CN114656675A - Composite graphite flame-retardant polystyrene bead and preparation method thereof - Google Patents
Composite graphite flame-retardant polystyrene bead and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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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
- C08J9/20—Making expandable particles by suspension polymerisation in the presence of the blowing agent
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/242—Applying crosslinking or accelerating agent onto compounding ingredients such as fillers, reinforcements
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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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
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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Abstract
The invention discloses a composite graphite flame-retardant polystyrene bead and a preparation method thereof, and relates to the technical field of preparation of polystyrene beads. According to the method, cage type Polysilsesquioxane (POSS) is added into a reaction kettle to be used as crosslinking, and the POSS is compounded with a polymer matrix in a copolymerization mode, a grafting mode or a blending mode, so that the composite material has an obvious delayed combustion characteristic, and meanwhile, methyl octabromoether is used as an auxiliary material, so that the flame retardance of polystyrene beads is improved; the composite graphite provided by the invention uses titanate coupling agent or PVP as a modifier of a graphite composite system, changes the surface activity of graphite and carbon black, enables the composite graphite and styrene monomer to be uniformly fused to form high-dispersity liquid drops, and further ensures the uniformity of polystyrene bead products.
Description
Technical Field
The invention relates to the technical field of preparation of polystyrene beads, in particular to a composite graphite flame-retardant polystyrene bead and a preparation method thereof.
Background
The polystyrene foam is classified into molded polystyrene foam (EPS) and extruded polystyrene foam (XPS) according to the manner of molding. EPS and XPS all have closed cell honeycomb structure, and this kind of structure that closes the porosity and make panel have extremely low hydroscopicity and thermal conductivity, higher compressive resistance and ageing resistance. Graphite polystyrene insulation boards are used in polystyrene boards mostly, the graphite polystyrene insulation boards are mainly applied to building insulation structures, the fireproof and flame retardant properties of the graphite polystyrene insulation boards cannot meet the fireproof requirements of national building materials, and the improvement of the flame retardant properties of graphite polystyrene plastics becomes a technical problem to be solved urgently.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of composite graphite flame-retardant polystyrene beads, which improves the flame retardant property.
In order to realize the technical purpose, the invention adopts the following scheme:
the preparation method of the composite graphite flame-retardant polystyrene bead comprises the following steps:
s1, adding 30 parts by weight of styrene monomer into a premixing kettle, starting to stir at normal temperature, and then adding into 4-7 parts by weight of composite graphite premixing kettle to obtain a composite graphite premixing liquid;
the composite graphite consists of graphite, graphitized carbon black and a modifier, wherein the weight ratio of graphite: graphitized carbon black: the mass percent of the modifier is 40-60%: 39-58%: 1-2%;
s2, adding 90-150 parts by weight of pure water into a reaction kettle, starting stirring, respectively adding 0.5-0.8 part by weight of sodium polymethacrylate, 0.1-0.15 part by weight of assistant dispersing agent and 0.001-0.002 part by weight of emulsifier at normal temperature, stirring for 10 minutes, and adding a pH regulator to enable the pH value of the reaction kettle solution to be 8-9; the pH regulator is inorganic alkaline substance, preferably sodium hydroxide.
S3, heating the reaction kettle to 30-40 ℃, adding 70 parts by weight of styrene monomer, and stirring to form a styrene suspension system;
s4, pumping the composite graphite premix solution in the S1 into a reaction kettle, and continuously stirring to form a graphite styrene suspension system, wherein at the moment, the graphite and styrene monomer form liquid drops with the thickness of 0.1-0.5 mm;
s5, heating the reaction kettle to 50-60 ℃, adding 0.3-0.6 part by weight of polyethylene wax, adding 0.5-0.8 part by weight of methyl octabromoether, 0.4-0.8 part by weight of initiator and 0.5-0.8 part by weight of cage-type polysilsesquioxane as crosslinking agents, and continuously stirring uniformly;
s6, raising the temperature in the reaction kettle to 85-95 ℃, wherein the temperature raising rate is 0.8-1.0 ℃/min;
s7, reacting at 85-95 ℃ for 3-5 h, adding a growth promoter according to the particle growth rate, wherein the total amount of the growth promoter is controlled to be 0.1-0.3 weight part;
s8, after the low-temperature reaction is finished, sealing the reaction kettle, and adding 6-9 parts by weight of foaming agent; raising the temperature in the reaction kettle to 120-130 ℃, wherein the temperature raising rate is 1.0-1.2 ℃/min, the high-temperature reaction constant temperature time is 2-4 h, and the reaction is finished;
s9, cooling and discharging, and discharging when the temperature is reduced to 40-50 ℃ to obtain the expandable polystyrene beads.
Further, the modifier in S1 is titanate coupling agent or polyvinylpyrrolidone (PVP).
Furthermore, in S2, the auxiliary dispersing agent is anhydrous sodium sulfate, and the emulsifying agent is sodium octadecyl benzene sulfonate.
Further, the initiator in S5 is any one or more of tert-butyl peroxydiethylhexanoate, tert-butyl peroxybenzoate, tert-butyl peroxyisononanoate, and dicumyl peroxide.
Further, in S7, the growth promoter is sodium hydrogencarbonate.
Further, the foaming agent in S8 is a fluorocarbon.
The polystyrene bead is obtained according to the preparation method of the composite graphite flame-retardant polystyrene bead.
Compared with the prior art, the invention has the beneficial effects that: firstly, cage type Polysilsesquioxane (POSS) is added into a reaction kettle to serve as a cross-linking agent, the POSS is compounded with a polymer matrix in a copolymerization, grafting or blending mode and the like, so that the composite material has an obvious delayed combustion characteristic, and meanwhile, methyl octabromoether is used as an auxiliary material, so that the flame retardance of polystyrene beads is improved; secondly, the composite graphite provided by the invention uses titanate coupling agent or PVP as a modifier of a graphite composite system, changes the surface activity of graphite and carbon black, enables the composite graphite and styrene monomer to be uniformly fused to form high-dispersity liquid drops, and further ensures the uniformity of polystyrene bead products; finally, the method adopts a physical foaming agent fluorocarbon, has the advantages of high foaming times, good foam stability, low bleeding amount and the like, and improves the structural stability of the polystyrene.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to fully understand the objects, features and effects of the invention, but the present invention is not limited thereto.
Example 1
The preparation method of the composite graphite flame-retardant polystyrene bead comprises the following steps:
s1, adding 30 parts by weight of styrene monomer into a premixing kettle, starting to stir at 25 ℃, and then adding into 4 parts by weight of composite graphite premixing kettle to obtain a composite graphite premixing liquid; the composite graphite consists of graphite, graphitized carbon black and a modifier, wherein the weight ratio of graphite: graphitized carbon black: the mass percentage of the titanate coupling agent LD-126 is 60%: 38%: 2 percent.
S2, adding 90 parts by weight of pure water into a reaction kettle, starting stirring, respectively adding 0.5 part by weight of sodium polymethacrylate, 0.1 part by weight of anhydrous sodium sulfate and 0.001 part by weight of sodium octadecylbenzene sulfonate at normal temperature, stirring for 10 minutes, and adding a pH regulator (NaOH) to enable the pH value of the solution in the reaction kettle to be 8.
And S3, heating the reaction kettle to 35 ℃, adding 70 parts by weight of styrene monomer, and stirring to form a styrene suspension system.
And S4, pumping the composite graphite premix solution in the S1 into a reaction kettle, and continuously stirring to form a graphite styrene suspension system, wherein at the moment, the graphite and styrene monomer form liquid drops with the thickness of 0.1-0.5 mm.
S5, heating the reaction kettle to 50 ℃, adding 0.5 weight part of PE3000 polyethylene wax, then adding 0.5 weight part of methyl octabromoether, 0.5 weight part of tert-butyl peroxydiethylhexanoate and 0.5 weight part of cage-type polysilsesquioxane, and continuing to stir uniformly.
S6, raising the temperature in the reaction kettle to 85 ℃, wherein the temperature raising rate is 0.8 ℃/min.
S7, reacting at 85 ℃ for 5h, adding sodium bicarbonate according to the particle growth rate, wherein the total amount of sodium bicarbonate is controlled to be 0.1-0.3 weight part.
S8, after the low-temperature reaction is finished, sealing the reaction kettle and adding 6 parts by weight of fluorocarbon; and (3) raising the temperature in the reaction kettle to 120 ℃, wherein the heating rate is 1.0 ℃/min, the high-temperature reaction constant temperature time is 4 hours, and the reaction is finished.
And S9, cooling and discharging, and discharging when the temperature is reduced to 40 ℃ to obtain the composite graphite polystyrene beads.
Example 2
The preparation method of the composite graphite flame-retardant polystyrene bead comprises the following steps:
s1, adding 30 parts by weight of styrene monomer into a premixing kettle, starting to stir at 25 ℃, and then adding 5 parts by weight of composite graphite into the premixing kettle to obtain a composite graphite premixed solution; the composite graphite consists of graphite, graphitized carbon black and a modifier, wherein the weight ratio of graphite: graphitized carbon black: the mass percent of the titanate coupling agent LD-126 is 60%: 38%: 2 percent.
S2, adding 110 parts by weight of pure water into a reaction kettle, starting stirring, respectively adding 0.7 part by weight of sodium polymethacrylate, 0.13 part by weight of anhydrous sodium sulfate and 0.0015 part by weight of sodium octadecylbenzenesulfonate at normal temperature, stirring for 10 minutes, and adding a pH regulator (NaOH) to enable the pH value of the solution in the reaction kettle to be 8.
And S3, heating the reaction kettle to 30 ℃, adding 70 parts by weight of styrene monomer, and stirring to form a styrene suspension system.
And S4, pumping the composite graphite premix solution in the S1 into a reaction kettle, and continuously stirring to form a graphite styrene suspension system, wherein at the moment, the graphite and styrene monomer form liquid drops with the thickness of 0.1-0.5 mm.
S5, heating the reaction kettle to 50 ℃, adding 0.3 weight part of PE3000 polyethylene wax, then adding 0.8 weight part of methyl octabromoether, 0.4 weight part of tert-butyl peroxydiethylhexanoate and 0.6 weight part of cage-type polysilsesquioxane, and continuing to stir uniformly.
S6, raising the temperature in the reaction kettle to 90 ℃, wherein the temperature raising rate is 0.8 ℃/min.
S7, reacting at 90 ℃ for 4h, adding sodium bicarbonate according to the particle growth rate, wherein the total amount of sodium bicarbonate is controlled to be 0.1-0.3 weight part.
S8, after the low-temperature reaction is finished, sealing the reaction kettle and adding 6 parts by weight of fluorocarbon; and (3) raising the temperature in the reaction kettle to 120 ℃, wherein the rate of temperature rise is 1.0 ℃/min, the constant temperature time of the high-temperature reaction is 4 hours, and the reaction is finished.
And S9, cooling and discharging, and discharging when the temperature is reduced to 40 ℃ to obtain the composite graphite polystyrene beads.
Example 3
The preparation method of the composite graphite flame-retardant polystyrene bead comprises the following steps:
s1, adding 30 parts by weight of styrene monomer into a premixing kettle, starting to stir at 25 ℃, and then adding 7 parts by weight of composite graphite into the premixing kettle to obtain a composite graphite premixed solution; the composite graphite consists of graphite, graphitized carbon black and a modifier, wherein the weight ratio of graphite: graphitized carbon black: the mass percentage of the titanate coupling agent LD-126 is 60%: 38%: 2 percent.
S2, adding 150 parts by weight of pure water into a reaction kettle, starting stirring, respectively adding 0.8 part by weight of sodium polymethacrylate, 0.15 part by weight of anhydrous sodium sulfate and 0.002 part by weight of sodium octadecylbenzene sulfonate at normal temperature, stirring for 10 minutes, and adding a pH regulator (NaOH) to enable the pH value of the solution in the reaction kettle to be 9.
And S3, heating the reaction kettle to 40 ℃, adding 70 parts by weight of styrene monomer, and stirring to form a styrene suspension system.
And S4, pumping the composite graphite premix solution in the S1 into a reaction kettle, and continuously stirring to form a graphite styrene suspension system, wherein at the moment, the graphite and styrene monomer form liquid drops with the thickness of 0.1-0.5 mm.
S5, heating the reaction kettle to 60 ℃, adding 0.6 weight part of PE3000 polyethylene wax, then adding 0.8 weight part of methyl octabromoether, 0.8 weight part of tert-butyl peroxydiethylhexanoate and 0.8 weight part of cage-type polysilsesquioxane, and continuing to stir uniformly.
S6, raising the temperature in the reaction kettle to 95 ℃, wherein the temperature raising rate is 1.0 ℃/min.
S7, reacting at 95 ℃ for 3h, adding sodium bicarbonate according to the particle growth rate, wherein the total amount of sodium bicarbonate is controlled to be 0.1-0.3 weight part.
S8, after the low-temperature reaction is finished, sealing the reaction kettle and adding 9 parts by weight of fluorocarbon; and (3) raising the temperature in the reaction kettle to 130 ℃, wherein the rate of temperature rise is 1.2 ℃/min, the constant temperature time of the high-temperature reaction is 2 hours, and the reaction is finished.
And S9, cooling and discharging, and discharging when the temperature is reduced to 50 ℃ to obtain the composite graphite polystyrene beads.
Example 4
The preparation method of the composite graphite flame-retardant polystyrene bead comprises the following steps:
s1, adding 30 parts by weight of styrene monomer into a premixing kettle, starting to stir at 25 ℃, and then adding into 4 parts by weight of composite graphite premixing kettle to obtain a composite graphite premixing liquid; the composite graphite consists of graphite, graphitized carbon black and a modifier, wherein the weight ratio of graphite: graphitized carbon black: the mass percentage of the polyvinylpyrrolidone is 60%: 38%: 2 percent.
S2, adding 90 parts by weight of pure water into a reaction kettle, starting stirring, respectively adding 0.5 part by weight of sodium polymethacrylate, 0.1 part by weight of anhydrous sodium sulfate and 0.001 part by weight of sodium octadecylbenzene sulfonate at normal temperature, stirring for 10 minutes, and adding a pH regulator (NaOH) to enable the pH value of the solution in the reaction kettle to be 8.
And S3, heating the reaction kettle to 35 ℃, adding 70 parts by weight of styrene monomer, and stirring to form a styrene suspension system.
And S4, pumping the composite graphite premix solution in the S1 into a reaction kettle, and continuously stirring to form a graphite styrene suspension system, wherein at the moment, the graphite and styrene monomer form liquid drops with the thickness of 0.1-0.5 mm.
S5, heating the reaction kettle to 50 ℃, adding 0.5 weight part of PE3000 polyethylene wax, then adding 0.5 weight part of methyl octabromoether, 0.5 weight part of tert-butyl peroxydiethylhexanoate and 0.5 weight part of cage-type polysilsesquioxane, and continuing to stir uniformly.
S6, raising the temperature in the reaction kettle to 85 ℃, wherein the temperature raising rate is 0.8 ℃/min.
S7, reacting at 85 ℃ for 5h, adding sodium bicarbonate according to the particle growth rate, wherein the total amount of sodium bicarbonate is controlled to be 0.1-0.3 weight part.
S8, after the low-temperature reaction is finished, sealing the reaction kettle and adding 6 parts by weight of fluorocarbon; and (3) raising the temperature in the reaction kettle to 120 ℃, wherein the heating rate is 1.0 ℃/min, the high-temperature reaction constant temperature time is 4 hours, and the reaction is finished.
And S9, cooling and discharging, and discharging when the temperature is reduced to 45 ℃ to obtain the composite graphite polystyrene beads.
Comparative example 1
The same method and proportion as in example 1 are adopted, and only POSS in the mixture is removed.
Comparative example 2
The same method and proportion as those of example 1 are adopted, and only the titanate coupling agent LD-126 is replaced by the silane coupling agent with the same mass part.
Comparative example 3
The same method and proportion as in example 1 were adopted, except that the fluorocarbon was replaced with equal parts by mass of n-pentane.
The products obtained in examples 1 to 6 were subjected to performance testing, and the thermal conductivity and compressive strength were tested according to GB/T10801.1-2021, and the combustion performance grades (monomer combustion tests and oxygen indexes) were tested according to DB/T29-88-2014 "national building envelope energy-saving testing technical Specification of Tianjin", the results of which are shown in Table 1.
Table 1 product performance test results
As can be seen from the data in Table 1, the product performance parameters of examples 1-4 are superior to those of comparative examples 1-3, and it can be seen from the two sets of single factor data that the change of the modifier in the composite graphite mainly affects the compressive strength of the product, and the compressive strength of the product is improved by using the titanate coupling agent or PVP. The flame retardant property of the product is improved by adding the cross-linking agent POSS, and the compression strength and the flame retardant property are improved by using the physical foaming agent.
Finally, it is noted that: the above-mentioned list is only the preferred embodiment of the present invention, and naturally those skilled in the art can make modifications and variations to the present invention, which should be considered as the protection scope of the present invention provided they are within the scope of the claims of the present invention and their equivalents.
Claims (7)
1. The preparation method of the composite graphite flame-retardant polystyrene beads is characterized by comprising the following steps:
s1, adding 30 parts by weight of styrene monomer into a premixing kettle, starting to stir at normal temperature, and then adding the styrene monomer into 4-7 parts by weight of composite graphite premixing kettle to obtain composite graphite premixing liquid;
the composite graphite consists of graphite, graphitized carbon black and a modifier, wherein the weight ratio of graphite: graphitized carbon black: the mass percent of the modifier is 40-60%: 39-58%: 1-2%;
s2, adding 90-150 parts by weight of pure water into a reaction kettle, starting stirring, respectively adding 0.5-0.8 part by weight of sodium polymethacrylate, 0.1-0.15 part by weight of assistant dispersing agent and 0.001-0.002 part by weight of emulsifier at normal temperature, stirring for 10 minutes, and adding a pH regulator to enable the pH value of the reaction kettle solution to be 8-9;
s3, heating the reaction kettle to 30-40 ℃, adding 70 parts by weight of styrene monomer, and stirring to form a styrene suspension system;
s4, pumping the composite graphite premix solution in the S1 into a reaction kettle, and continuously stirring to form a graphite styrene suspension system, wherein at the moment, the graphite and styrene monomer form liquid drops with the thickness of 0.1-0.5 mm;
s5, heating the reaction kettle to 50-60 ℃, adding 0.3-0.6 part by weight of polyethylene wax, then adding 0.5-0.8 part by weight of methyl octabromoether, 0.4-0.8 part by weight of initiator and 0.5-0.8 part by weight of cage polysilsesquioxane, and continuing to stir uniformly;
s6, raising the temperature in the reaction kettle to 85-95 ℃, wherein the temperature raising rate is 0.8-1.0 ℃/min;
s7, reacting at 85-95 ℃ for 3-5 h, adding a growth promoter according to the particle growth rate, wherein the total amount of the growth promoter is controlled to be 0.1-0.3 weight part;
s8, after the low-temperature reaction is finished, sealing the reaction kettle, and adding 6-9 parts by weight of foaming agent; raising the temperature in the reaction kettle to 120-130 ℃, raising the temperature at a rate of 1.0-1.2 ℃/min, keeping the temperature for 2-4 h, and finishing the reaction;
s9, cooling and discharging, and discharging when the temperature is reduced to 40-50 ℃ to obtain the expandable polystyrene beads.
2. The method for preparing composite graphite flame-retardant polystyrene beads according to claim 1, wherein the modifier in S1 is a titanate coupling agent or polyvinylpyrrolidone.
3. The method for preparing composite graphite flame-retardant polystyrene beads according to claim 1, wherein the dispersion aid in S2 is anhydrous sodium sulfate, and the emulsifier is sodium octadecylbenzene sulfonate.
4. The method of claim 1, wherein the initiator used in S5 is one or more selected from the group consisting of tert-butyl peroxydiethylhexanoate, tert-butyl peroxybenzoate, tert-butyl peroxyisononanoate and dicumyl peroxide.
5. The method of claim 1, wherein the growth promoter in S7 is sodium bicarbonate.
6. The method of claim 1, wherein the blowing agent of S8 is a fluorocarbon.
7. A polystyrene bead obtained by the method for preparing a composite graphite flame-retardant polystyrene bead according to any one of claims 1 to 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115536916A (en) * | 2022-11-02 | 2022-12-30 | 应急管理部天津消防研究所 | Bromine-containing composite flame retardant and application thereof |
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| CN102675550A (en) * | 2012-05-10 | 2012-09-19 | 华东理工大学 | High-impact-resistance polystyrene polymer and preparation method thereof |
| CN107141384A (en) * | 2016-08-16 | 2017-09-08 | 新疆蓝山屯河新材料有限公司 | A kind of production method of high blackness graphite expandable polystyrene particle |
| CN111635495A (en) * | 2020-06-29 | 2020-09-08 | 刘裕玲 | Cage polysilsesquioxane-graphene modified polystyrene with high thermal conductivity and preparation method thereof |
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- 2022-04-25 CN CN202210436099.4A patent/CN114656675A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675550A (en) * | 2012-05-10 | 2012-09-19 | 华东理工大学 | High-impact-resistance polystyrene polymer and preparation method thereof |
| CN107141384A (en) * | 2016-08-16 | 2017-09-08 | 新疆蓝山屯河新材料有限公司 | A kind of production method of high blackness graphite expandable polystyrene particle |
| CN111635495A (en) * | 2020-06-29 | 2020-09-08 | 刘裕玲 | Cage polysilsesquioxane-graphene modified polystyrene with high thermal conductivity and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115536916A (en) * | 2022-11-02 | 2022-12-30 | 应急管理部天津消防研究所 | Bromine-containing composite flame retardant and application thereof |
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