CN115521394A - High-flame-retardancy polystyrene foam material and preparation method thereof - Google Patents
High-flame-retardancy polystyrene foam material and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/16—Making expandable particles
- C08J9/18—Making expandable particles by impregnating polymer particles with the blowing agent
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—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
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
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- C08F212/08—Styrene
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- C08J9/0066—Use of inorganic compounding ingredients
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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
- C08J9/14—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 organic
- C08J9/141—Hydrocarbons
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
- C08J9/232—Forming foamed products by sintering expandable particles
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- 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
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/08—Copolymers of styrene
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/325—Calcium, strontium or barium phosphate
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Abstract
The invention discloses a high flame-retardant polystyrene foam material and a preparation method thereof, belonging to the technical field of foam materials and comprising the following steps: preparing monomers by utilizing p-amino styrene and diphenyl chlorophosphate; carrying out suspension polymerization on styrene, a flame-retardant monomer, graphite and BPO by adopting a disperse phase to obtain beads; preparing the beads, the calcium hydroxy phosphate and the n-pentane into composite beads, and finally pre-foaming and superheated steam foaming and forming. According to the invention, the polystyrene beads are prepared by polymerizing the flame-retardant monomer and styrene, and on one hand, the flame-retardant monomer is distributed on the side chain of the polystyrene molecular chain in a chemical bonding manner, so that the compatibility problem of polystyrene and flame-retardant components is solved, and the effects of high-efficiency flame retardance and no negative influence on the mechanical formation of polystyrene are achieved; on the other hand, the graphite plays a role in heat insulation, and can be used for realizing synergistic flame retardance with flame retardant components in the flame retardant monomer, so that the flame retardant and heat insulation performance of the polystyrene foam is further improved.
Description
Technical Field
The invention belongs to the technical field of foaming materials, and particularly relates to a high-flame-retardancy polystyrene foaming material and a preparation method thereof.
Background
The polystyrene foam plastic is prepared by taking polystyrene resin as a main body and adding additives such as a foaming agent and the like, and is a most used buffer material at present. It has closed pore structure, small water absorption and excellent water resistance; the density is small, generally 0.015-0.03; the mechanical strength is good, and the buffering performance is excellent; the processability is good, and the molding forming is easy; good colorability, strong temperature adaptability, excellent radiation resistance and the like, and has high dimensional precision and uniform structure. And therefore its occupancy is high in exterior wall insulation.
The polystyrene material is a polymer material mainly containing C, H elements, is a rigid foam plastic with a closed cell structure, is in a thin-wall and porous state after foaming, is one of materials with the lowest limit oxygen index in all polymer materials, is extremely easy to burn, can be ignited at a lower temperature, and can be burnt violently once being ignited, flame spreads to the whole surface at a high speed, so that the base material is highly contracted and melted without forming carbon, and simultaneously, a large amount of black smoke, toxic gas and molten drops with open fire are generated, and the burning development is more serious.
Chinese patent (201310018147.9) discloses a fireproof flame-retardant polystyrene foam, which has the technical key points that: inorganic flame retardant, water-soluble adhesive, inorganic dispersant, strength enhancer, water and foaming agent are added into polystyrene foam plastic particles extracted by mixing waste polystyrene foam plastic and common polystyrene foam plastic particles. Wherein the inorganic flame retardant is one of titanium oxide, aluminum oxide or boric acid. The compatibility of the flame-retardant component used by the method and polystyrene foam particles is poor, and the flame-retardant property and the mechanical property of the obtained polystyrene material are difficult to meet the use requirements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high-flame-retardancy polystyrene foam material and a preparation method thereof.
The invention prepares polystyrene beads by carrying out dispersed phase suspension polymerization on self-synthesized flame-retardant monomer and styrene, and finally obtains polystyrene foam material by a foaming process; on one hand, the flame-retardant monomer not only contains a styrene structure, and can participate in the polymerization process of polystyrene, so that the flame-retardant component (phosphate component) contained in the flame-retardant monomer is distributed on the side chain of the polystyrene molecular chain in a chemical bonding manner, thereby solving the problem of compatibility of the polystyrene and the flame-retardant component, and achieving the effects of high-efficiency flame retardance and no negative influence on the mechanical formation of the polystyrene; on the other hand, graphite is added in the polymerization process, the graphite is used as a sheet-like material, and the graphite can promote the dispersion of the graphite in polystyrene in the polymerization process, so that the graphite plays a heat insulation role, and can be synergistically flame-retardant (physically and chemically combined) with flame-retardant components in a flame-retardant monomer, thereby further improving the flame-retardant and heat-insulating properties of polystyrene foam.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a high-flame-retardancy polystyrene foam material comprises the following steps:
s1, adding p-aminostyrene, benzene and triethylamine into a round-bottom flask, placing the round-bottom flask in an ice bath condition, slowly dropping diphenyl chlorophosphate into the flask by using a constant-pressure dropping funnel, stirring and reacting for 1h under the ice bath condition after dropping is finished, performing reflux reaction for 2h, and performing rotary evaporation on a product to remove a solvent to obtain a flame-retardant monomer;
-NH on p-amino styrene molecule 2 Reacting with halogenated groups on molecules of diphenyl chlorophosphate to obtain a flame-retardant monomer, wherein the flame-retardant monomer contains a flame-retardant active component and a styrene structure, so that the flame-retardant monomer can participate in the subsequent chemical reaction process;
s2, putting styrene and a flame-retardant monomer into a high-pressure reaction kettle, adding graphite and BPO (benzoyl peroxide) into the kettle, starting stirring (the rotating speed is 500 r/min), setting the temperature in the kettle to be 82-84 ℃, adding a dispersant solution into the reaction kettle when the viscosity of the system reaches 1200cP, setting the temperature in the kettle to be 79 ℃ and keeping for 90min, raising the temperature in the kettle to 81 ℃ and keeping for 4h, raising the temperature to 86 ℃ at the temperature raising rate of 5 min/DEG C after beads in the reaction kettle sink in water, keeping for 6.5h, cooling the temperature of the system to be below 40 ℃, discharging, and obtaining the beads through separation, washing, drying and screening;
preparing polystyrene beads through dispersed phase suspension polymerization;
s3, putting the beads obtained in the step S2, calcium hydroxy phosphate and n-pentane into a high-pressure reaction kettle, starting stirring for 30min, then sealing the kettle, setting the rotation speed to be 550r/min, setting the temperature in the kettle to be 90 ℃, stirring for 6h at constant temperature, then starting cooling, reducing the temperature to be below 30 ℃, starting the kettle, discharging, washing and drying to obtain composite beads;
and S4, storing the composite beads under a closed condition of 35 ℃ for 20d, then pre-foaming the composite beads, specifically, placing the composite beads at 95 ℃ for 2-3min, placing the pre-foamed composite beads at normal temperature and normal pressure for 24h (at the moment, air can permeate into cells through a cell membrane, the internal pressure of the cells is balanced with the external pressure, so that the cell structures are more elastic), finally placing the composite beads in a mold, introducing superheated steam for heating, maintaining the heating for 10-30S (the beads are expanded again, and a whole block is formed due to the existence of gaps among the expanded particles, so that a foam finished product consistent with the mold style is formed), introducing water for cooling, and then forming the composite beads to obtain the high-flame-retardancy polystyrene foam material.
Further, the ratio of the amounts of p-amino styrene, benzene, triethylamine and diphenyl chlorophosphate in step S1 was 0.01mol.
Further, in step S2, the ratio of the amounts of styrene, flame retardant monomer, graphite, BPO, dispersant solution used was 135g.
Further, the dispersant solution is a solution formed by uniformly mixing a dispersant and water according to the proportion of 2-3g.
Still further, the dispersant is hydroxypropyl methylcellulose or hydroxypropyl cellulose.
Further, the ratio of the amount of beads, calcium hydroxyphosphate and n-pentane used in step S3 was 150g.
The invention has the beneficial effects that:
the invention prepares polystyrene beads by carrying out dispersed phase suspension polymerization on self-synthesized flame-retardant monomer and styrene, and finally obtains polystyrene foam material by a foaming process; on one hand, the flame-retardant monomer not only contains a styrene structure and can participate in the polymerization process of polystyrene, so that the flame-retardant component (phosphate ester component) contained in the flame-retardant monomer is distributed on the side chain of the polystyrene molecular chain in a chemical bonding manner, thereby solving the problem of compatibility of the polystyrene and the flame-retardant component, and achieving the effects of high-efficiency flame retardance and no negative influence on the mechanical formation of the polystyrene; on the other hand, graphite is added in the polymerization process, the graphite is used as a sheet-like material, and the graphite can promote the dispersion of the graphite in polystyrene in the polymerization process, so that the graphite plays a heat insulation role, and can be synergistically flame-retardant (physically and chemically combined) with flame-retardant components in a flame-retardant monomer, thereby further improving the flame-retardant and heat-insulating properties of polystyrene foam.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a high-flame-retardancy polystyrene foam material comprises the following steps:
s1, adding 0.1mol of p-aminostyrene, 50g of benzene and 10g of triethylamine into a round-bottom flask, placing the round-bottom flask in an ice bath condition, slowly dropping 0.1mol of diphenyl chlorophosphate into the flask by using a constant-pressure dropping funnel, stirring and reacting for 1h under the ice bath condition after dropping is finished, performing reflux reaction for 2h, and performing rotary evaporation on a product to remove a solvent to obtain a flame-retardant monomer;
s2, putting 135g of styrene and 10g of flame-retardant monomer into a high-pressure reaction kettle, adding 4g of graphite and 1.5g of BPO (benzoyl peroxide) into the kettle, starting stirring (the rotating speed is 500 r/min), setting the temperature in the kettle to be 82 ℃, adding 300mL of dispersant solution into the reaction kettle when the viscosity of the system reaches 1200cP, setting the temperature in the kettle to be 79 ℃ and keeping for 90min, raising the temperature in the kettle to 81 ℃ and keeping for 4h, raising the temperature to 86 ℃ at the temperature raising rate of 5 min/DEG C after the beads in the reaction kettle sink in water, keeping for 6.5h, finally cooling the temperature of the system to be lower than 40 ℃, discharging, and obtaining the beads through separation, washing, drying and screening; the dispersant solution is formed by uniformly mixing hydroxypropyl methylcellulose and water according to the proportion of 2g;
s3, putting 150g of the beads obtained in the step S2, 1g of calcium hydroxy phosphate and 15.5g of n-pentane into a high-pressure reaction kettle, opening and stirring for 30min, then sealing, setting the rotation speed to be 550r/min, setting the temperature in the kettle to be 90 ℃, stirring at constant temperature for 6h, then opening and cooling, reducing the temperature to be below 30 ℃, opening the kettle, discharging, washing and drying to obtain composite beads;
and S4, storing the composite beads under a sealed condition of 35 ℃ for 20 days, and then pre-foaming, specifically, placing the composite beads at 95 ℃ for 2min, placing the pre-foamed composite beads at normal temperature and normal pressure for 24h, finally placing the composite beads in a mold, introducing superheated steam for heating, keeping heating for 10S, introducing water for cooling, and molding to obtain the high-flame-retardancy polystyrene foam material.
Example 2
A preparation method of a high-flame-retardancy polystyrene foam material comprises the following steps:
s1, adding 0.1mol of p-aminostyrene, 50g of benzene and 10g of triethylamine into a round-bottom flask, placing the round-bottom flask in an ice bath condition, slowly dripping 0.1mol of diphenyl chlorophosphate into the flask by using a constant-pressure dropping funnel, stirring and reacting for 1h under the ice bath condition after dripping is finished, performing reflux reaction for 2h, and performing rotary evaporation on a product to remove a solvent to obtain a flame-retardant monomer;
s2, putting 135g of styrene and 10g of flame-retardant monomer into a high-pressure reaction kettle, adding 4g of graphite and 1.5g of BPO (benzoyl peroxide) into the kettle, starting stirring (the rotating speed is 500 r/min), setting the temperature in the kettle to be 83 ℃, adding 300mL of dispersant solution into the reaction kettle when the viscosity of the system reaches 1200cP, setting the temperature in the kettle to be 79 ℃ and keeping for 90min, raising the temperature in the kettle to 81 ℃ and keeping for 4h, raising the temperature to 86 ℃ at the temperature raising rate of 5 min/DEG C after the beads in the reaction kettle sink in water, keeping for 6.5h, finally cooling the temperature of the system to be lower than 40 ℃, discharging, and obtaining the beads through separation, washing, drying and screening; the dispersing agent solution is formed by uniformly mixing hydroxypropyl cellulose and water according to the proportion of 2.5g;
s3, putting 150g of the beads obtained in the step S2, 1g of calcium hydroxy phosphate and 15.5g of n-pentane into a high-pressure reaction kettle, opening and stirring for 30min, then sealing, setting the rotation speed to be 550r/min, setting the temperature in the kettle to be 90 ℃, stirring at constant temperature for 6h, then opening and cooling, reducing the temperature to be below 30 ℃, opening the kettle, discharging, washing and drying to obtain composite beads;
and S4, storing the composite beads under a sealed condition of 35 ℃ for 20 days, and then pre-foaming, specifically, placing the composite beads at 95 ℃ for 2-3min, placing the pre-foamed composite beads at normal temperature and normal pressure for 24h, finally placing the composite beads in a mold, introducing superheated steam for heating, keeping heating for 20S, introducing water for cooling, and molding to obtain the high-flame-retardancy polystyrene foam material.
Example 3
A preparation method of a high-flame-retardancy polystyrene foam material comprises the following steps:
s1, adding 0.1mol of p-aminostyrene, 50g of benzene and 10g of triethylamine into a round-bottom flask, placing the round-bottom flask in an ice bath condition, slowly dropping 0.1mol of diphenyl chlorophosphate into the flask by using a constant-pressure dropping funnel, stirring and reacting for 1h under the ice bath condition after dropping is finished, performing reflux reaction for 2h, and performing rotary evaporation on a product to remove a solvent to obtain a flame-retardant monomer;
s2, putting 135g of styrene and 10g of flame-retardant monomer into a high-pressure reaction kettle, adding 4g of graphite and 1.5g of BPO (benzoyl peroxide) into the kettle, starting stirring (the rotating speed is 500 r/min), setting the temperature in the kettle to be 84 ℃, adding 300mL of dispersant solution into the reaction kettle when the viscosity of the system reaches 1200cP, setting the temperature in the kettle to be 79 ℃ and keeping for 90min, raising the temperature in the kettle to 81 ℃ and keeping for 4h, raising the temperature to 86 ℃ at the temperature raising rate of 5 min/DEG C after the beads in the reaction kettle sink in water, keeping for 6.5h, finally cooling the temperature of the system to be lower than 40 ℃, discharging, and obtaining the beads through separation, washing, drying and screening; the dispersing agent solution is formed by uniformly mixing hydroxypropyl methyl cellulose and water according to the proportion of 3g;
s3, putting 150g of the beads obtained in the step S2, 1g of calcium hydroxy phosphate and 15.5g of n-pentane into a high-pressure reaction kettle, opening and stirring for 30min, then sealing the kettle, setting the rotation speed to be 550r/min, setting the temperature in the kettle to be 90 ℃, stirring for 6h at constant temperature, then opening and cooling, reducing the temperature to be below 30 ℃, opening the kettle, discharging, washing and drying to obtain composite beads;
and S4, storing the composite beads under a sealed condition of 35 ℃ for 20d, and then pre-foaming, specifically, placing the composite beads at 95 ℃ for 3min, placing the pre-foamed composite beads at normal temperature and normal pressure for 24h, finally placing the composite beads in a mold, introducing superheated steam for heating, keeping heating for 30S, introducing water for cooling, and molding to obtain the high-flame-retardancy polystyrene foam material.
The expanded polystyrene particles obtained in examples 1 to 3 were processed into test specimens, and the following property tests were carried out:
compressive strength: testing the 10% compressive strength by using a universal mechanical testing machine;
and (3) testing the heat conductivity coefficient: testing according to GB/T10294-2008;
apparent density: measured by archimedes drainage method;
and (3) testing the flame retardant property: LOI is tested according to GB/T2408-2008;
the results obtained are shown in the following table:
| example 1 | Example 2 | Example 3 | |
| 10% compressive strength/KPa | 136 | 141 | 138 |
| Thermal conductivity/W.m -1 ·K -1 | 0.0325 | 0.0320 | 0.0324 |
| Apparent density/kg m -3 | 22.1 | 22.0 | 22.1 |
| Expansion ratio | 45.8 | 45.9 | 45.8 |
| LOI/％ | 35.7 | 36.0 | 35.9 |
As can be seen from the data in the table above, the polystyrene foam material obtained by the invention has satisfactory compressive strength and low thermal conductivity, which indicates that the mechanical property and the heat insulation property can meet the requirements; the flame retardant has an LOI coefficient of more than 35 percent, which indicates that the flame retardant has higher flame retardant property.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. The preparation method of the high-flame-retardancy polystyrene foam material is characterized by comprising the following steps of:
s1, adding p-aminostyrene, benzene and triethylamine into a round-bottom flask, placing the round-bottom flask in an ice bath condition, slowly dropping diphenyl chlorophosphate into the flask by using a constant-pressure dropping funnel, stirring and reacting for 1h under the ice bath condition after dropping is finished, performing reflux reaction for 2h, and performing rotary evaporation on a product to remove a solvent to obtain a flame-retardant monomer;
s2, putting styrene and a flame-retardant monomer into a high-pressure reaction kettle, adding graphite and BPO into the kettle, starting stirring, setting the temperature in the kettle to be 82-84 ℃, adding a dispersant solution into the reaction kettle when the viscosity of the system reaches 1200cP, setting the temperature in the kettle to be 79 ℃ and keeping the temperature for 90min, raising the temperature in the kettle to 81 ℃ and keeping the temperature for 4h, raising the temperature to 86 ℃ at a temperature raising rate of 5 min/DEG C after the beads in the reaction kettle sink in water, keeping the temperature for 6.5h, cooling the temperature of the system to be below 40 ℃, discharging, separating, washing, drying and screening to obtain beads;
s3, putting the beads obtained in the step S2, calcium hydroxy phosphate and n-pentane into a high-pressure reaction kettle, starting stirring for 30min, then sealing the kettle, setting the rotation speed to be 550r/min, setting the temperature in the kettle to be 90 ℃, stirring for 6h at constant temperature, then starting cooling, reducing the temperature to be below 30 ℃, starting the kettle, discharging, washing and drying to obtain composite beads;
and S4, storing the composite beads under a sealed condition of 35 ℃ for 20 days, and then pre-foaming, specifically, placing the composite beads at 95 ℃ for 2-3min, placing the pre-foamed composite beads at normal temperature and normal pressure for 24h, finally placing the composite beads in a mold, introducing superheated steam for heating, keeping heating for 10-30S, introducing water for cooling, and molding to obtain the high-flame-retardancy polystyrene foam material.
2. The method for preparing a high flame-retardant polystyrene foam material according to claim 1, wherein the ratio of the amounts of p-amino styrene, benzene, triethylamine and diphenyl chlorophosphate in step S1 is 0.01mol.
3. The preparation method of the high flame-retardant polystyrene foam material according to claim 1, wherein the dosage ratio of the styrene, the flame-retardant monomer, the graphite, the BPO and the dispersant solution in the step S2 is 13510 g.
4. The method for preparing a high flame-retardant polystyrene foam material according to claim 1, wherein the dispersant solution is a solution formed by uniformly mixing a dispersant and water according to a ratio of 2-3g.
5. The method for preparing a high flame-retardant polystyrene foam material according to claim 4, wherein the dispersing agent is hydroxypropyl methyl cellulose or hydroxypropyl cellulose.
6. The method for preparing a high flame-retardant polystyrene foam material according to claim 1, wherein the ratio of the used amount of the beads, the calcium hydroxy phosphate and the n-pentane in the step S3 is 150g.
7. A high flame-retardant polystyrene foam prepared by the method according to any one of claims 1 to 6.
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| CN202211112664.8A CN115521394A (en) | 2022-09-14 | 2022-09-14 | High-flame-retardancy polystyrene foam material and preparation method thereof |
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| CN202211112664.8A CN115521394A (en) | 2022-09-14 | 2022-09-14 | High-flame-retardancy polystyrene foam material and preparation method thereof |
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