and phosphorus pentoxide are any one or more of.
The initiator is benzoyl peroxide.
A kind of above-mentioned surface is modified the preparation method of hydridization carbosphere/unsaturated polyester (UP) composite flame-proof material, mainly includes
Following steps:
(1) carbosphere is weighed to stir 60~240 minutes under 40-60 DEG C of water bath condition in sodium hydroxide solution, spend from
Sub- water washing is dried to obtain particle A；
(2) surface modifier is dissolved in acetic acid solution, obtains solution B；
(3) it disperses particle A in deionized water, is added in solution B, stir 100~500 minutes, obtain solution C；
(4) supernatant is removed after standing solution C, is successively washed using acetic acid solution and deionized water, is dried to obtain
Grain D；
(5) it disperses particle D and urea in dimethylformamide, is heated to 110-120 DEG C, is added under agitation
Phosphate stirs 100~500 minutes, and benefit is washed with deionized, and obtains surface modified carbon microballoon after dry；
(6) surface modified carbon microballoon, initiator benzoyl peroxide are added in unsaturated polyester resin, stirring 20~
60 minutes, solution E was obtained after mixing；
(7) solution E is poured into Teflon mould, drying box is put into after injection molding, obtains a kind of table after solidification demoulding
Face is modified hydridization carbosphere/unsaturated polyester (UP) composite flame-proof material.
The step (1), (3), (5), (6) described stirring revolving speed be 100~700 revs/min.
In the step (6) additive amount of the modified hydridization carbosphere in surface be unsaturated polyester resin weight 1%~
3%；The additive amount of initiator is the 2% of unsaturated polyester resin weight.
Condition of cure described in the step (7) are as follows: constant temperature 60 minutes under the conditions of 80 DEG C, constant temperature 180 divides under the conditions of 110 DEG C
Clock.
Compared with prior art, the present invention has the advantage that:
(1) surface modifying method raw material sources provided by the invention are extensive, environmentally protective, cost is relatively low, and process
Simple process is suitble to industrialized production.
(2) surface modified carbon microballoon/unsaturated polyester composite provided by the invention compares unmodified carbosphere/insatiable hunger
And polyester composite, solve the problems, such as that compatibility is poor between carbosphere and unsaturated polyester (UP) to a certain extent.
(3) surface modified carbon microballoon/unsaturated polyester (UP) flame retardant composite material provided by the invention, it is micro- to compare unmodified carbon
Ball/unsaturated polyester composite and pure unsaturated polyester (UP), surface modifier and phosphatic introducing have been postponed and have reached maximum heat
The time of weight loss rate, composite material have higher thermal stability.
Detailed description of the invention
Fig. 1 is the FTIR spectrum figure of carbosphere used in embodiment 2 and 3.
Fig. 2 is the FTIR spectrum figure of surface modified carbon microballoon prepared by embodiment 3.
Fig. 3 is the thermogravimetric (left side) after the unsaturated polyester composite that embodiment 1,2 and 6 provides solidifies in nitrogen atmosphere
With thermal weight loss rate (right side) curve.
Specific embodiment
The present invention is done below with reference to specific embodiment and more comprehensively, is meticulously described, but protection scope of the present invention
It is not limited to embodiment in detail below.
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Except there is a special instruction, the various reagents used in the present invention, raw material be can commodity commercially or
Person can the product as made from well known method.
With reference to the accompanying drawings and examples, the technical solution used to invention is further elaborated.
Embodiment 1
The preparation of pure unsaturated polyester (UP), specifically comprises the following steps:
2 parts of benzoyl peroxides are added in 100 parts of unsaturated polyester (UP)s, stirred 30~60 points with revolving speed 500r/ minutes
Mold is poured into after clock, 80 DEG C constant temperature 1 hour, 110 DEG C of constant temperature 3h, cooling and demolding after taking-up.
Referring to table 1, it can be seen that the oxygen index (OI) of embodiment 1 is only 19.8%.
Referring to attached drawing 3, it is thermogravimetric (left side) and thermal weight loss rate (right side) curve of the embodiment 1 in nitrogen atmosphere.It can be with
The temperature (T0.1) for finding out 2 weightlessness 10% of embodiment is 334 DEG C, and Residual carbon is 10.9wt%, thermal weight loss after 750 DEG C
Temperature (the T of rate peak valuemax) be 415 DEG C, maximum weight loss rate be 1.44%/DEG C, thermal stability is poor.
Embodiment 2
3 parts of carbospheres and 2 parts of benzoyl peroxides are added separately in 97 parts of unsaturated polyester (UP), with 500 turns of revolving speed/
Minute stirring 20~pour into mold after sixty minutes, 80 DEG C constant temperature 1 hour, 110 DEG C of constant temperature 3h, cooling and demolding after taking-up.
Referring to table 1, it can be seen that the oxygen index (OI) of embodiment 2 is 21.4%, and 19.8% than embodiment 1 is high by 1.6%.
Referring to attached drawing 3, it is the thermogravimetric (left side) in a nitrogen atmosphere of embodiment 2 and thermal weight loss rate (right side) curve.It can be with
Find out, the temperature (T of 2 weightlessness 10% of embodiment0.1) it is 353 DEG C, than 1 high 19 DEG C of embodiment.Carbon residue of the embodiment 2 at 750 DEG C
Rate is 19.7wt%, also 3.9wt% higher than the Residual carbon of embodiment 3 much larger than the 10.9wt% of embodiment 1.Thermal weight loss rate
Temperature (the T of peak valuemax) promoted from 415 DEG C of embodiment 1 to 417 DEG C, and maximum weight loss rate from 1.44%/DEG C be reduced to
1.32%/DEG C.
Embodiment 3
3 parts of carbospheres are stirred 180 minutes under 45 DEG C of water bath conditions with 300 revs/min of revolving speed in sodium hydroxide solution,
Particle A is dried to obtain after being washed with deionized；
6 parts of chitosans are dissolved in acetic acid solution, solution B is obtained；
It disperses 1 part of particle A in deionized water, is added in solution B, stirred 240 minutes with 300 revs/min of revolving speed,
Obtain solution C；
Supernatant is removed after solution C is stood, is successively washed using acetic acid solution and deionized water, and particle D is dried to obtain；
It disperses 3 parts of particle D and 6 parts of urea in dimethylformamide, is heated to 110 DEG C, 3 are added under agitation
Part phosphoric acid, is stirred 180 minutes with 300 revs/min of revolving speed, and benefit is washed with deionized, and obtains surface modified carbon microballoon after dry；
3 parts of surface modified carbon microballoons and 2 parts of benzoyl peroxides are added separately in 97 parts of unsaturated polyester (UP), to turn
Fast 500r/ minutes stirring 20~pour into mold after sixty minutes, 80 DEG C constant temperature 1 hour, 110 DEG C of constant temperature 3h, it is cooling de- after taking-up
Mould.
Referring to attached drawing 1, it is the FTIR spectrum figure of carbosphere.As seen from Figure 1, it is located at 1034cm-1With
3430cm-1The 2 strong peak at place respectively corresponds bending and the stretching vibration peak of-OH, 1634cm-1Occur that-C=O's is flexible
Vibration peak illustrates that carbosphere surface has oxygen-containing functional group, provides possibility for surface modification.
Referring to attached drawing 2, it is the FTIR spectrum figure of surface modified carbon microballoon and surface modifier chitosan.By scheming
2 as can be seen that be located at 1400cm-1For the crystallization sensitivity peak of chitosan, 1602cm-1And 3156cm-1Be-NH bending vibration and
Stretching vibration absworption peak, 3415cm-1The stretching vibration absworption peak that neighbouring strong absworption peak is-OH.And for surface modified carbon microballoon
For, it is located at 3156cm-1And 1602cm-1- NH stretching vibration and bending vibration absorption peak disappear, and in 544cm-1,
1150cm-1And 1632cm-1Place has found new characteristic peak, respectively corresponds the spy of the stretching vibration and-NHCO- with P-O and P=O
Levy peak.
Referring to table 1, it can be seen that the oxygen index (OI) of embodiment 3 is 21.5%, and 19.8% than embodiment 1 is high by 1.7%, and real
It is close to apply example 2, is higher by 0.1%.
Referring to attached drawing 3, it is the thermogravimetric (left side) in a nitrogen atmosphere of embodiment 3 and thermal weight loss rate (right side) curve.By Fig. 3
As can be seen that temperature (the T of 3 weightlessness 10% of embodiment0.1) it is 351 DEG C, than 1 high 17 DEG C of embodiment, 2 low 2 DEG C of embodiment.Implement
Residual carbon of the example 3 at 750 DEG C is 15.8wt%, greater than the 10.9wt% of embodiment 1, but it is 3.9wt% smaller than embodiment 2, this
It is because surface modifier and phosphatic introducing can promote surface modified carbon microballoon/unsaturated polyester (UP) flame retardant composite material heat
It decomposes, leaves less carbon residue, but the carbon-coating formed is finer and close, this is the T of embodiment 30.1It is lower than embodiment 2, but reach
Temperature (the T of thermal weight loss rate peak valuemax) higher, maximum heat weight loss rate bigger reason.
A kind of surface modified carbon microballoon/unsaturated polyester (UP) flame retardant composite material, the limit as obtained by above-described embodiment
Oxygen index (OI) and vertical combustion grade are as shown in table 1:
1 embodiment 1,2 of table and 3 limit oxygen index and vertical combustion grade
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Oxygen index (OI) (%) | 19.8 | 21.4 | 21.5 |
A kind of surface modified carbon microballoon/unsaturated polyester (UP) flame retardant composite material as obtained by above-described embodiment, in nitrogen
Thermogravimetric Data under gas atmosphere is as shown in table 2:
Thermogravimetric Data under 2 embodiment of table, 1,2,3 nitrogen atmosphere
Claims (8)
1. a kind of modified hydridization carbosphere/unsaturated polyester (UP) composite flame-proof material in surface, which is characterized in that the unsaturated polyester (UP)
Flame retardant composite material is mainly composed of the following raw materials by weight: 97~100 parts of unsaturated polyester (UP), 1~3 part of carbosphere, surface changes
2~6 parts of agent, 1~2 part of phosphate, 2~6 parts of urea, 2 parts of initiator of property.
2. the modified hydridization carbosphere/unsaturated polyester (UP) flame retardant composite material in surface according to claim 1, feature exist
In the surface modifier is that chitin, chitosan and cellulose are any one or more of.
3. the modified hydridization carbosphere/unsaturated polyester (UP) flame retardant composite material in surface according to claim 1, feature exist
In the phosphate is that triethyl phosphate, phosphoric acid and phosphorus pentoxide are any one or more of.
4. the modified hydridization carbosphere/unsaturated polyester (UP) flame retardant composite material in surface according to claim 1, feature exist
In the initiator is benzoyl peroxide.
5. a kind of preparation method of the modified hydridization carbosphere/unsaturated polyester (UP) flame retardant composite material in surface described in claim 1,
It is characterized in that, mainly comprising the steps that
(1) it weighs carbosphere to stir 60~240 minutes under 40-60 DEG C of water bath condition in sodium hydroxide solution, uses deionized water
Washing is dried to obtain particle A；
(2) surface modifier is dissolved in acetic acid solution, obtains solution B；
(3) it disperses particle A in deionized water, is added in solution B, stir 100~500 minutes, obtain solution C；
(4) supernatant is removed after standing solution C, is successively washed using acetic acid solution and deionized water, and particle D is dried to obtain；
(5) it disperses particle D and urea in dimethylformamide, is heated to 110-120 DEG C, phosphoric acid is added under agitation
Salt stirs 100~500 minutes, and benefit is washed with deionized, and obtains surface modified carbon microballoon after dry；
(6) surface modified carbon microballoon, initiator benzoyl peroxide are added in unsaturated polyester resin, stir 20~60 points
Clock obtains solution E after mixing；
(7) solution E is poured into Teflon mould, is put into drying box after injection molding, a kind of surface is obtained after solidification demoulding and is changed
Property hydridization carbosphere/unsaturated polyester (UP) composite flame-proof material.
6. the preparation method of the modified hydridization carbosphere/unsaturated polyester (UP) flame retardant composite material in surface according to claim 5,
It is characterized in that, (1), (3), (5), (6) described stirring revolving speed be 100~700 revs/min.
7. the preparation method of the modified hydridization carbosphere/unsaturated polyester (UP) flame retardant composite material in surface according to claim 5,
It is characterized in that, the additive amount of the modified hydridization carbosphere in surface is the 1%~3% of unsaturated polyester resin weight in step (6)；
The additive amount of initiator is the 2% of unsaturated polyester resin weight.
8. the preparation method of high flame retardant unsaturated polyester composite according to claim 5, which is characterized in that step
(7) condition of cure described in are as follows: constant temperature 60 minutes under the conditions of 80 DEG C, constant temperature 180 minutes under the conditions of 110 DEG C.
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| CN111117180A (en) * | 2020-01-10 | 2020-05-08 | 南京工业大学 | Preparation method and application of flame-retardant unsaturated polyester resin composite material containing nano hybrid of nitrogen and carbon |
-
2019
- 2019-01-04 CN CN201910010811.2A patent/CN110172236A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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