CN115109298B - Flame-retardant polystyrene composite material and preparation method thereof - Google Patents

Flame-retardant polystyrene composite material and preparation method thereof Download PDF

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CN115109298B
CN115109298B CN202210952413.4A CN202210952413A CN115109298B CN 115109298 B CN115109298 B CN 115109298B CN 202210952413 A CN202210952413 A CN 202210952413A CN 115109298 B CN115109298 B CN 115109298B
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polyvinyl alcohol
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朱建成
王建男
张士亮
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Siyang Lantian New Material Technology Co ltd
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Abstract

The invention discloses a flame-retardant polystyrene composite material and a preparation method thereof. The composite material has good flame retardance and excellent mechanical strength, and can be used for preparing building heat insulation materials.

Description

Flame-retardant polystyrene composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of polystyrene composite materials, and particularly relates to a flame-retardant polystyrene composite material and a preparation method thereof.
Background
In order to realize energy conservation and heat preservation, the building outer wall is usually made of materials such as benzene plates, and the materials have good heat preservation performance, but are easy to age and have a low service life under the combined action of cold and hot alternation, water, air and the like. The heat insulating material is made into the wall body, so that the heat insulating material becomes a good solution. The polystyrene foam material is an excellent substitute, has high strength and light weight, has excellent heat preservation and insulation performance, and is a building heat preservation material which is very popular at present.
Polystyrene is a polymer synthesized by free radical addition polymerization of styrene monomer, is usually amorphous random polymer, is nontoxic, odorless, colorless and transparent, has glass transition temperature higher than 100 ℃, has excellent heat insulation, insulation and transparency, and has good processability and chemical corrosion resistance, but is brittle and easy to crack at low temperature. The polystyrene comprises common polystyrene, expanded polystyrene, high impact polystyrene and syndiotactic polystyrene, wherein the expanded polystyrene has small density, strong oxidation resistance and corrosion resistance, has wide application in the aspects of heat resistance, cold resistance, moisture resistance, vibration resistance, oxidation resistance, noise resistance and the like, and can be used for preparing building thermal insulation materials.
The polystyrene foam material is used for preparing the building thermal insulation material, the most important performance indexes are low thermal conductivity and good mechanical property, the inorganic filler is introduced into the traditional polystyrene foam material for improving the mechanical property, however, the compatibility of the inorganic filler and a polymer matrix is poor, and the stability of a finished product is easily reduced, so that the performance of the product is reduced.
In addition, polystyrene is easy to burn, and a large amount of molten drops are generated during burning, and a large amount of black smoke is accompanied, so that the life and property safety of people are greatly threatened, and the existing polystyrene foaming material is directly used for preparing the building thermal insulation material, so that the fire risk is great. Therefore, the polystyrene foam material must be subjected to flame retardant treatment to be used for preparing the building insulation material.
The flame retardant commonly used for polystyrene mainly comprises red phosphorus, ATH, MH, APP, aluminum hypophosphite, EG and the like, and specifically can be prepared into flame-retardant polystyrene by a melt processing method. However, flame retardant polystyrene prepared by melt processing still has some disadvantages, such as secondary processing of materials, requiring synthesis of polystyrene from monomers by polymerization and subsequent processing. In the processing process, the flame retardant is difficult to achieve a good dispersing effect, and the flame retardant effect and the mechanical strength are affected.
Patent application CN102503519a discloses a composite building insulation material. The building thermal insulation material is a wall filling material, and the composite building thermal insulation material filling material is formed by fully stirring, pouring and curing polystyrene particles and foam concrete or polyurethane particles and foam concrete, wherein the polystyrene particles can be crushed waste polystyrene products, and the polyurethane particles can be crushed waste polyurethane products. The building thermal insulation material obtained by the technology has no flame retardance, has great fire risk and has general mechanical strength.
Patent application CN112497588A discloses a method for preparing a crosslinked polystyrene building insulation material, which comprises subjecting a polystyrene raw material to a crushing treatment, a granulating treatment, a particle size screening treatment and an impurity filtering treatment to obtain polystyrene particles, subjecting the polystyrene particles to a heating and melting treatment and adding a corresponding amount of a crosslinking agent to obtain a polystyrene melt, and subjecting the polystyrene melt to a cooling treatment, a molding treatment, a cutting treatment and a packaging treatment to obtain a polystyrene building insulation board, wherein the crosslinking crystallization degree in the polystyrene is controlled by controlling the adding amount of the crosslinking agent, and fine bubbles are formed in the polystyrene to improve the insulation property of the polystyrene, so that the polystyrene building insulation board which can be assembled and spliced in any form, and has simple manufacture and low manufacture cost is obtained. The technology of the patent does not carry out flame retardant treatment, and the flame retardant effect of the product is general.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a flame-retardant polystyrene composite material and a preparation method thereof, which have good flame retardance and excellent mechanical strength and can be used for preparing building heat-insulating materials.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the flame-retardant polystyrene composite material comprises the following specific steps:
(1) 2 to 3 parts of polyvinyl alcohol and 5 to 6 parts of phytic acid are subjected to esterification reaction to obtain grafted polyvinyl alcohol, and then the grafted polyvinyl alcohol and 1.5 to 2.5 parts of carboxymethyl cellulose cerium are uniformly mixed to obtain a premix;
(2) Coating the premix by using polystyrene to obtain a coated premix;
(3) Taking 8-10 parts of coating premix and 350-400 parts of polystyrene, uniformly stirring, then adding 2.5-3.5 parts of foaming agent and 2-3 parts of perfluorinated hexanone, uniformly stirring, placing in supercritical carbon dioxide fluid for swelling, releasing pressure, and foaming to obtain the flame-retardant polystyrene composite material.
Preferably, in the step (1), the preparation method of the grafted polyvinyl alcohol is as follows: heating polyvinyl alcohol to dissolve in deionized water, adding phytic acid and 4-dimethylaminopyridine, stirring, mixing uniformly, preserving heat at 65-75 ℃ and stirring for 3-4 hours, naturally cooling to room temperature, adding absolute ethyl alcohol, centrifuging to obtain precipitate, drying, and crushing to obtain the grafted polyvinyl alcohol.
Further preferably, the amounts of deionized water, 4-dimethylaminopyridine and absolute ethyl alcohol are 25 to 30 times, 0.8 to 1.2 times and 35 to 40 times of the weight of the polyvinyl alcohol respectively.
Preferably, in the step (1), the polymerization degree of the polyvinyl alcohol is 1800 to 2000.
Preferably, in the step (1), the preparation method of the carboxymethyl cellulose cerium comprises the following steps: dissolving sodium carboxymethylcellulose with water to prepare sodium carboxymethylcellulose aqueous solution with the mass concentration of 0.2-0.3%, dissolving cerium nitrate with water to prepare cerium nitrate aqueous solution with the mass concentration of 0.2-0.3%, dropwise adding the cerium nitrate aqueous solution into the sodium carboxymethylcellulose aqueous solution while stirring, continuously stirring for 10-15 minutes after the dropwise adding, filtering to obtain solid, drying and crushing to obtain the sodium carboxymethylcellulose aqueous solution.
Further preferably, the mass ratio of sodium carboxymethyl cellulose to cerium nitrate is 1:1.5 to 2.
Preferably, the specific method of the step (2) comprises the following steps of: firstly, 9-12 parts of polystyrene is dissolved by using 200-250 parts of ethyl acetate to prepare a polystyrene solution, then 7.5-11.5 parts of premix is added into the polystyrene solution, the mixture is stirred and mixed uniformly to obtain a mixed solution, then 220-260 parts of n-hexane is dropwise added, polystyrene is separated out from the mixed solution and coated on the surface of the premix to form a coating layer, and the coating premix is obtained by centrifuging, taking a precipitate and drying.
Preferably, in the step (3), the foaming agent is n-pentane and isopentane according to a mass ratio of 3-4: 6 to 7.
Preferably, in step (3), the swelling process conditions are: swelling for 2-3 hours at 40-50 ℃ under 25-35 MPa of carbon dioxide.
Preferably, in the step (3), the pressure is relieved to atmospheric pressure at 8-10 MPa/s.
Preferably, in the step (3), the foaming conditions are: the temperature is 100-120 ℃ and the pressure is 0.02-0.03 MPa.
The flame-retardant polystyrene composite material is prepared by the preparation method.
The application of the flame-retardant polystyrene composite material in the preparation of building thermal insulation materials.
Compared with the prior art, the invention has the following beneficial effects:
the invention firstly obtains grafted polyvinyl alcohol by esterification reaction of polyvinyl alcohol and phytic acid, then evenly mixes the polyvinyl alcohol with carboxymethyl cellulose cerium to obtain a premix, then coats the premix by using polystyrene to obtain a coated premix, then mixes the coated premix with polystyrene, a foaming agent and perfluoro-hexanone, swells by supercritical carbon dioxide, relieves pressure and foams to obtain the flame-retardant polystyrene composite material. The composite material has good flame retardance and excellent mechanical strength, and can be used for preparing building heat insulation materials.
1. The polyvinyl alcohol forms a covering layer in the combustion process, and the combustible gas generated by thermal decomposition of the high polymer material is difficult to escape, so that the combustion process is stopped due to anaerobic supplement, the effect of isolating air is achieved, the cracking of the material is inhibited, and the flame retardant effect is achieved. The phytic acid consists of 6 phosphoric acid groups, has high phosphorus content, can generate acidic substances such as metaphosphoric acid and the like by thermal decomposition, promotes the formation of a carbon layer, reduces the heat transfer efficiency, effectively inhibits the generation of volatile substances in a gas phase, and has good flame retardant property. According to the invention, the grafted polyvinyl alcohol is obtained through esterification reaction of the polyvinyl alcohol and the phytic acid, so that the synergistic effect is better, and the flame retardant effect is better.
2. The carboxymethyl cellulose cerium is prepared from sodium carboxymethyl cellulose and cerium nitrate serving as raw materials, contains a large amount of hydroxyl groups, has a synergistic flame-retardant effect on the grafted polyvinyl alcohol, and further improves the flame-retardant effect of the product. Meanwhile, the carboxymethyl cellulose cerium also has a certain reinforcing effect, and is beneficial to improving the mechanical properties of the product.
3. According to the invention, the premix is coated by the polystyrene, so that the surface of the premix is coated with a layer of polystyrene, the dispersibility of the premix in the polystyrene is improved, and the mechanical strength and flame retardance of the product are ensured.
4. The invention adds foaming agent and perfluoro-hexanone into the mixture of polystyrene and coating premix, swells in supercritical carbon dioxide fluid, and foams after pressure relief. The boiling point of the perfluorinated hexanone is low, foaming can be promoted by cooperating with a foaming agent, and the bubble structure of the obtained product is optimized. The perfluorinated hexanone can also rapidly reduce the temperature of a fire scene, inhibit combustion, and a small amount of perfluorinated hexanone remained in the formed bubbles can synergistically play a role in flame retardance. After swelling in the supercritical carbon dioxide fluid, the pressure is relieved, the foaming is carried out, the full mixing of materials is promoted, the mechanical strength of the product is ensured, and meanwhile, the flame retardant effect of the product is further improved.
5. Because the premix is coated by the polystyrene, the coated premix is uniformly dispersed in the system in the polystyrene foaming process, so that the flame retardance can be better exerted, the flame retardance effect is improved, and the mechanical strength of the product is not influenced.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
All goods in the invention are purchased through market channels unless specified otherwise.
Example 1
The preparation method of the flame-retardant polystyrene composite material comprises the following specific steps:
(1) Dissolving sodium carboxymethylcellulose with water to prepare sodium carboxymethylcellulose aqueous solution with the mass concentration of 0.2%, dissolving cerium nitrate with water to prepare cerium nitrate aqueous solution with the mass concentration of 0.2%, dropwise adding the cerium nitrate aqueous solution into the sodium carboxymethylcellulose aqueous solution while stirring, continuously stirring for 10 minutes after the dropwise adding is finished, filtering to obtain solid, drying and crushing to obtain cerium carboxymethylcellulose; the mass ratio of the sodium carboxymethyl cellulose to the cerium nitrate is 1:1.5;
2g of polyvinyl alcohol (with the polymerization degree of 1800) is heated and dissolved in 50g of deionized water, then 5g of phytic acid and 1.6g of 4-dimethylaminopyridine are added, stirred and mixed uniformly, the mixture is kept at the temperature of 65 ℃ and stirred for 3 hours, naturally cooled to the room temperature, 70g of absolute ethyl alcohol is added, and the mixture is centrifugally taken, deposited, dried and crushed to obtain grafted polyvinyl alcohol; uniformly mixing the obtained grafted polyvinyl alcohol with 1.5g of carboxymethyl cellulose cerium to obtain a premix;
(2) 9g of polystyrene is dissolved by 200g of ethyl acetate to prepare a polystyrene solution, then 7.5g of premix is added into the polystyrene solution, the mixture is stirred and mixed uniformly to obtain a mixed solution, then 220g of n-hexane is dropwise added, polystyrene is separated out from the mixed solution and coated on the surface of the premix to form a coating layer, and the coating layer is centrifugally deposited and dried to obtain a coated premix;
(3) And then 8g of coating premix and 350g of polystyrene are uniformly stirred, then 2.5g of foaming agent (obtained by mixing n-pentane and isopentane according to the mass ratio of 3:6) and 2g of perfluorinated hexanone are added, uniformly stirred and mixed, placed in supercritical carbon dioxide fluid for swelling, relieved to atmospheric pressure at 8MPa/s, and foamed, so that the flame-retardant polystyrene composite material is obtained.
Wherein, in the step (3), the swelling process conditions are as follows: swelling for 2 hours at 40 ℃ under 25MPa of carbon dioxide; the foaming conditions are as follows: the temperature is 100 ℃ and the pressure is 0.02MPa.
Example 2
The preparation method of the flame-retardant polystyrene composite material comprises the following specific steps:
(1) Dissolving sodium carboxymethylcellulose with water to prepare sodium carboxymethylcellulose aqueous solution with the mass concentration of 0.3%, dissolving cerium nitrate with water to prepare cerium nitrate aqueous solution with the mass concentration of 0.3%, dropwise adding the cerium nitrate aqueous solution into the sodium carboxymethylcellulose aqueous solution while stirring, continuously stirring for 15 minutes after the dropwise adding is finished, filtering to obtain solid, drying and crushing to obtain cerium carboxymethylcellulose; the mass ratio of the sodium carboxymethyl cellulose to the cerium nitrate is 1:2;
heating and dissolving 3g of polyvinyl alcohol (with a polymerization degree of 2000) in 90g of deionized water, then adding 6g of phytic acid and 3.6g of 4-dimethylaminopyridine, stirring and uniformly mixing, preserving heat and stirring for 4 hours at 75 ℃, naturally cooling to room temperature, adding 120g of absolute ethyl alcohol, centrifuging to obtain precipitate, drying and crushing to obtain grafted polyvinyl alcohol; uniformly mixing the obtained grafted polyvinyl alcohol with 2.5g of carboxymethyl cellulose cerium to obtain a premix;
(2) Dissolving 12g of polystyrene with 250g of ethyl acetate to prepare a polystyrene solution, adding 11.5g of premix into the polystyrene solution, stirring and uniformly mixing to obtain a mixed solution, dropwise adding 260g of n-hexane, separating out the polystyrene from the mixed solution and coating the polystyrene on the surface of the premix to form a coating layer, centrifuging to obtain a precipitate, and drying to obtain a coated premix;
(3) And then uniformly stirring 10g of coating premix and 400g of polystyrene, then adding 3.5g of foaming agent (obtained by mixing n-pentane and isopentane according to the mass ratio of 4:7) and 3g of perfluorinated hexanone, uniformly stirring, placing in supercritical carbon dioxide fluid for swelling, releasing pressure to atmospheric pressure at 10MPa/s, and foaming to obtain the flame-retardant polystyrene composite material.
Wherein, in the step (3), the swelling process conditions are as follows: swelling for 3 hours at 50 ℃ under 35MPa of carbon dioxide; the foaming conditions are as follows: the temperature is 120 ℃ and the pressure is 0.03MPa.
Example 3
The preparation method of the flame-retardant polystyrene composite material comprises the following specific steps:
(1) Dissolving sodium carboxymethylcellulose with water to prepare sodium carboxymethylcellulose aqueous solution with the mass concentration of 0.25%, dissolving cerium nitrate with water to prepare cerium nitrate aqueous solution with the mass concentration of 0.25%, dropwise adding the cerium nitrate aqueous solution into the sodium carboxymethylcellulose aqueous solution while stirring, continuously stirring for 12 minutes after the dropwise adding is finished, filtering to obtain solid, drying and crushing to obtain cerium carboxymethylcellulose; the mass ratio of the sodium carboxymethyl cellulose to the cerium nitrate is 1:1.8;
2.5g of polyvinyl alcohol (polymerization degree 1900) is heated and dissolved in 70g of deionized water, then 5.5g of phytic acid and 2.8g of 4-dimethylaminopyridine are added, stirred and mixed uniformly, the mixture is kept at the temperature of 70 ℃ and stirred for 3.5 hours, naturally cooled to room temperature, 100g of absolute ethyl alcohol is added, and the mixture is centrifuged to obtain precipitate, dried and crushed to obtain grafted polyvinyl alcohol; uniformly mixing the obtained grafted polyvinyl alcohol with 2g of carboxymethyl cellulose cerium to obtain a premix;
(2) Dissolving 10g of polystyrene with 220g of ethyl acetate to prepare a polystyrene solution, adding 10g of premix into the polystyrene solution, stirring and uniformly mixing to obtain a mixed solution, then dropwise adding 240g of n-hexane, separating out the polystyrene from the mixed solution and coating the polystyrene on the surface of the premix to form a coating layer, centrifuging, taking out a precipitate, and drying to obtain a coated premix;
(3) And then taking 9g of coating premix and 380g of polystyrene, uniformly stirring, adding 3g of foaming agent (obtained by mixing n-pentane and isopentane according to a mass ratio of 3.5:6.5) and 2.5g of perfluorinated hexanone, uniformly stirring, placing in supercritical carbon dioxide fluid for swelling, releasing pressure to atmospheric pressure at 9MPa/s, and foaming to obtain the flame-retardant polystyrene composite material.
Wherein, in the step (3), the swelling process conditions are as follows: swelling for 2.5 hours at 45 ℃ under 30MPa of carbon dioxide; the foaming conditions are as follows: the temperature is 110 ℃ and the pressure is 0.03MPa.
Comparative example 1
A preparation method of polystyrene composite material comprises the following specific steps:
(1) 2g of polyvinyl alcohol (with the polymerization degree of 1800) is heated and dissolved in 50g of deionized water, then 5g of phytic acid and 1.6g of 4-dimethylaminopyridine are added, stirred and mixed uniformly, the mixture is kept at the temperature of 65 ℃ and stirred for 3 hours, naturally cooled to the room temperature, 70g of absolute ethyl alcohol is added, and the mixture is centrifugally taken, deposited, dried and crushed to obtain grafted polyvinyl alcohol;
(2) 9g of polystyrene is dissolved by 200g of ethyl acetate to prepare a polystyrene solution, then 7.5g of grafted polyvinyl alcohol is added into the polystyrene solution, the mixture is stirred and mixed uniformly to obtain a mixed solution, then 220g of normal hexane is dropwise added, polystyrene is separated out from the mixed solution and coated on the surface of the grafted polyvinyl alcohol to form a coating layer, and the coating layer is centrifugally deposited and dried to obtain a coating premix;
(3) And then 8g of coating premix and 350g of polystyrene are uniformly stirred, then 2.5g of foaming agent (obtained by mixing n-pentane and isopentane according to the mass ratio of 3:6) and 2g of perfluorinated hexanone are added, uniformly stirred and mixed, placed in supercritical carbon dioxide fluid for swelling, relieved to atmospheric pressure at 8MPa/s, and foamed, so that the polystyrene composite material is obtained.
Wherein, in the step (3), the swelling process conditions are as follows: swelling for 2 hours at 40 ℃ under 25MPa of carbon dioxide; the foaming conditions are as follows: the temperature is 100 ℃ and the pressure is 0.02MPa.
Comparative example 2
A preparation method of polystyrene composite material comprises the following specific steps:
(1) Dissolving sodium carboxymethylcellulose with water to prepare sodium carboxymethylcellulose aqueous solution with the mass concentration of 0.2%, dissolving cerium nitrate with water to prepare cerium nitrate aqueous solution with the mass concentration of 0.2%, dropwise adding the cerium nitrate aqueous solution into the sodium carboxymethylcellulose aqueous solution while stirring, continuously stirring for 10 minutes after the dropwise adding is finished, filtering to obtain solid, drying and crushing to obtain cerium carboxymethylcellulose; the mass ratio of the sodium carboxymethyl cellulose to the cerium nitrate is 1:1.5;
2g of polyvinyl alcohol (with the polymerization degree of 1800) is heated and dissolved in 50g of deionized water, then 5g of phytic acid and 1.6g of 4-dimethylaminopyridine are added, stirred and mixed uniformly, the mixture is kept at the temperature of 65 ℃ and stirred for 3 hours, naturally cooled to the room temperature, 70g of absolute ethyl alcohol is added, and the mixture is centrifugally taken, deposited, dried and crushed to obtain grafted polyvinyl alcohol; uniformly mixing the obtained grafted polyvinyl alcohol with 1.5g of carboxymethyl cellulose cerium to obtain a premix;
(2) 9g of polystyrene is dissolved by 200g of ethyl acetate to prepare a polystyrene solution, then 7.5g of premix is added into the polystyrene solution, the mixture is stirred and mixed uniformly to obtain a mixed solution, then 220g of n-hexane is dropwise added, polystyrene is separated out from the mixed solution and coated on the surface of the premix to form a coating layer, and the coating layer is centrifugally deposited and dried to obtain a coated premix;
(3) And then 8g of coating premix and 350g of polystyrene are uniformly stirred, then 2.5g of foaming agent (obtained by mixing n-pentane and isopentane according to the mass ratio of 3:6) and 2g of perfluorinated hexanone are added, uniformly stirred and mixed, and foamed, so that the polystyrene composite material is obtained.
Wherein, in the step (3), the foaming conditions are as follows: the temperature is 100 ℃ and the pressure is 0.02MPa.
The polystyrene composite materials obtained in examples 1 to 3 and comparative examples 1 and 2 were examined for properties by the following specific methods:
1. mechanical strength:
the test of compressive strength was carried out with reference to GB/T8813-2020 determination of compressive Properties of rigid foam,
2. flame retardancy:
flame retardant rating was tested with reference to UL94 standard.
Limiting oxygen index was tested with reference to astm d 2863.
Total heat release analysis: the test was carried out using a cone calorimeter produced by FTT in the united kingdom. The irradiation power was 35kW/m 2 Testing was performed using the ISO5660-1:2002 standard.
The test results are shown in Table 1.
TABLE 1 Performance test results
Compressive Strength (MPa) Flame retardant rating Limiting oxygen index (%) Total heat release (MJ/m) 2 )
Example 1 0.26 V-0 38.7 57
Example 2 0.26 V-0 38.9 60
Example 3 0.28 V-0 38.3 55
Comparative example 1 0.15 V-1 25.5 78
Comparative example 2 0.21 V-0 28.6 73
As can be seen from Table 1, the styrene composites obtained in examples 1 to 3 have good flame retardant rating, high limiting oxygen index, high temperature at maximum thermal weight loss rate, and small mass loss rate at the temperature, indicating good flame retardance; the high compressive strength indicates that the high-strength heat-insulating material has good mechanical properties and can be used for preparing building heat-insulating materials.
Comparative example 1 omits the carboxymethyl cellulose cerium, comparative example 2 omits the supercritical carbon dioxide fluid swelling treatment, and the mechanical strength and the flame retardance of the obtained product are obviously deteriorated, which means that the carboxymethyl cellulose cerium synergistically improves the flame retardance with other components and plays a role in reinforcing, and the supercritical carbon dioxide fluid swelling treatment is favorable for uniformly dispersing all the components, so that the flame retardance and the mechanical strength are improved.
The technical idea of the present invention is described by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must be implemented depending on the above embodiments. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of individual raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.

Claims (8)

1. The preparation method of the flame-retardant polystyrene composite material is characterized by comprising the following specific steps:
(1) 2 to 3 parts of polyvinyl alcohol and 5 to 6 parts of phytic acid are subjected to esterification reaction to obtain grafted polyvinyl alcohol, and then the grafted polyvinyl alcohol and 1.5 to 2.5 parts of carboxymethyl cellulose cerium are uniformly mixed to obtain a premix;
(2) Coating the premix by using polystyrene to obtain a coated premix;
(3) Taking 8-10 parts of coating premix and 350-400 parts of polystyrene, uniformly stirring, then adding 2.5-3.5 parts of foaming agent and 2-3 parts of perfluorinated hexanone, uniformly stirring, placing in supercritical carbon dioxide fluid for swelling, releasing pressure and foaming to obtain the flame-retardant polystyrene composite material;
the specific method of the step (2) comprises the following steps of: 9-12 parts of polystyrene is dissolved by using 200-250 parts of ethyl acetate to prepare a polystyrene solution, then 7.5-11.5 parts of premix is added into the polystyrene solution, the mixture is stirred and mixed uniformly to obtain a mixed solution, then 220-260 parts of n-hexane is dropwise added, polystyrene is separated out from the mixed solution and coated on the surface of the premix to form a coating layer, and the coating layer is obtained by centrifuging, taking a precipitate and drying the precipitate to obtain the coated premix;
in the step (3), the swelling process conditions are as follows: swelling for 2-3 hours at 40-50 ℃ under 25-35 MPa of carbon dioxide.
2. The process according to claim 1, wherein in the step (1), the grafted polyvinyl alcohol is prepared by the following steps: heating polyvinyl alcohol to dissolve in deionized water, adding phytic acid and 4-dimethylaminopyridine, stirring uniformly, preserving heat at 65-75 ℃ for 3-4 hours, naturally cooling to room temperature, adding absolute ethyl alcohol, centrifuging, taking precipitate, drying, and crushing to obtain the grafted polyvinyl alcohol.
3. The process according to claim 1, wherein the polymerization degree of the polyvinyl alcohol in the step (1) is 1800 to 2000.
4. The preparation method according to claim 1, wherein in the step (1), the preparation method of the carboxymethyl cellulose cerium is as follows: dissolving sodium carboxymethylcellulose with water to prepare sodium carboxymethylcellulose aqueous solution with the mass concentration of 0.2-0.3%, dissolving cerium nitrate with water to prepare cerium nitrate aqueous solution with the mass concentration of 0.2-0.3%, dropwise adding the cerium nitrate aqueous solution into the sodium carboxymethylcellulose aqueous solution while stirring, continuously stirring for 10-15 minutes after the dropwise adding, filtering to obtain solid, drying and crushing to obtain the sodium carboxymethylcellulose aqueous solution.
5. The preparation method of claim 1, wherein in the step (3), the foaming agent is n-pentane and isopentane according to a mass ratio of 3-4: 6 to 7.
6. The method according to claim 1, wherein in the step (3), the foaming conditions are: the temperature is 100-120 ℃ and the pressure is 0.02-0.03 MPa.
7. A flame retardant polystyrene composite obtained by the method according to any one of claims 1 to 6.
8. The use of the flame retardant polystyrene composite of claim 7 in the preparation of a building insulation material.
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