CN115612220A - Flame-retardant polystyrene bead, flame-retardant polystyrene insulation board and preparation method - Google Patents
Flame-retardant polystyrene bead, flame-retardant polystyrene insulation board and preparation method Download PDFInfo
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Abstract
The invention relates to a flame-retardant polystyrene bead, a flame-retardant polystyrene insulation board and a preparation method thereof. The method comprises the following steps: pre-foaming and curing the polystyrene beads; based on the mass percentage of polystyrene beadsThe raw materials comprise 10 to 15 percent of flame retardant; adding the cured pre-expanded polystyrene beads to the ungelled SiO 2 Stirring mechanically in the hydrogel to SiO 2 The hydrogel completely wraps the surface of the polystyrene beads; adding phosphoric acid solution until gel is generated, and reacting for 10-20 min; then NaOH solution is added to adjust the pH value of the system to 9.5-10 to obtain SiO 2 Wet gel coated polystyrene beads; mixing SiO 2 And (3) aging, surface modification and supercritical drying the polystyrene beads coated with the wet gel to obtain the flame-retardant polystyrene beads. The technical problem to be solved is how to improve the flame retardant property and the heat insulation property of the polystyrene heat insulation material, so that the heat conductivity coefficient is less than or equal to 0.026W/(m.K), the limiting oxygen index is more than or equal to 35%, the vertical combustion level reaches V0 level, and the horizontal combustion level reaches V2 level to V1 level.
Description
Technical Field
The invention belongs to the technical field of heat insulation materials, and particularly relates to flame-retardant polystyrene beads, a flame-retardant polystyrene heat insulation board and a preparation method.
Background
The traditional polystyrene heat-insulating material in China at present has poor fireproof performance, the combustion performance is mostly B-level, and a large amount of toxic and harmful gases are generated during combustion, the potential safety hazard is large, the mechanical strength is low, and the application is also limited.
SiO 2 The aerogel can effectively penetrate through sunlight and simultaneously prevent infrared heat radiation of environmental temperature, and is an inorganic non-combustible material, so researchers develop a large amount of scientific research work by taking the aerogel as a flame retardant in recent years. However, since in aerogel preparationThe introduction of organic functional groups may result in poor thermal stability of the aerogel material, and these organic components also become potential fire risk factors.
To date, much research has been done on aerogel materials as flame retardant modifiers. The application of the aerogel material as a flame-retardant modifier in a polystyrene heat-insulating material mainly comprises the following two components: one method is to use aerogel particles as cores and adopt a suspension polymerization method to prepare aerogel/polystyrene expandable beads, such as SiO 2 The preparation and forming research of the aerogel PS core-shell composite thermal insulation material are recorded in a related way, but the production process of the method is more complicated and is not suitable for large-scale popularization and application, and the flame retardant and thermal insulation performance of the polystyrene thermal insulation material prepared by the technical means is not greatly improved; and secondly, the aerogel particles are simply added physically in the forming process, but the flame retardant and heat insulation performance of the polystyrene heat insulation material prepared by the technical means is not greatly improved, the heat conductivity coefficient difference of each measurement point of the polystyrene heat insulation material prepared by the method is large, a plurality of flammable points exist in the material, and the problems of poor fireproof performance and poor combustion performance of the polystyrene heat insulation material cannot be solved.
Disclosure of Invention
The invention mainly aims to provide flame-retardant polystyrene beads, a flame-retardant polystyrene insulation board and a preparation method thereof, and aims to solve the technical problems of improving the flame retardance and the heat insulation performance of a polystyrene insulation material, ensuring that the heat conductivity coefficient is less than or equal to 0.026W/(m.K), the limiting oxygen index is more than or equal to 35%, the vertical combustion level reaches V0 level, and the horizontal combustion level reaches V2 level to V1 level, so that the flame-retardant polystyrene beads, the flame-retardant polystyrene insulation board and the preparation method thereof are more suitable for practical use.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a preparation method of flame-retardant polystyrene beads, which comprises the following steps:
1) Pre-foaming and curing the polystyrene beads; the raw materials of the polystyrene beads comprise 10-15% of flame retardant by mass percentage;
2) Adding the cured pre-expanded polystyrene beads to the ungelled SiO 2 In the hydrogel, mechanically stirring until SiO 2 The hydrogel completely wraps the surface of the polystyrene beads; adding phosphoric acid solution until gel is generated, and reacting for 10-20 min; then NaOH solution is added to adjust the pH value of the system to 9.5-10 to obtain SiO 2 Wet gel coated polystyrene beads;
3) Subjecting the SiO 2 And (3) aging, surface modification and supercritical drying the polystyrene beads coated with the wet gel to obtain the flame-retardant polystyrene beads.
The purpose of the invention and the technical problem to be solved can be further realized by adopting the following technical measures.
Preferably, the preparation method is characterized in that the flame retardant is at least one selected from expanded graphite, high ammonium polyphosphate, pentaerythritol, microencapsulated red phosphorus, aluminum hydroxide and zinc borate.
Preferably, in the preparation method, the pre-expansion is performed by placing the polystyrene beads in water vapor at 100 ℃ and keeping the saturated steam pressure of 0.4 to 0.6MPa for 30 to 40 seconds; the curing is to place the pre-expanded polystyrene beads at a position where air flows for 20 to 30 hours at room temperature.
Preferably, the preparation method is as described above, wherein the SiO is 2 The hydrogel was prepared as follows: adding absolute ethyl alcohol and deionized water into inorganic sodium silicate, adjusting the pH value to 3.0-4.0 by using 0.1-1 mol/L phosphoric acid solution, and stirring for 5-10 min; the molar ratio of the inorganic sodium silicate to the absolute ethyl alcohol to the deionized water is 1.
Preferably, the preparation method is as described above, wherein the aging is to form the SiO 2 The polystyrene beads coated by the wet gel are heated to 45-55 ℃ and are kept warm in absolute ethyl alcohol for 12-24 h.
Preferably, in the preparation method, the surface modification is to add the aged polystyrene beads into a mixed solution of hexamethyldisilazane and ethanol to react for 12 to 24 hours; the molar ratio of hexamethyldisilazane to ethanol in the mixed solution is 1:1.
preferably, in the above preparation method, the supercritical drying is to place the surface-modified polystyrene beads in a supercritical drying kettle, introduce carbon dioxide gas into the supercritical drying kettle to perform drying treatment, increase the pressure for 1.5 hours, and perform pressure-maintaining reaction for 8 to 10 hours under the condition of the pressure of 15 to 16 Mpa.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The invention provides a flame-retardant polystyrene bead prepared according to the preparation method of the flame-retardant polystyrene bead.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The invention provides a preparation method of a flame-retardant polystyrene insulation board, which comprises the following steps: filling the flame-retardant polystyrene beads into a mold, introducing high-pressure steam with the pressure of 0.4-0.6 MPa to perform steam compression molding for 180s, and demolding; and (3) drying and aging the demoulded plate at the temperature of 60-70 ℃.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The flame-retardant polystyrene insulation board is prepared according to the preparation method of the flame-retardant polystyrene insulation board provided by the invention.
By means of the technical scheme, the flame-retardant polystyrene bead, the flame-retardant polystyrene insulation board and the preparation method provided by the invention at least have the following advantages:
the invention provides flame-retardant polystyrene beads, a flame-retardant polystyrene insulation board and a preparation method, wherein the polystyrene beads are prepared through suspension polymerization, and the flame retardance of the polystyrene beads is improved by controlling the addition of 10-15% of a flame retardant into a polystyrene raw material; meanwhile, a layer of SiO is uniformly and firmly coated on the surface of the polystyrene bead 2 The aerogel further enhances the flame retardance and the heat insulation of the polystyrene material; furthermore, the invention adopts non-flammable inorganic sodium silicate as a silicon source and phosphoric acid as an acid catalyst and a flame retardant, so that the inorganic sodium silicate and the phosphoric acid have good flame retardance on one hand, and SiO can be avoided on the other hand 2 Introduction of organic components into aerogels to provide two-dimensional propertiesSignificantly improve SiO 2 Flame retardancy and thermal stability of aerogels; as can be seen from the above, the technical scheme of the invention adopts hydrophobic SiO 2 Microcosmically compounding aerogel, coating the surface of the multi-element flame-retardant primary foaming polystyrene bead, and compounding a flame retardant and an inorganic silicon source SiO 2 The comprehensive effect of the aerogel is used for synergistically modifying the flame retardance and the heat insulation of the polystyrene, and the SiO of the super heat-insulating material is exerted to the maximum extent 2 Aerogel and organic heat-insulating material polystyrene, thereby preparing the A-grade molded polystyrene heat-insulating material with low heat conductivity coefficient and combustion performance; specifically, the heat conductivity coefficient of the flame-retardant polystyrene beads and the flame-retardant polystyrene insulation board prepared by the invention is less than or equal to 0.026W/(m.K), the limiting oxygen index is greater than or equal to 35%, the vertical combustion level reaches V0 level, and the horizontal combustion level reaches V2-V1 level; in addition, the preparation method in the technical scheme of the invention has simple and convenient operation, and can prepare polystyrene and prepare SiO (silicon dioxide) as inorganic silicon source in suspension polymerization 2 Based on aerogel, the two are compounded to form a core of polystyrene beads and SiO 2 The aerogel is in a core-shell structure of a shell, and can be used for manufacturing a plate, so that large-scale industrial production can be carried out.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic view of the preparation process of flame-retardant polystyrene beads and an insulation board.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description, the structures, the characteristics and the effects of the flame retardant polystyrene beads, the flame retardant polystyrene insulation board and the preparation method according to the present invention are provided with reference to the accompanying drawings and the preferred embodiments.
The invention provides a preparation method of flame-retardant polystyrene beads, which comprises the following steps as shown in figure 1The method comprises the following steps: pre-foaming polystyrene beads, and curing; the cured pre-expanded polystyrene beads are then added to the ungelled SiO 2 Stirring mechanically in the hydrogel to SiO 2 The hydrogel completely wraps the surface of the polystyrene beads; adding phosphoric acid solution until gel is generated, and reacting for 10-20 min; then NaOH solution is added to adjust the PH value of the system to 9.5 to 10 to obtain SiO 2 Wet gel coated polystyrene beads; subjecting the SiO to 2 And (3) aging, surface modification and supercritical drying the polystyrene beads coated with the wet gel to obtain the flame-retardant polystyrene beads.
In the above technical solution, the polystyrene beads are polymerized by suspension polymerization, and the specific polymerization process is disclosed in the literature "zhao, pander, chen, flame retardant graphite/polystyrene insulation material preparation test research [ J ]," non-metal mine "2022, 1 (45): 34-36.) ", which is not described in detail in this patent. Wherein the polymerization raw materials comprise styrene and a flame retardant; in the technical scheme of the invention, the polymerization raw materials comprise 10-15% of flame retardant by mass percentage. The flame retardant can be a single flame retardant or a composite flame retardant. The flame retardant is selected from at least one of expanded graphite, high ammonium polyphosphate, pentaerythritol, microcapsule red phosphorus, aluminum hydroxide and zinc borate. Furthermore, the flame retardant is selected from at least two of expanded graphite, high ammonium polyphosphate, pentaerythritol, microcapsule red phosphorus, aluminum hydroxide and zinc borate, namely the product prepared by adopting the composite flame retardant has better performance.
When the composite flame retardant is adopted, the technical scheme can obtain better flame retardant effect.
Preferably, the flame retardant is a composite flame retardant of expanded graphite, high ammonium polyphosphate and pentaerythritol, wherein the mass ratio of the expanded graphite to the high ammonium polyphosphate to the pentaerythritol is preferably 5; at the moment, the heat conductivity coefficient of the polystyrene insulation board prepared by the technical scheme of the invention can be as low as 0.024W/(m.K), the limiting oxygen index can reach 41%, the vertical combustion grade reaches V0 grade, and the horizontal combustion grade reaches V1 grade.
Preferably, the flame retardant is a composite flame retardant of expanded graphite, aluminum hydroxide and zinc borate, wherein the mass ratio of the expanded graphite to the aluminum hydroxide to the zinc borate is preferably 5; at the moment, the heat conductivity coefficient of the polystyrene insulation board prepared by the technical scheme of the invention can be as low as 0.025W/(m.K), the limiting oxygen index can reach 38%, the vertical combustion level reaches V0 level, and the horizontal combustion level reaches V1 level.
The polystyrene beads prepared by the above suspension polymerization were pre-expanded and aged. The pre-foaming and curing requirements in the step can adopt the pre-foaming and curing processes of polystyrene beads in the prior art; preferably, the pre-foaming is performed by placing the polystyrene beads in water vapor at 100 ℃ and keeping the polystyrene beads at a saturated steam pressure of 0.4 to 0.6MPa for 30 to 40 seconds; the curing is to place the pre-expanded polystyrene beads at a position where air flows for 20 to 30 hours at room temperature.
In the above technical scheme, the SiO 2 The preparation technology of the hydrogel is critical, and the specific steps are as follows: adding anhydrous ethanol and deionized water into inorganic sodium silicate, and controlling the molar ratio of the inorganic sodium silicate to the anhydrous ethanol to the deionized water to be 1; then, the pH value of the mixed solution is adjusted to 3.0 to 4.0 by using 0.1 to 1mol/L phosphoric acid solution, and the mixed solution is stirred for 5 to 10min to form SiO 2 A hydrogel. The inorganic sodium silicate is selected as the silicon source, on one hand, the low cost of the inorganic sodium silicate is considered, and on the other hand, the inorganic sodium silicate is also more important, so that the introduction of organic components in the hydrogel is reduced or avoided, the thermal stability of the hydrogel is improved, and the organic components are reduced to become potential fire risk factors. The pH value of a phosphoric acid solution adjusting system is selected, and the phosphoric acid has certain flame retardance, so that the system can be adjusted to be in an acid environment to be subjected to hydrolysis reaction, meanwhile, the flame retardance of the phosphoric acid can improve the thermal stability of the phosphoric acid, and potential fire risk factors of the phosphoric acid are reduced.
The polystyrene beads are pre-expanded and cured according to the steps to prepare SiO 2 After the hydrogel, the cured pre-expanded polystyrene beads were added to the ungelled SiO 2 In the hydrogel, mechanically stirring to make the SiO 2 Polystyrene beads completely encapsulated with hydrogelThe surface of the pellet is formed with "aged pre-expanded polystyrene beads" as core and "SiO 2 Hydrogel is a core-shell structure of the shell; then, adding a phosphoric acid solution into the system, taking the phosphoric acid solution as an acid catalyst to perform hydrolysis reaction in the system until gel is generated, and reacting for 10-20 min; then NaOH solution is added into the system to adjust the pH value of the system to 9.5-10, so that the gel undergoes polycondensation reaction to obtain SiO 2 Wet gel coated polystyrene beads. The product structure is now "cured pre-expanded polystyrene beads" as core and "SiO 2 The wet gel "is a core-shell structure of the shell.
Then the SiO is put into 2 Aging the polystyrene beads coated with the wet gel, modifying the surfaces of the polystyrene beads, performing supercritical drying, and drying the SiO coated on the surfaces of the polystyrene beads through sol-gel reaction and supercritical carbon dioxide 2 Wet gel to SiO 2 Obtaining the flame-retardant polystyrene beads by using aerogel; the structure of the flame-retardant polystyrene bead is that ' cured pre-expanded polystyrene bead ' is used as a core and ' SiO 2 Aerogel "is a core-shell structure of the shell. Through the core-shell structure, siO is enabled 2 Aerogel uniformly and firmly wrapped in the polystyrene beads and SiO 2 The silicon source of the aerogel adopts inorganic sodium silicate, so that the introduction of organic components is avoided or reduced to the greatest extent, meanwhile, a flame retardant with the mass percentage of 10-15% is added into the raw materials during suspension polymerization of the polystyrene beads to strengthen the flame retardance of the polystyrene beads, and through the comprehensive application of the technical means, the flame-retardant polystyrene beads prepared by the invention have excellent flame retardance and heat insulation performance, the test data of the embodiment shows that the heat conductivity coefficient of the flame-retardant polystyrene beads prepared by the invention is less than or equal to 0.026W/(m.K), the vertical combustion level reaches V0 level, and the horizontal combustion level reaches V2 level to V1 level.
In the above technical solution, the aging is preferably performed by using the SiO 2 The polystyrene beads coated by the wet gel are heated to 45-55 ℃ and are kept warm in absolute ethyl alcohol for 12-24 h. The surface modification is preferably carried out by adding hexamethyldisilazane and ethanol into aged polystyrene beads and mixingReacting in the solution for 12-24 h; the molar ratio of hexamethyldisilazane to ethanol in the mixed solution is 1:1. the invention carries out SiO 2 The surface modification of the wet gel is preferably carried out by adopting an alkaline system, aiming at avoiding the problem that the surface modification under acidic condition can damage an alkaline coating layer formed on the surface of the particle due to alkaline polycondensation reaction, so that the SiO coated on the surface of the polystyrene bead 2 The wet gel layer can be effectively protected. The supercritical drying is to place the surface modified polystyrene beads into a supercritical drying kettle, introduce carbon dioxide gas into the supercritical drying kettle for drying treatment, boost the pressure for 1.5 hours, and perform pressure-maintaining reaction for 8 to 10 hours under the condition of the pressure of 15 to 16 Mpa; the temperature of the supercritical drying is controlled by the conventional temperature of carbon dioxide drying, generally 30-60 ℃, and is not particularly limited in the patent.
The invention also provides the flame-retardant polystyrene bead prepared by the preparation method of the flame-retardant polystyrene bead. The flame-retardant polystyrene bead has excellent flame-retardant performance and heat-insulating performance, and can be used for preparing a flame-retardant polystyrene heat-insulating plate, so that the polystyrene heat-insulating plate also has excellent flame-retardant performance and heat-insulating performance.
The invention also provides a preparation method of the flame-retardant polystyrene insulation board, which comprises the following steps: filling the flame-retardant polystyrene beads into a mold, introducing high-pressure steam with the pressure of 0.4-0.6 MPa to perform steam compression molding for 180s, and demolding; and (3) drying and aging the demoulded plate at the temperature of 60-70 ℃.
The invention also provides the flame-retardant polystyrene insulation board prepared by the preparation method of the flame-retardant polystyrene insulation board. The flame-retardant polystyrene insulation board has excellent flame-retardant performance and heat-insulating performance. The heat conductivity coefficient is less than or equal to 0.026W/(m.K), the limiting oxygen index is more than or equal to 35%, the vertical combustion grade reaches V0 grade, and the horizontal combustion grade reaches V2 grade to V1 grade.
The present invention will be further described with reference to the following examples, which should not be construed as limiting the scope of the invention, but rather as providing those skilled in the art with the necessary understanding that certain insubstantial modifications and variations of the invention can be made without departing from the spirit and scope of the invention as defined above.
Unless otherwise specified, the following materials, reagents and the like are commercially available products well known to those skilled in the art; unless otherwise specified, all methods are well known in the art. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Example 1
The embodiment of the invention provides a multi-modified flame-retardant polystyrene insulation board, which comprises the following specific steps:
preparation of expandable polystyrene beads:
preparing expandable polystyrene beads by using expanded graphite as a flame retardant and styrene as a polymerization monomer by using a suspension polymerization method for later use; the specific process of the suspension polymerization method in this example is shown in "zhao, pander, chen, gao li yang, reishi, flame retardant graphite/polystyrene insulation material preparation experimental research [ J ]," non-metal mineral "2022, 1 (45): 34-36.) "; the mass percentage of the flame retardant in the polymerization raw materials is 10wt%.
Pre-foaming and curing of polystyrene beads:
placing a certain amount of expandable polystyrene beads in steam at 100 ℃, and pre-expanding for 40s under the saturated steam pressure of 0.6 MPa; then, the pre-expanded polystyrene beads were left at room temperature and allowed to stand for 20 hours for aging while passing air through a good place.
SiO 2 Preparing hydrogel:
adding a proper amount of absolute ethyl alcohol and deionized water into inorganic sodium silicate serving as a silicon source, wherein the molar ratio of the inorganic sodium silicate to the absolute ethyl alcohol to the deionized water is 1; then 1mol/L phosphoric acid dilute solution is used for adjusting the pH value of the solution to be 3.0-4.0, and the solution is stirred for 5-10 min.
Polystyrene bead coating:
to excess ungelled SiO 2 Adding the pre-expanded polystyrene beads into the hydrogel, and mechanically stirring until the surfaces of the polystyrene beads are completely coated with SiO 2 Wrapping the hydrogel; then, adding 1mol/L phosphoric acid solution into the system until gelation occurs, and reacting for 10min; adding 1mol/L NaOH solution to adjust the pH value of the system to be alkaline 9.5-10, then heating to 45-55 ℃, and carrying out heat preservation and aging in absolute ethyl alcohol for 12h; after aging is finished, transferring the aged polystyrene beads to a modification container, adding a mixed solution of hexamethyldisilazane and ethanol with a molar ratio of 1; and finally, placing the surface-modified polystyrene beads in a supercritical drying kettle, introducing carbon dioxide gas for drying treatment, boosting pressure for 1.5h, keeping the pressure for reaction for 8h after the pressure reaches 15MPa, then deflating to normal pressure, and opening the kettle to obtain the coated and modified polystyrene beads.
Preparing a flame-retardant polystyrene insulation board:
filling the prepared coated modified polystyrene beads into a mold, introducing high-pressure steam with the pressure of 0.4MPa, performing steam compression molding for 180s, and demolding; and then, putting the demoulded sample into an environment with the temperature of 60 ℃ for drying and aging treatment to obtain the multi-modified flame-retardant polystyrene insulation board. The technical indexes are shown in table 1 after inspection.
Example 2
The embodiment of the invention provides a multi-element modified flame-retardant polystyrene insulation board, which comprises the following specific steps:
preparation of expandable polystyrene beads:
the difference from example 1 is that: the polymerization raw materials contain 15wt% of a flame retardant, the flame retardant is a composite flame retardant of expanded graphite, high ammonium polyphosphate and pentaerythritol, and the mass ratio of the expanded graphite to the high ammonium polyphosphate to the pentaerythritol is preferably 5.
Pre-foaming and curing of polystyrene beads:
the difference from example 1 is that: the prefoaming is carried out for 30s under the saturated steam pressure of 0.4 MPa; the curing time is 30h.
SiO 2 Preparing hydrogel:
the difference from example 1 is that: the pH value of the solution is adjusted by using 0.5mol/L phosphoric acid dilute solution.
Polystyrene bead coating:
the difference from example 1 is that: the gel reaction time is 20min; the aging time is 24h; the surface modification time is 12h; the supercritical drying is carried out for 10 hours after 16 MPa.
Preparing a flame-retardant polystyrene insulation board:
the same as in example 1. The technical indexes are shown in table 1 after inspection.
Example 3
The embodiment of the invention provides a multi-element modified flame-retardant polystyrene insulation board, which comprises the following specific steps:
preparation of expandable polystyrene beads:
the difference from example 1 is that: the polymerization raw materials contain 12wt% of a flame retardant, the flame retardant is a composite flame retardant of expanded graphite, aluminum hydroxide and zinc borate, and the mass ratio of the expanded graphite to the aluminum hydroxide to the zinc borate is preferably 5.
Pre-foaming and curing of polystyrene beads:
the difference from example 1 is that: the prefoaming is carried out for 35s under the saturated steam pressure of 0.5 MPa; the curing time is 25h.
SiO 2 Preparing hydrogel:
the difference from example 1 is that: the pH value of the solution is adjusted by using 0.1mol/L diluted phosphoric acid solution.
Coating polystyrene beads:
the difference from example 1 is that: the gel reaction time is 15min; the aging time is 24h; the surface modification time is 24h; the supercritical drying is carried out for 10 hours after 15 MPa.
Preparing a flame-retardant polystyrene insulation board:
the same as in example 1. The technical indexes are shown in table 1 after inspection.
Comparative example 1
The comparative example is used for preparing the flame-retardant polystyrene heat-insulation board, and the specific steps are as follows:
preparation of expandable polystyrene beads:
the same as in example 1.
Pre-foaming and curing of polystyrene beads:
the same as in example 1.
Preparing a flame-retardant polystyrene insulation board:
the same as in example 1. The technical indexes are shown in table 1 after inspection.
Comparative example 2
The comparative example is used for preparing the flame-retardant polystyrene heat-insulation board, and the specific steps are as follows:
preparation of expandable polystyrene beads:
the same as in example 1.
Pre-foaming and curing of polystyrene beads:
the same as in example 1.
Preparing a flame-retardant polystyrene insulation board:
mixing 5 percent of SiO with the mass percentage of 40-50 mu m in the prepared pre-expanded polystyrene beads 2 And (3) uniformly stirring the aerogel hydrophobic powder and the aerogel hydrophobic powder, filling the mixture into a mold, and performing the subsequent process as in example 1.
SiO added in this comparative example 2 The aerogel hydrophobic powder can generate an aggregation effect along with airflow when being subjected to steam molding to cause SiO 2 The aerogel hydrophobic powder is unevenly dispersed in the flame-retardant polystyrene insulation board, so that the performance indexes of the flame-retardant polystyrene insulation board prepared by the method of the comparative example have larger difference in parameters at different positions; in the test of the comparative example, 5 points are randomly selected to measure the heat conduction data, and the results are respectively 0.027W/(m.K), 0.032W/(m.K), 0.030W/(m.K), 0.029W/(m.K) and 0.031W/(m.K), wherein the performance of each point has larger fluctuation, and the flame retardant performance is reduced in the area with high heat conductivity coefficient.
TABLE 1
The features of the invention claimed and/or described in the specification may be combined, and are not limited to the combinations set forth in the claims by the recitations therein. The technical solutions obtained by combining the technical features in the claims and/or the specification also belong to the scope of the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of flame-retardant polystyrene beads is characterized by comprising the following steps:
1) Pre-foaming polystyrene beads, and curing; the raw materials of the polystyrene beads comprise 10-15% of flame retardant by mass percentage;
2) Adding the cured pre-expanded polystyrene beads to the ungelled SiO 2 Stirring mechanically in the hydrogel to SiO 2 The hydrogel completely wraps the surface of the polystyrene beads; adding phosphoric acid solution until gel is generated, and reacting for 10-20 min; then NaOH solution is added to adjust the pH value of the system to 9.5-10 to obtain SiO 2 Wet gel coated polystyrene beads;
3) Subjecting the SiO 2 And (3) aging, surface modification and supercritical drying the polystyrene beads coated with the wet gel to obtain the flame-retardant polystyrene beads.
2. The preparation method according to claim 1, wherein the flame retardant is at least one selected from expanded graphite, high ammonium polyphosphate, pentaerythritol, microencapsulated red phosphorus, aluminum hydroxide and zinc borate.
3. The production method according to claim 1, wherein the pre-expansion is carried out by placing the polystyrene beads in steam at 100 ℃ and maintaining the polystyrene beads at a saturated steam pressure of 0.4 to 0.6MPa for 30 to 40 seconds; the curing is to place the pre-expanded polystyrene beads in a position where air flows for 20 to 30 hours at room temperature.
4. The method of claim 1, wherein the SiO is 2 The hydrogel was prepared as follows: adding absolute ethyl alcohol and deionized water into inorganic sodium silicate, adjusting the pH value to 3.0-4.0 by using 0.1-1 mol/L phosphoric acid solution, and stirring for 5-10 min; the molar ratio of the inorganic sodium silicate to the absolute ethyl alcohol to the deionized water is 1.
5. The method of claim 1, wherein the aging is to age the SiO 2 The polystyrene beads coated by the wet gel are heated to 45-55 ℃ and are kept warm in absolute ethyl alcohol for 12-24 h.
6. The preparation method according to claim 1, wherein the surface modification is to add the aged polystyrene beads to a mixed solution of hexamethyldisilazane and ethanol for reaction for 12-24 h; the molar ratio of hexamethyldisilazane to ethanol in the mixed solution is 1:1.
7. the preparation method according to claim 1, wherein the supercritical drying comprises placing the surface-modified polystyrene beads in a supercritical drying kettle, introducing carbon dioxide gas into the supercritical drying kettle for drying, increasing the pressure for 1.5h, and maintaining the pressure under the condition of 15-16 MPa for 8-10 h.
8. A flame-retardant polystyrene bead prepared according to the method for preparing a flame-retardant polystyrene bead of any one of claims 1 to 7.
9. The preparation method of the flame-retardant polystyrene insulation board is characterized by comprising the following steps of: filling the flame-retardant polystyrene beads of claim 8 into a mold, introducing high-pressure steam with the pressure of 0.4-0.6 MPa to perform steam compression molding for 180s, and demolding; and (3) drying and aging the demoulded plate at the temperature of 60-70 ℃.
10. The flame-retardant polystyrene insulation board prepared by the preparation method of the flame-retardant polystyrene insulation board according to claim 9.
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