CN106995565A - A kind of preparation method of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic - Google Patents
A kind of preparation method of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- 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
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- C08K2003/2241—Titanium dioxide
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- C08K2003/265—Calcium, strontium or barium carbonate
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a kind of preparation method of the fire-retardant sol-gel modified poly styrene composite material of phosphotidic, the composite stability of invention is good, combination property is superior, adulterated citric acid by monomer, also there is more preferable heat-insulating property, the present invention is used as inorganic filler using calcium carbonate, change the high hard material such as conventionally employed graphene, silica, effectively reduce the proportion of finished product, the effect of lightweight is realized, is readily transported, processes, installs, reduce cost, the material environment friendly of the present invention is good, and fire-retardant fireproof is strong, biocidal property is good.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of system of the fire-retardant sol-gel modified poly styrene composite material of phosphotidic
Preparation Method.
Background technology
At present, with advances in technology, ubiquitous new product, new things give people life, the work side of bringing
Just quick to starve service, the life of people there occurs earth-shaking change.In order to ensure national public property and citizen's person peace
Entirely, in order to eliminate disaster hidden-trouble, while having enjoyed life comfortable, fast, " high-quality and safe life " will be increasingly becoming life
In indispensable key factor.Under historical background so at a tremendous pace, fire retardant plastic material also just doting on into market
Youngster.The material with superior characteristics such as good anti-flammability, low-density, low cost, good combination properties because being applied to wall
The fields such as wall switch, socket, tubing, breaker of plastic casing, motor component, sheet material.In recent years, also there are many manufacturing enterprises both at home and abroad
Begin one's study and develop flame retardant plastics, but the fire retardant added at present is more with halogenated flame retardant, it is outstanding during long-term use
It is to produce the noxious material of hydrogen halides in combustion process, and the health and environment to people can all cause great harm；
Building energy-saving heat-insulating material is the core key technology of building energy conservation, directly determines construction quality, energy-saving effect and construction
It is insulation material using expanded polystyrene (EPS) as representative that progress is widely used at present, and it is so that light weight, thermal insulation be good, raw material
Be easy to get, easy construction, the significant advantage such as with low cost, the occupancy volume in building energy-saving heat-insulating material market is up to more than 85%, so
And expanded polystyrene (EPS) belongs to macromolecule construction material, the significant drawback with easy firing, security difference in recent years, is thus drawn
The building fire of hair, causes the casualties and property loss of heaviness, and exploitation highly effective flame-retardant expanded polystyrene (EPS) material has turned into
The hot issue in building energy-saving heat-insulating material field；
And in order to improve the fire resistance of polystyrene material, often add wherein graphene, the high intensity such as silica without
Machine filler, but the compatibility of inorganic filler and polystyrene is poor, solution causes to reunite, and reduces the stability_intensity of finished product,
The proportion height of finished product is easily caused using the inorganic filler of high intensity simultaneously, transport, the difficulty installed are added, while in order to carry
The service life of high material, can be applied to various poor environments, improve its antibacterial antiseptic property be also it is very necessary,
Therefore the present invention have studied the preferable lightweight polyphenyl ethene composite of a kind of feature of environmental protection, anti-flammability, biocidal property.
The content of the invention
It is an object of the invention to proportion height, poor fire, the ring existed for polystyrene material of the prior art
There is provided a kind of preparation method of the fire-retardant sol-gel modified poly styrene composite material of phosphotidic for the problems such as guarantor property is poor, biocidal property is poor.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic, comprises the following steps：
（1）The Tri-isopropylphenyl phosphate of 1-2 parts by weight is taken, in the absolute ethyl alcohol for being added to 10-13 times of its weight, stirring is equal
It is even；
（2）The titanyl sulfate of 16-20 parts by weight is taken, in the deionized water for being added to 30-40 times of its weight, is stirred, is added dropwise
Concentration is 10-11% ammoniacal liquor, and regulation pH is 10-12, and stirring reaction 1-2 hours, the carboxymethyl for adding 0.1-0.2 parts by weight is fine
The plain sodium of dimension, stirs, obtains titanium sol dispersion；
（3）Calcium oxide, the sodium carbonate mixing of 20-27 parts by weight of 20-24 parts by weight are taken, 40-50 times of compound weight is added to
Deionized water in, stir 2-3 hour, be added dropwise 5-8 parts by weight concentration be 6-8% aqueous hydrogen peroxide solution, raise temperature be
70-80 DEG C, insulated and stirred 10-20 minutes is mixed with the alcoholic solution of above-mentioned Tri-isopropylphenyl phosphate, is stirred to normal temperature, is obtained hydroxyl
The fire-retardant calcium carbonate soln of base；
（4）3,4- diaminobenzoic acids, the POCl3 mixing of 7-9 parts by weight of 10-13 parts by weight are taken, compound weight is added to
In the deionized water of 40-50 times of amount, stir, the fire-retardant calcium carbonate soln of pentaerythrite, hydroxyl, titanium with 10-16 parts by weight
Sol dispersion is mixed, and is sent in reactor, insulation reaction 70-80 minutes at 190-210 DEG C, discharging cooling, obtains amino phosphorus
It is esterified colloidal sol；
（5）The DMAP of 0.1-0.2 parts by weight is taken to be added to the DIPEA of 16-20 times of its weight
In, stir, obtain amine dispersion liquid；
（6）The styrene of 170-190 parts by weight is taken, in the absolute ethyl alcohol for being added to 1.6-2 times of its weight, 3-4 parts by weight are added
18 phosgenes, magnetic agitation 20-30 minutes is distilled off ethanol, obtains chloride styrene；
（7）Take in above-mentioned amino phosphotidic colloidal sol, the tetrahydrofuran for being added to 2-3 times of its weight, stir, add amine and disperse
Liquid, is sent in ice-water bath, and above-mentioned chloride styrene is added dropwise, and tetrahydrofuran is distilled off in stirring reaction 2-3 hours, discharging,
Obtain phosphotidic calcium carbonate styrene monomer colloidal sol；
（8）The ammonium persulfate of 6-8 parts by weight is taken, in the deionized water for being added to 57-60 times of its weight, is stirred；
（9）Above-mentioned phosphotidic calcium carbonate styrene monomer colloidal sol is taken, mixes, stirs with the citric acid of 1-2 parts by weight, is sent into
Into reactor, nitrogen is passed through, above-mentioned ammonium persulfate aqueous solution is added, stirs, rise temperature is 75-80 DEG C, adds 4-5
The stannous octoate of parts by weight, insulation reaction 5-6 hours adds the pentane foaming agent of 10-14 parts by weight, and rise temperature is 110-
120 DEG C, 2-3 hours are incubated, product is sent in foaming machine, in 0.3- by cooling discharging after washing, dry, screening
Steam is heated 1-2 hours at 0.4Mpa, 140-150 DEG C, discharging, room temperature cooling, produces the fire-retardant phosphotidic sol-gel modified poly-
Benzene composite material.
Advantages of the present invention：
The present invention uses titanyl sulfate for presoma, is hydrolyzed in the basic conditions, then with POCl3,3,4- diaminourea
Benzoic acid is raw material, is mixed with titanium colloidal sol, by esterification, obtains amino phosphotidic colloidal sol, then styrene is carried out into acyl chlorides
Change is handled, and is catalyzed under the alkaline solution of the DIPEA of DMAP, molten with amino phosphotidic
Glue blended cross linking, obtains phosphotidic calcium carbonate styrene monomer colloidal sol, then is polymerize with this monomer, is sent out by pentane foaming agent
Bubble, obtains composite；
The titanium colloidal sol that composite of the present invention is added can effectively improve the bacteriostasis property of finished-product material, with hydroxylating calcium carbonate
Blending, by being crosslinked again after amino phosphide, is finally polymerize as monomer so that titanium dioxide, calcium carbonate can be with
It is effectively dispersed in polymer, effectively reduces reunion, improves the stability_intensity of finished composite material；
The composite of the present invention produces non-flammable gases in combustion, the system for being in molten state is expanded into one
Step foaming, at the same time, phosphatization ester dehydration carbonization form inorganic matter and charcoal residue, and system is further expanded foamed, are formed
Uniform foamed char, and the calcium carbonate added can further promote the formation of uniform fine and close carbon-coating, the carbon-coating can have
The thermal decomposition product of the prevention material internal of effect enters flame zone, and prevents the oxygen of outside from entering in matrices of composite material, rises
To heat-insulated, oxygen barrier effect, phosphatization ester serves the effect of cooperative flame retardant with inorganic filler, improves the fire prevention of finished-product material
Property；
The composite stability of the present invention is good, and combination property is superior, by monomer doping citric acid, also with more preferable insulation
Performance, the present invention, as inorganic filler, changes the high hard material such as conventionally employed graphene, silica using calcium carbonate,
The proportion of finished product is effectively reduced, the effect of lightweight is realized, is readily transported, processes, installs, cost is reduced, the present invention
Composite environmental protection it is good, harm is not resulted in environment and human body, it is safe to use.
Embodiment
Embodiment 1
A kind of preparation method of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic, comprises the following steps：
（1）The Tri-isopropylphenyl phosphate of 1 parts by weight is taken, in the absolute ethyl alcohol for being added to 10 times of its weight, is stirred；
（2）The titanyl sulfate of 16 parts by weight is taken, in the deionized water for being added to 30 times of its weight, is stirred, concentration, which is added dropwise, is
10% ammoniacal liquor, regulation pH is 10, and stirring reaction 1 hour adds the sodium carboxymethylcellulose of 0.1 parts by weight, stirs, obtain
Titanium sol dispersion；
（3）Calcium oxide, the sodium carbonate mixing of 20 parts by weight of 20 parts by weight are taken, the deionized water of 40 times of compound weight is added to
In, stir 2 hours, the concentration that 5 parts by weight are added dropwise is 6% aqueous hydrogen peroxide solution, rise temperature is 70 DEG C, insulated and stirred 10
Minute, mixed with the alcoholic solution of above-mentioned Tri-isopropylphenyl phosphate, stir to normal temperature, obtain the fire-retardant calcium carbonate soln of hydroxyl；
（4）3,4- diaminobenzoic acids, the POCl3 mixing of 7 parts by weight of 10 parts by weight are taken, compound weight 40 is added to
In deionized water again, stir, the fire-retardant calcium carbonate soln of pentaerythrite, hydroxyl with 10 parts by weight, titanium sol dispersion
Mixing, is sent in reactor, insulation reaction 70 minutes at 190 DEG C, discharging cooling, obtains amino phosphotidic colloidal sol；
（5）The DMAP of 0.1 parts by weight is taken to be added in the DIPEA of 16 times of its weight, stirring is equal
It is even, obtain amine dispersion liquid；
（6）The styrene of 170 parts by weight is taken, in the absolute ethyl alcohol for being added to 1.6 times of its weight, 18 carbon of 3 parts by weight are added
Acyl chlorides, magnetic agitation 20 minutes, is distilled off ethanol, obtains chloride styrene；
（7）Above-mentioned amino phosphotidic colloidal sol is taken, in the tetrahydrofuran for being added to 2 times of its weight, is stirred, amine is added and disperses
Liquid, is sent in ice-water bath, and above-mentioned chloride styrene is added dropwise, and stirring reaction 2 hours, discharging is distilled off tetrahydrofuran, obtained
Phosphotidic calcium carbonate styrene monomer colloidal sol；
（8）The ammonium persulfate of 6-8 parts by weight is taken, in the deionized water for being added to 57 times of its weight, is stirred；
（9）Above-mentioned phosphotidic calcium carbonate styrene monomer colloidal sol is taken, mixes, stirs with the citric acid of 1 parts by weight, be sent to
In reactor, nitrogen is passed through, above-mentioned ammonium persulfate aqueous solution is added, stirs, rise temperature is 75 DEG C, adds 4 parts by weight
Stannous octoate, insulation reaction 5 hours, add 10 parts by weight pentane foaming agent, rise temperature be 110 DEG C, be incubated 2 hours,
Cooling discharging, product is sent in foaming machine after washing, dry, screening, steam heating 1 is small at 0.3Mpa, 140 DEG C
When, discharging, room temperature cooling produces the sol-gel modified poly styrene composite material of fire-retardant phosphotidic.
Performance test：
The fire resistance of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic of the present embodiment 1, mechanical experimental results
Show：
Oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, bending strength 0.29Mpa, compressive strength 0.22Mpa, heat conduction
Coefficient 0.031w/m.k.
Embodiment 2
A kind of preparation method of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic, comprises the following steps：
（1）The Tri-isopropylphenyl phosphate of 2 parts by weight is taken, in the absolute ethyl alcohol for being added to 13 times of its weight, is stirred；
（2）The titanyl sulfate of 20 parts by weight is taken, in the deionized water for being added to 40 times of its weight, is stirred, concentration, which is added dropwise, is
11% ammoniacal liquor, regulation pH is 12, and stirring reaction 2 hours adds the sodium carboxymethylcellulose of 0.2 parts by weight, stirs, obtain
Titanium sol dispersion；
（3）Calcium oxide, the sodium carbonate mixing of 27 parts by weight of 24 parts by weight are taken, the deionized water of 50 times of compound weight is added to
In, stir 3 hours, the concentration that 8 parts by weight are added dropwise is 8% aqueous hydrogen peroxide solution, rise temperature is 80 DEG C, insulated and stirred 20
Minute, mixed with the alcoholic solution of above-mentioned Tri-isopropylphenyl phosphate, stir to normal temperature, obtain the fire-retardant calcium carbonate soln of hydroxyl；
（4）3,4- diaminobenzoic acids, the POCl3 mixing of 9 parts by weight of 13 parts by weight are taken, compound weight 50 is added to
In deionized water again, stir, the fire-retardant calcium carbonate soln of pentaerythrite, hydroxyl with 16 parts by weight, titanium sol dispersion
Mixing, is sent in reactor, insulation reaction 80 minutes at 210 DEG C, discharging cooling, obtains amino phosphotidic colloidal sol；
（5）The DMAP of 0.2 parts by weight is taken to be added in the DIPEA of 20 times of its weight, stirring is equal
It is even, obtain amine dispersion liquid；
（6）The styrene of 190 parts by weight is taken, in the absolute ethyl alcohol for being added to 2 times of its weight, 18 phosphinylidynes of 4 parts by weight are added
Chlorine, magnetic agitation 30 minutes, is distilled off ethanol, obtains chloride styrene；
（7）Above-mentioned amino phosphotidic colloidal sol is taken, in the tetrahydrofuran for being added to 3 times of its weight, is stirred, amine is added and disperses
Liquid, is sent in ice-water bath, and above-mentioned chloride styrene is added dropwise, and stirring reaction 3 hours, discharging is distilled off tetrahydrofuran, obtained
Phosphotidic calcium carbonate styrene monomer colloidal sol；
（8）The ammonium persulfate of 6-8 parts by weight is taken, in the deionized water for being added to 60 times of its weight, is stirred；
（9）Above-mentioned phosphotidic calcium carbonate styrene monomer colloidal sol is taken, mixes, stirs with the citric acid of 2 parts by weight, be sent to
In reactor, nitrogen is passed through, above-mentioned ammonium persulfate aqueous solution is added, stirs, rise temperature is 80 DEG C, adds 5 parts by weight
Stannous octoate, insulation reaction 6 hours, add 14 parts by weight pentane foaming agent, rise temperature be 120 DEG C, be incubated 3 hours,
Cooling discharging, product is sent in foaming machine after washing, dry, screening, steam heating 2 is small at 0.4Mpa, 150 DEG C
When, discharging, room temperature cooling produces the sol-gel modified poly styrene composite material of fire-retardant phosphotidic.
Performance test：
The fire resistance of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic of the present embodiment 2, mechanical experimental results
Show：
Oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, bending strength 0.27Mpa, compressive strength 0.16Mpa, heat conduction
Coefficient 0.030w/m.k.
Claims (1)
1. a kind of preparation method of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic, it is characterised in that including following step
Suddenly：
（1）The Tri-isopropylphenyl phosphate of 1-2 parts by weight is taken, in the absolute ethyl alcohol for being added to 10-13 times of its weight, stirring is equal
It is even；
（2）The titanyl sulfate of 16-20 parts by weight is taken, in the deionized water for being added to 30-40 times of its weight, is stirred, is added dropwise
Concentration is 10-11% ammoniacal liquor, and regulation pH is 10-12, and stirring reaction 1-2 hours, the carboxymethyl for adding 0.1-0.2 parts by weight is fine
The plain sodium of dimension, stirs, obtains titanium sol dispersion；
（3）Calcium oxide, the sodium carbonate mixing of 20-27 parts by weight of 20-24 parts by weight are taken, 40-50 times of compound weight is added to
Deionized water in, stir 2-3 hour, be added dropwise 5-8 parts by weight concentration be 6-8% aqueous hydrogen peroxide solution, raise temperature be
70-80 DEG C, insulated and stirred 10-20 minutes is mixed with the alcoholic solution of above-mentioned Tri-isopropylphenyl phosphate, is stirred to normal temperature, is obtained hydroxyl
The fire-retardant calcium carbonate soln of base；
（4）3,4- diaminobenzoic acids, the POCl3 mixing of 7-9 parts by weight of 10-13 parts by weight are taken, compound weight is added to
In the deionized water of 40-50 times of amount, stir, the fire-retardant calcium carbonate soln of pentaerythrite, hydroxyl, titanium with 10-16 parts by weight
Sol dispersion is mixed, and is sent in reactor, insulation reaction 70-80 minutes at 190-210 DEG C, discharging cooling, obtains amino phosphorus
It is esterified colloidal sol；
（5）The DMAP of 0.1-0.2 parts by weight is taken to be added to the DIPEA of 16-20 times of its weight
In, stir, obtain amine dispersion liquid；
（6）The styrene of 170-190 parts by weight is taken, in the absolute ethyl alcohol for being added to 1.6-2 times of its weight, 3-4 parts by weight are added
18 phosgenes, magnetic agitation 20-30 minutes is distilled off ethanol, obtains chloride styrene；
（7）Take in above-mentioned amino phosphotidic colloidal sol, the tetrahydrofuran for being added to 2-3 times of its weight, stir, add amine and disperse
Liquid, is sent in ice-water bath, and above-mentioned chloride styrene is added dropwise, and tetrahydrofuran is distilled off in stirring reaction 2-3 hours, discharging,
Obtain phosphotidic calcium carbonate styrene monomer colloidal sol；
（8）The ammonium persulfate of 6-8 parts by weight is taken, in the deionized water for being added to 57-60 times of its weight, is stirred；
（9）Above-mentioned phosphotidic calcium carbonate styrene monomer colloidal sol is taken, mixes, stirs with the citric acid of 1-2 parts by weight, is sent into
Into reactor, nitrogen is passed through, above-mentioned ammonium persulfate aqueous solution is added, stirs, rise temperature is 75-80 DEG C, adds 4-5
The stannous octoate of parts by weight, insulation reaction 5-6 hours adds the pentane foaming agent of 10-14 parts by weight, and rise temperature is 110-
120 DEG C, 2-3 hours are incubated, product is sent in foaming machine, in 0.3- by cooling discharging after washing, dry, screening
Steam is heated 1-2 hours at 0.4Mpa, 140-150 DEG C, discharging, room temperature cooling, produces the fire-retardant phosphotidic sol-gel modified poly-
Benzene composite material.
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2017
- 2017-04-14 CN CN201710242520.7A patent/CN106995565A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108623907A (en) * | 2018-05-15 | 2018-10-09 | 温州市赢创新材料技术有限公司 | A kind of Sun-proof bamboo moulding material and preparation method thereof |
| CN111411250A (en) * | 2020-04-07 | 2020-07-14 | 中国科学技术大学 | Expandable microsphere foaming agent, preparation method thereof and foaming material |
| CN111411250B (en) * | 2020-04-07 | 2021-07-09 | 广东广纳新材料有限公司 | Expandable microsphere foaming agent, preparation method thereof and foaming material |
| CN117467210A (en) * | 2023-12-28 | 2024-01-30 | 南方珠江科技有限公司 | Wind power generation cable with high wear resistance |
| CN117467210B (en) * | 2023-12-28 | 2024-03-08 | 南方珠江科技有限公司 | Wind power generation cable with high wear resistance |
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