CN120059281A - Preparation process of polystyrene flame-retardant insulation board - Google Patents
Preparation process of polystyrene flame-retardant insulation board Download PDFInfo
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Abstract
The invention relates to the technical field of polystyrene, and discloses a preparation process of a polystyrene flame-retardant insulation board, and mixing the polystyrene resin, the polystyrene resin-based flame retardant, the aminated silica aerogel, the foaming agent, the nucleating agent and the like in an extruder, and then extruding and foaming to obtain the polystyrene flame-retardant heat-insulating board. The silica aerogel disclosed by the invention is uniformly dispersed in the polystyrene insulation board, so that the heat conductivity coefficient of the insulation board is reduced, and the insulation performance is improved. The polystyrene-based flame retardant contains a nitrogen-containing structure of triazole and a large amount of phosphate structures of dioxaphosphene to form the nitrogen-phosphorus flame retardant, has a good condensed phase flame retardant effect, improves the limiting oxygen index of the heat insulation board, and has better flame retardant property.
Description
Technical Field
The invention relates to the technical field of polystyrene, in particular to a preparation process of a polystyrene flame-retardant heat-insulating board.
Background
After the polystyrene is foamed, the obtained polystyrene foam has the advantages of large porosity, low heat conductivity coefficient, good heat insulation performance, excellent mechanical property, and wide application in the aspects of heat insulation plates, building materials and the like. However, the polystyrene foam board has the defects of easy combustion and the like, and limits the practical application of the polystyrene heat-insulating board in fireproof materials and the like. The above problems can be solved by adding flame retardant to the foam board, and common flame retardant is inorganic flame retardant, nitrogen-phosphorus flame retardant, brominated flame retardant, etc. The nitrogen-phosphorus halogen-free flame retardant has the advantages of environmental protection, small addition amount, good flame retardant effect and the like. Development of novel nitrogen-phosphorus halogen-free flame retardant is a research hotspot.
The silica aerogel is a porous nano solid material with low density and light weight, has very low heat conductivity coefficient, and has important application in the aspects of heat insulation materials, flame retardant materials and the like. And adding silica aerogel into the polystyrene foam material to obtain the novel heat-insulating material with lower heat conductivity coefficient. However, silica aerogel has poor compatibility with polystyrene, and the mechanical properties of the silica aerogel can be influenced by adding the silica aerogel into polystyrene foam materials. Patent CN113736184B discloses a high-strength flame-retardant insulation board and a preparation method thereof, polystyrene, modified silica aerogel, modified expanded graphite, microencapsulated red phosphorus and the like are used as raw materials, and the obtained insulation board has the advantages of high strength and good flame retardance. Compared with the invention, the invention improves the compatibility of the silica aerogel and the polystyrene resin, and improves the mechanical property and the heat insulation property of the polystyrene heat insulation board.
Disclosure of Invention
The invention solves the technical problem that the polystyrene flame-retardant heat-insulating board provided by the invention has good mechanical property, excellent flame retardant property and low heat conductivity coefficient.
The technical scheme is that the preparation process of the polystyrene flame-retardant insulation board comprises the following steps:
Step (1), adding toluene with a structural formula of The intermediate of the flame retardant of (2) is azo-bis-isobutyronitrile, heated to 75-85 ℃ in nitrogen atmosphere, stirred and reacted for 18-24 hours, decompressed and concentrated, filtered and washed by ethanol to obtain the polystyrene-based flame retardant.
And (2) adding 100 parts by weight of polystyrene resin, 8-25 parts by weight of polystyrene resin-based flame retardant, 1-5 parts by weight of aminated silica aerogel, 0.6-0.9 part by weight of foaming agent azodicarbonamide or diisopropyl azodicarboxylate, 0.5-0.7 part by weight of antioxidant 1010, antioxidant 1076 or antioxidant 168 and 2.5-4 parts by weight of nucleating agent talcum powder into a double-screw extruder for melt extrusion, and then extruding and foaming in a single-screw extruder to obtain the polystyrene flame-retardant heat-insulating plate.
Further, in the step (1), the mass ratio of the flame retardant intermediate to the azodiisobutyronitrile is 1 (0.003-0.004).
Further, in the step (2), the temperature of the 1-6 region of the twin-screw extruder is 180-220 ℃, the screw rotating speed is 50-100r/min, the temperature of the 1-3 region of the single-screw extruder is 80-125 ℃, and the screw rotating speed is 50-80r/min.
Further, the preparation process of the amino silica aerogel comprises the steps of adding tetraethoxysilane into ethanol, stirring, dropwise adding a hydrochloric acid solution to adjust the pH value to 3-3.5, heating to 60-65 ℃, stirring for reacting for 1.5-2.5h, cooling, adding N, N-dimethylformamide, stirring, dropwise adding an ethanol solution containing 3-aminopropyl triethoxysilane, wherein the mass ratio of the tetraethoxysilane to the 3-aminopropyl triethoxysilane is 1 (0.7-1.1), stirring, pouring into a mould, standing for gelation, pouring gel into ethanol, heating to 40-50 ℃, aging for 18-24h, taking out the gel, washing with ethanol and petroleum ether in sequence, and drying to obtain the amino silica aerogel.
And S1, adding 5-carboxyl-3-amino-1, 2, 4-triazole, 4-vinylbenzaldehyde and glacial acetic acid with the mass ratio of (0.97-1.07) to (0.76-0.84) into ethanol, heating to 75-80 ℃, condensing and refluxing for 3-5 hours, cooling and filtering, adding precipitate into ethanol, adding sodium borohydride, stirring for 3-4 hours, heating and volatilizing, cooling and crystallizing, washing with water, and drying to obtain an intermediate A. The reaction formula is:
。
And S2, adding an intermediate A, 5-dimethyl-1, 3, 2-dioxaphosphorinane lactam chloride and triethylamine with the mass ratio of 1 (1.52-1.81) (0.83-0.91) into dichloromethane, stirring and reacting for 12-18h at 20-30 ℃, heating and volatilizing, cooling and crystallizing, washing with water and acetone in sequence, and drying to obtain the flame retardant intermediate. The reaction formula is:
。
The method has the beneficial effects that tetraethoxysilane and 3-aminopropyl triethoxysilane are utilized to carry out a cohydrolysis reaction, so that the silicon dioxide aerogel containing amino is obtained. Further azo diisobutyronitrile is used as an initiator to initiate a fire retardant intermediate containing a styrene structure to carry out polymerization reaction, so as to obtain the polystyrene-based fire retardant containing a nitrogen-containing structure of triazole and a large amount of phosphate structures of dioxaphosphites. And then the polystyrene flame-retardant insulation board is obtained by melt blending and extrusion foaming molding with polystyrene resin, amino silica aerogel, polystyrene flame retardant, foaming agent and the like in a single screw extruder.
In the high-temperature melting process, carboxyl groups of the polystyrene-based flame retardant can react with amino groups of the silica aerogel, so that polystyrene molecular chains are grafted on the surface of the silica aerogel, the compatibility of the silica aerogel and polystyrene resin is improved, the aerogel is excellent in dispersion, the influence on the mechanical properties of the insulation board is smaller, and the insulation board can maintain good impact strength and mechanical properties.
The silica aerogel disclosed by the invention is uniformly dispersed in the polystyrene insulation board, so that the heat conductivity coefficient of the insulation board is reduced, and the insulation performance is improved. The polystyrene-based flame retardant disclosed by the invention contains a nitrogen-containing structure of triazole and a large number of phosphate structures of dioxaphosphorite, so that the nitrogen-phosphorus flame retardant is formed, a good condensed phase flame retardant effect is achieved, the limiting oxygen index of the heat insulation board is improved, and the heat insulation board has better flame retardant property.
Drawings
FIG. 1 is a nuclear magnetic resonance hydrogen spectrum of a flame retardant intermediate.
FIG. 2 is an infrared spectrum of a polystyrene based flame retardant.
FIG. 3 is an infrared spectrum of an aminated silica aerogel.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, preferred embodiments of the present invention will be described below with reference to specific examples. The test methods or methods described in the examples below are conventional methods, unless otherwise indicated, and the reagents and materials, unless otherwise indicated, are commercially available or prepared in conventional manners.
Example 1 (1) to 800mL ethanol, 21.4g of 5-carboxy-3-amino-1, 2, 4-triazole, 20g of 4-vinylbenzaldehyde, 15.2g of glacial acetic acid are added, heated to 80 ℃, the mixture is subjected to condensation reflux reaction for 5 hours, cooled and filtered, the precipitate is added to ethanol, 6.2g of sodium borohydride is added, the mixture is stirred and reacted for 4 hours, heated and volatilized, cooled and crystallized, washed with water and dried to obtain an intermediate A.
(2) To 200mL of methylene dichloride, 10g of intermediate A,15.2g of 5, 5-dimethyl-1, 3, 2-dioxaphosphorinane lactam chloride, 8.3g of triethylamine and 30 ℃ are added, and the mixture is stirred and reacted for 12 hours, heated, volatilized, cooled, crystallized, washed by water and acetone in sequence and dried to obtain a flame retardant intermediate. The nuclear magnetic hydrogen spectrogram of FIG. 1 shows that the chemical shift value of the flame retardant intermediate is ：11.09（s,1H）,8.08（m,2H）,7.71（m,2H）,6.08（m,1H）,5.73（m,1H）,5.41（m,1H）,4.96-4.85（m,2H）,4.32-4.09（m,8H）,3.09（s,6H）,2.96（s,6H）.
(3) 40G of the flame retardant intermediate and 0.13g of azobisisobutyronitrile were added to 140mL of toluene, and the mixture was heated to 80℃under a nitrogen atmosphere, stirred and reacted for 18 hours, concentrated under reduced pressure, filtered, and washed with ethanol to obtain a polystyrene-based flame retardant. The infrared spectrum of FIG. 2 shows that 2972cm -1、1477cm-1 is the vibration absorption peak of C-H, CH 2 in the molecular chain of polystyrene, respectively. 3254cm -1 is the absorption peak of carboxyl-OH. 1624cm -1 is the absorption peak of the c=n bond in triazole. 1176cm -1、1058cm-1 are the absorption peaks of the P=O bond and the P-O-C bond, respectively, in the phosphate group. Indicating that the intermediate of the flame retardant is polymerized to produce the polystyrene-based flame retardant.
(4) Adding 20g of ethyl orthosilicate into 20mL of ethanol, stirring, dropwise adding a hydrochloric acid solution with the mass fraction of 0.4% to adjust the pH value to 3, heating to 65 ℃, stirring for reacting for 2 hours, cooling, adding 3mL of N, N-dimethylformamide, stirring, dropwise adding 40mL of ethanol solution containing 17g of 3-aminopropyl triethoxysilane, stirring, pouring into a mould, standing for gelation, pouring the gel into 100mL of ethanol, heating to 40 ℃, aging for 24 hours, taking out the gel, washing with ethanol and petroleum ether in sequence, and drying to obtain the amino silica aerogel. The infrared spectrum of FIG. 3 shows that 1176 cm -1 to 1232cm -1 are the absorption peaks of the silica S-O bonds. Characteristic absorption peaks for amino groups of 1512cm -1 and 697cm -1. It can be seen that amino groups are introduced on the silica aerogel surface.
(5) Adding 1kg of polystyrene resin, 80g of polystyrene flame retardant, 10g of amino silica aerogel, 6.8g of foaming agent azodicarbonamide, 5.7g of antioxidant 1076 and 40g of nucleating agent talcum powder into a double-screw extruder for melt extrusion, wherein the temperature of a 1-6 region is 180 ℃, 195 ℃, 210 ℃, 220 ℃ and 210 ℃ and the screw rotating speed is 100r/min, and then extruding and foaming in a single-screw extruder to obtain the polystyrene flame-retardant heat-insulating plate, wherein the temperature of the 1-3 region is 180 ℃, 205 ℃ and 225 ℃ and the screw rotating speed is 80 r/min.
Example 2 (1) to 600mL ethanol was added 19.4g of 5-carboxy-3-amino-1, 2, 4-triazole, 20g of 4-vinylbenzaldehyde, 16.8g of glacial acetic acid, heated to 75 ℃, subjected to condensation reflux reaction for 3 hours, cooled and filtered, the precipitate was added to ethanol, 6.5g of sodium borohydride was added, stirred and reacted for 3 hours, heated and volatilized, cooled and crystallized, washed with water, and dried to obtain intermediate A.
(2) To 250mL of methylene dichloride, 10g of intermediate A,18.1g of 5, 5-dimethyl-1, 3, 2-dioxaphosphorinane lactam chloride, 9.1g of triethylamine and 20 ℃ are added, and the mixture is stirred and reacted for 18 hours, heated, volatilized, cooled, crystallized, washed by water and acetone in sequence and dried to obtain the flame retardant intermediate.
(3) 40G of the flame retardant intermediate and 0.12g of azobisisobutyronitrile were added to 120mL of toluene, and the mixture was heated to 85℃under a nitrogen atmosphere, stirred and reacted for 18 hours, concentrated under reduced pressure, filtered, and washed with ethanol to obtain a polystyrene-based flame retardant.
(4) Adding 20g of ethyl orthosilicate into 30mL of ethanol, stirring, dropwise adding a hydrochloric acid solution with the mass fraction of 0.4% to adjust the pH value to 3, heating to 65 ℃, stirring for reacting for 2 hours, cooling, adding 3mL of N, N-dimethylformamide, stirring, dropwise adding 40mL of ethanol solution containing 22g of 3-aminopropyl triethoxysilane, stirring, pouring into a mould, standing for gelation, pouring the gel into 100mL of ethanol, heating to 40 ℃, aging for 24 hours, taking out the gel, washing with ethanol and petroleum ether in sequence, and drying to obtain the amino silica aerogel.
(5) Adding 1kg of polystyrene resin, 140g of polystyrene based flame retardant, 20g of amino silica aerogel, 6g of foaming agent azodicarbonamide, 5.7g of antioxidant 1010 and 40g of nucleating agent talcum powder into a double-screw extruder for melt extrusion, wherein the temperature of a 1-6 region is 180 ℃, 195 ℃, 210 ℃, 220 ℃ and 210 ℃, the screw rotating speed is 100r/min, and then extruding and foaming in a single-screw extruder, wherein the temperature of a 1-3 region is 180 ℃, 205 ℃ and 225 ℃ and the screw rotating speed is 50r/min, so as to obtain the polystyrene flame-retardant heat-insulating plate.
Example 3 (1) to 150mL of toluene was added 40g of the flame retardant intermediate (prepared in example 1), 0.16g of azobisisobutyronitrile, heated to 75 ℃ under nitrogen, stirred for 18h, concentrated under reduced pressure, filtered, and washed with ethanol to give a polystyrene based flame retardant.
(2) Adding 20g of ethyl orthosilicate into 25mL of ethanol, stirring, dropwise adding a hydrochloric acid solution with the mass fraction of 0.4% to adjust the pH value to 3.5, heating to 60 ℃, stirring and reacting for 2.5h, cooling, adding 4mL of N, N-dimethylformamide, stirring, dropwise adding 40mL of an ethanol solution containing 14g of 3-aminopropyl triethoxysilane, stirring, pouring into a mold, standing for gelation, pouring the gel into 100mL of ethanol, heating to 45 ℃, aging for 18h, taking out the gel, washing with ethanol and petroleum ether in sequence, and drying to obtain the amino silica aerogel.
(3) Adding 1kg of polystyrene resin, 200g of polystyrene based flame retardant, 35g of aminated silica aerogel, 9g of foaming agent diisopropyl azodicarboxylate, 7g of antioxidant 1076 and 25g of nucleating agent talcum powder into a double-screw extruder for melt extrusion, wherein the temperature of a 1-6 area is 180 ℃, 195 ℃, 210 ℃, 220 ℃ and 210 ℃, the screw rotating speed is 50r/min, and then extruding and foaming in a single-screw extruder, wherein the temperature of a 1-3 area is 180 ℃, 205 ℃ and 225 ℃ and the screw rotating speed is 50r/min, so as to obtain the polystyrene flame-retardant heat-insulating plate.
Example 4 (1) to 150mL of toluene was added 40g of the flame retardant intermediate (prepared in example 1), 0.12g of azobisisobutyronitrile, heated to 80 ℃ under nitrogen atmosphere, stirred for 24 hours, concentrated under reduced pressure, filtered, and washed with ethanol to give polystyrene based flame retardant.
(2) Adding 20g of ethyl orthosilicate into 30mL of ethanol, stirring, dropwise adding a hydrochloric acid solution with the mass fraction of 0.4% to adjust the pH value to 3, heating to 65 ℃, stirring and reacting for 1.5h, cooling, adding 3mL of N, N-dimethylformamide, stirring, dropwise adding 45mL of ethanol solution containing 20g of 3-aminopropyl triethoxysilane, stirring, pouring into a mould, standing for gelation, pouring the gel into 100mL of ethanol, heating to 50 ℃, aging for 18h, taking out the gel, washing with ethanol and petroleum ether in sequence, and drying to obtain the amino silica aerogel.
(3) Adding 1kg of polystyrene resin, 250g of polystyrene based flame retardant, 50g of amino silica aerogel, 8.2g of foaming agent azodicarbonamide, 5g of antioxidant 168 and 30g of nucleating agent talcum powder into a double-screw extruder for melt extrusion, wherein the temperature of a 1-6 area is 180 ℃, 195 ℃, 210 ℃, 220 ℃ and 210 ℃, the screw rotating speed is 50r/min, and then extruding and foaming in a single-screw extruder, wherein the temperature of a 1-3 area is 180 ℃, 205 ℃ and 225 ℃ and the screw rotating speed is 80r/min, so as to obtain the polystyrene flame-retardant heat-insulating plate.
Comparative example 1, this comparative example differs from example 1 in that no polystyrene-based flame retardant was added.
(1) Adding 1kg of polystyrene resin, 10g of amino silica aerogel, 6.8g of foaming agent azodicarbonamide, 5.7g of antioxidant 1076 and 40g of nucleating agent talcum powder into a double-screw extruder for melt extrusion, wherein the temperature of a 1-6 region is 180 ℃, 195 ℃, 210 ℃, 220 ℃ and 210 ℃, the screw rotating speed is 100r/min, and then extruding and foaming in a single-screw extruder, and the temperature of a 1-3 region is 180 ℃, 205 ℃ and 225 ℃ and the screw rotating speed is 80r/min to obtain the polystyrene flame-retardant heat-insulating plate.
Comparative example 2 this comparative example differs from example 1 in that intermediate a was used to prepare polystyrene based flame retardant.
(1) To 140mL of toluene, 40g of intermediate A,0.13g of azobisisobutyronitrile was added, and the mixture was heated to 80℃under a nitrogen atmosphere, stirred and reacted for 18 hours, concentrated under reduced pressure, filtered, and washed with ethanol to obtain a polystyrene-based flame retardant.
(2) Adding 1kg of polystyrene resin, 80g of polystyrene based flame retardant, 10g of amino silica aerogel, 6.8g of foaming agent azodicarbonamide, 5.7g of antioxidant 1076 and 40g of nucleating agent talcum powder into a double-screw extruder for melt extrusion, wherein the temperature of a 1-6 region is 180 ℃, 195 ℃, 210 ℃, 220 ℃ and 210 ℃, the screw rotating speed is 100r/min, and then extruding and foaming in a single-screw extruder, wherein the temperature of a 1-3 region is 180 ℃, 205 ℃ and 225 ℃ and the screw rotating speed is 80r/min, so as to obtain the polystyrene flame-retardant heat-insulating plate.
Comparative example 3 this comparative example differs from example 1 in that no 3-aminopropyl triethoxysilane was added to prepare the silica aerogel.
(1) Adding 20g of ethyl orthosilicate into 20mL of ethanol, stirring, dropwise adding a hydrochloric acid solution with mass fraction of 0.4% to adjust the pH to 3, heating to 65 ℃, stirring for reacting for 2 hours, cooling, adding 3mL of N, N-dimethylformamide, stirring, pouring into a mould, standing for gelation, pouring the gel into 100mL of ethanol, heating to 40 ℃, aging for 24 hours, taking out the gel, washing with ethanol and petroleum ether in sequence, and drying to obtain the silica aerogel.
(2) Adding 1kg of polystyrene resin, 80g of polystyrene flame retardant, 10g of silica aerogel, 6.8g of foaming agent azodicarbonamide, 5.7g of antioxidant 1076 and 40g of nucleating agent talcum powder into a double-screw extruder for melt extrusion, wherein the temperature of a 1-6 region is 180 ℃, 195 ℃, 210 ℃, 220 ℃ and 210 ℃, the screw rotating speed is 100r/min, and then extruding and foaming in a single-screw extruder to obtain the polystyrene flame-retardant heat-insulating plate, wherein the temperature of a 1-3 region is 180 ℃, 205 ℃ and 225 ℃ and the screw rotating speed is 80 r/min.
The compression performance of the polystyrene flame-retardant heat-insulating board is tested according to the method GB/T8813-2020.
The flame retardant property is tested according to the part 2 of the combustion behavior of GB/T2406.2-2009 plastics measured by an oxygen index method, namely a room temperature test method.
And testing the aperture and the porosity of the polystyrene flame-retardant heat-insulating plate by adopting a mercury-pressing aperture analyzer.
The thermal conductivity is tested by referring to the steady-state thermal resistance and related characteristics of the GB/T10294-2008 heat insulation material by a test protection hot plate method.
TABLE 1
Table 1 shows that the limiting oxygen index of the polystyrene flame-retardant heat-insulating plate of the embodiment 1-4 reaches more than 27.9%, the porosity is large, the heat conductivity coefficient is low, the heat-insulating performance is good, the compression strength is large, and the mechanical property is good, because the polystyrene flame retardant and the aminated silica aerogel are added, the carboxyl of the polystyrene flame retardant can react with the amino of the silica aerogel in the high-temperature melting process of the extruder, so that the polystyrene molecular chain is grafted on the surface of the silica aerogel, the compatibility of the silica aerogel and the polystyrene resin is improved, the dispersion of the aerogel is good, the influence on the mechanical property of the heat-insulating plate is smaller, and the heat-insulating plate can maintain good impact strength and mechanical property. Meanwhile, the silica aerogel is uniformly dispersed in the polystyrene insulation board, so that the heat conductivity coefficient of the insulation board is reduced, and the insulation performance is improved. The polystyrene-based flame retardant contains a nitrogen-containing structure of triazole and a large amount of phosphate structures of dioxaphosphene to form the nitrogen-phosphorus flame retardant, has a good condensed phase flame retardant effect, remarkably improves the flame retardant property of the insulation board, and has a higher limiting oxygen index.
The polystyrene-based flame retardant is not added in comparative example 1, the heat-insulating board is easy to burn, the limiting oxygen index is very low, the compression strength is low, and the heat conductivity coefficient is high, because the compatibility of the silica aerogel and the polystyrene resin is poor, the mechanical property of the heat-insulating board is greatly affected, and the silica aerogel is difficult to uniformly disperse in the polystyrene matrix, so that the heat conductivity coefficient of the board is high, and the heat-insulating property is poor.
The polystyrene-based flame retardant obtained in comparative example 2 does not contain a phosphate structure of dioxaphosphorite, has poor flame retardant effect, is easy to burn and has lower limiting oxygen index, but the polystyrene-based flame retardant contains carboxyl and can react with amino of silica aerogel in the high-temperature melting process of an extruder, thereby being beneficial to improving the compatibility of the silica aerogel in polystyrene foaming plates, improving the dispersibility, and being higher in compression strength and lower in heat conductivity coefficient.
The silica aerogel of comparative example 3 does not contain amino groups, cannot react with carboxyl groups of polystyrene-based flame retardants, so that polystyrene molecular chains cannot be grafted on the surface of the silica aerogel, the compatibility of the aerogel and polystyrene resin is poor, the dispersibility is poor, and the compression strength of the plate is low and the heat conductivity coefficient is high.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (8)
1. The preparation process of the polystyrene flame-retardant heat-insulating board is characterized by comprising the following steps of:
Step (1), adding toluene with a structural formula of Heating the intermediate of the flame retardant of (2) azodiisobutyronitrile to a reaction temperature in nitrogen atmosphere, stirring the mixture for reaction, concentrating the mixture under reduced pressure, filtering the mixture, and washing the mixture to obtain the polystyrene-based flame retardant;
And (2) adding 100 parts by weight of polystyrene resin, 8-25 parts by weight of polystyrene resin-based flame retardant, 1-5 parts by weight of amino silica aerogel, 0.6-0.9 part by weight of foaming agent, 0.5-0.7 part by weight of antioxidant and 2.5-4 parts by weight of nucleating agent into a double-screw extruder for melt extrusion, and then extruding and foaming in a single-screw extruder to obtain the polystyrene flame-retardant insulation board.
2. The process for preparing the polystyrene flame-retardant heat-insulating board according to claim 1, wherein the mass ratio of the flame retardant intermediate to the azodiisobutyronitrile in the step (1) is 1 (0.003-0.004).
3. The process for preparing the polystyrene flame-retardant insulation board according to claim 1, wherein the reaction temperature in the step (1) is 75-85 ℃ and the reaction time is 18-24h.
4. The process for preparing a polystyrene flame-retardant insulation board according to claim 1, wherein the foaming agent in the step (2) comprises azodicarbonamide or diisopropyl azodicarbonate, the nucleating agent comprises talcum powder, and the antioxidant comprises antioxidant 1010, antioxidant 1076 or antioxidant 168.
5. The process for preparing a polystyrene flame-retardant insulation board according to claim 1, wherein the temperature of the 1-6 region of the twin-screw extruder in the step (2) is 180-220 ℃, the screw rotation speed is 50-100r/min, the temperature of the 1-3 region of the single-screw extruder is 180-225 ℃ and the screw rotation speed is 50-80r/min.
6. The preparation process of the polystyrene flame-retardant heat-insulating plate according to claim 1, wherein the preparation process of the amino silica aerogel is characterized in that ethyl orthosilicate is added into ethanol, a hydrochloric acid solution is dropwise added after stirring to adjust the pH to 3-3.5, the mixture is heated to 60-65 ℃, the mixture is stirred for 1.5-2.5 hours, N-dimethylformamide is added after cooling, an ethanol solution containing 3-aminopropyl triethoxysilane is dropwise added after stirring, the mixture is poured into a mold after stirring, standing is carried out for gelation, then the gel is poured into ethanol, the mixture is heated to 40-50 ℃, aged for 18-24 hours, the gel is taken out, washed and dried, and the amino silica aerogel is obtained.
7. The preparation process of the polystyrene flame-retardant heat-insulating board according to claim 6, wherein the mass ratio of the tetraethoxysilane to the 3-aminopropyl triethoxysilane is 1 (0.7-1.1).
8. The process for preparing the polystyrene flame-retardant heat-insulating plate according to claim 2, wherein the process for preparing the flame retardant intermediate is as follows:
S1, adding 5-carboxyl-3-amino-1, 2, 4-triazole, 4-vinylbenzaldehyde and glacial acetic acid with the mass ratio of (0.97-1.07) to (0.76-0.84) into ethanol, heating to 75-80 ℃, condensing and refluxing for 3-5 hours, cooling and filtering, adding precipitate into ethanol, adding sodium borohydride, stirring for 3-4 hours, heating and volatilizing, cooling and crystallizing, washing and drying to obtain an intermediate A;
And S2, adding an intermediate A, 5-dimethyl-1, 3, 2-dioxaphosphorinane lactam chloride and triethylamine with the mass ratio of 1 (1.52-1.81) (0.83-0.91) into dichloromethane, stirring and reacting for 12-18h at 20-30 ℃, heating and volatilizing, cooling and crystallizing, washing and drying to obtain the intermediate of the flame retardant.
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| CN120383758A (en) * | 2025-06-27 | 2025-07-29 | 广州孚达保温隔热材料有限公司 | A method for preparing impact-resistant polystyrene extruded board |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN120383758A (en) * | 2025-06-27 | 2025-07-29 | 广州孚达保温隔热材料有限公司 | A method for preparing impact-resistant polystyrene extruded board |
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