CN116376565B - Flame retardant, preparation method and application thereof - Google Patents

Flame retardant, preparation method and application thereof Download PDF

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Publication number
CN116376565B
CN116376565B CN202310619436.8A CN202310619436A CN116376565B CN 116376565 B CN116376565 B CN 116376565B CN 202310619436 A CN202310619436 A CN 202310619436A CN 116376565 B CN116376565 B CN 116376565B
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chitosan
flame retardant
phosphorylated chitosan
phosphorylated
pet
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CN116376565A (en
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杨伟鑫
吴思瑶
朱逸枫
周玉波
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Hefei Changyang New Material Technology Co ltd
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Hefei Changyang New Material Technology Co ltd
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    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00—Fireproofing materials
    • C09K21/14—Macromolecular materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/007—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process employing compositions comprising nanoparticles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
    • C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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    • C09K21/00—Fireproofing materials
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
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    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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    • C08K2003/0806—Silver
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Abstract

The application discloses a flame retardant, a preparation method and application thereof, and belongs to the technical field of flame retardants. The flame retardant comprises phosphorylated chitosan and nano silver particles combined with amino positions of the phosphorylated chitosan; the mass ratio of the phosphorylated chitosan to the nano silver particles is 100:0.1-2. The flame retardant has better flame retardance and antibacterial property. Products such as PET films containing the flame retardant can also have better flame retardance and antibacterial property. The preparation methods of the flame retardant and the PET film are simple, easy to operate and suitable for industrial production.

Description

Flame retardant, preparation method and application thereof
Technical Field
The application relates to the technical field of flame retardants, in particular to a flame retardant and a preparation method and application thereof.
Background
Chitosan is commonly used as an antibacterial treatment agent and shows antibacterial and bactericidal activity in vitro, but the antibacterial and bactericidal effects brought by chitosan are limited, and meanwhile, the addition of chitosan cannot improve the flame retardant property of related application materials.
In view of this, the present application has been made.
Disclosure of Invention
It is an object of the present application to provide a flame retardant having superior flame retardancy and antibacterial properties. The second purpose of the application is to provide a preparation method of the flame retardant.
The application also provides an application of the flame retardant.
The fourth object of the present application is to provide a PET film containing the above flame retardant.
The fifth object of the present application is to provide a method for producing the PET film.
The application can be realized as follows:
in a first aspect, the present application provides a flame retardant; the flame retardant comprises phosphorylated chitosan and nano silver particles combined with amino positions of the phosphorylated chitosan;
the mass ratio of the phosphorylated chitosan to the nano silver particles is 100:0.1-2.
In a second aspect, the present application provides a method for preparing a flame retardant according to the previous embodiment, comprising the steps of: the nano silver particles are combined with amino positions of the phosphorylated chitosan.
In an alternative embodiment, the solution of phosphorylated chitosan is mixed and reacted with an aqueous solution of silver nitrate under ultrasonic conditions, followed by centrifugal washing and drying.
In an alternative embodiment, the preparation of the flame retardant includes at least one of the following features:
characteristic one: the solution of the phosphorylated chitosan is prepared by dissolving phosphorylated chitosan in acetic acid solution; wherein the concentration of the acetic acid solution is 0.1-1mol/L;
and the second characteristic is: 5-15g of phosphorylated chitosan is correspondingly dissolved in each liter of acetic acid solution;
and (3) the following characteristics: the concentration of the aqueous solution of silver nitrate is 0.5-2g/L.
In alternative embodiments, the reaction conditions include at least one of the following features:
characteristic one: the ultrasonic power is 100-300W;
and the second characteristic is: the reaction temperature is 70-100 ℃;
and (3) the following characteristics: the reaction time is 12-48h.
In an alternative embodiment, the phosphorylated chitosan is obtained by:
dissolving chitosan, urea and orthophosphoric acid in N, N-dimethylformamide, stirring under protective atmosphere for reaction, cooling, separating solid from liquid, washing the separated solid phase, and drying.
In an alternative embodiment, the preparation of phosphorylated chitosan includes at least one of the following features:
characteristic one: the mass ratio of the chitosan, the urea and the orthophosphoric acid is 1-4:10:2-3;
and the second characteristic is: the protective atmosphere is nitrogen atmosphere;
and (3) the following characteristics: the reaction temperature is 140-160 ℃;
and four characteristics: the reaction time is 0.5-3h.
In a third aspect, the present application provides the use of a flame retardant according to the previous embodiments in a wood material or a polymeric material. In a fourth aspect, the present application provides a PET sheet comprising a PET material and a flame retardant according to the foregoing embodiments.
In an alternative embodiment, the PET film has at least one of the following characteristics:
characteristic one: the mass ratio of the flame retardant to the PET material is 1-8:100;
and the second characteristic is: the thickness of the PET film is 50-250 μm.
In a fifth aspect, the present application provides a method for preparing a PET film according to the foregoing embodiment, comprising the steps of: blending and casting the flame retardant and the PET material;
the casting temperature is 260-280 ℃.
The beneficial effects of the application include:
the flame retardant provided by the application comprises phosphorylated chitosan and nano silver particles combined with amino positions of the phosphorylated chitosan, and has better flame retardance and antibacterial property. The mass ratio of the phosphorylated chitosan to the nano silver particles is controlled to be 100:0.1-2, and the coordination effect of the phosphorylated chitosan and the nano silver particles can be simultaneously and maximally exerted.
By adding the flame retardant into the PET film or other materials, compared with the method that the phosphorylated chitosan and the nano silver are directly added into the PET material or other materials, the antibacterial effect of the PET film or the corresponding materials can be improved, and the protonated amino released by the chitosan and the silver released by the silver nano ions act together with negative potential on the surface of bacterial cell membranes, so that efficient bacteriostasis is achieved. The corresponding PET film and other materials can have good antibacterial property and flame retardance.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The flame retardant provided by the application, and a preparation method and application thereof are specifically described below.
The present application proposes a flame retardant (hereinafter may also be referred to as "phosphorylated chitosan-based nanosilver") comprising phosphorylated chitosan and nanosilver particles bound to amino positions of the phosphorylated chitosan.
The mass ratio of the phosphorylated chitosan to the nano silver particles is 100:0.1-2, such as 100:0.1, 100:0.2, 100:0.5, 100:1, 100:1.2, 100:1.5, 100:1.8 or 100:2, etc., and any other value in the range of 100:0.1-2 can be used.
If the mass ratio of the phosphorylated chitosan to the nano silver particles is lower than 100:0.1 (such as 100:0.05), the method is unfavorable for simultaneously obtaining better flame retardance and antibacterial property; if the mass ratio of phosphorylated chitosan to nano-silver particles is higher than 100:2 (e.g., 100:5), chitosan may not provide enough amino sites to reduce silver ions to elemental silver.
In the present application, the preparation of the flame retardant may include, for example: the nano silver particles are combined with amino positions of the phosphorylated chitosan.
For reference, the solution of phosphorylated chitosan and the aqueous solution of silver nitrate may be mixed and reacted under ultrasonic conditions, followed by centrifugal washing and drying to obtain the flame retardant.
In the reaction process, silver ions contained in the silver nitrate react with amino groups of chitosan in the phosphorylated chitosan, and are reduced into silver simple substances by ammonia, namely silver nano particles are generated in situ.
Wherein, the solution of the phosphorylated chitosan is obtained by dissolving the phosphorylated chitosan in acetic acid solution. The concentration of the acetic acid solution may be 0.1 to 1mol/L, such as 0.1mol/L, 0.2mol/L, 0.5mol/L, 0.8mol/L, 1mol/L, etc., and may be any other value within the range of 0.1 to 1 mol/L.
5-15g of phosphorylated chitosan is dissolved in each liter of acetic acid solution. For example, the amount of the phosphorylated chitosan dissolved per liter of the acetic acid solution may be 5g, 8g, 10g, 12g, 15g, or the like, or may be any other value within the range of 5 to 15 g.
The acetic acid solution with specific concentration is used for dissolving the phosphorylated chitosan, so that the pH value is easy to control to be about 2-3, on one hand, the phosphorylated chitosan can be fully dissolved, and on the other hand, the reaction of amino groups in the chitosan and silver can be facilitated.
The concentration of the aqueous solution of silver nitrate is 0.5-2g/L, such as 0.5g/L, 0.8g/L, 1g/L, 1.2g/L, 1.5g/L, 1.8g/L, or 2g/L, etc., and may be any other value within the range of 0.5-2g/L.
If the concentration of the aqueous solution of silver nitrate is lower than 0.5g/L, the amount of silver ions is smaller, which is not beneficial to improving the antibacterial effect of the PET film by matching with phosphorylated chitosan; if the concentration of the aqueous solution of silver nitrate is higher than 2g/L, the silver content is higher, so that the silver particles generated in situ are easy to be larger in size and smaller in specific surface area, and the action and effect of the silver particles are reduced.
In the present application, the ultrasonic power used for the reaction of the solution of phosphorylated chitosan and the aqueous solution of silver nitrate may be 100 to 300W, for example, 100W, 150W, 200W, 250W, 300W, or the like, or any other value within the range of 100 to 300W.
By carrying out ultrasound with the ultrasonic power, silver particles with proper sizes can be generated in situ. If the ultrasonic power is lower than 100W, larger silver particles are obtained; if the ultrasonic power is higher than 300W, silver particles having a smaller size are obtained.
The reaction temperature may be 70-100deg.C, such as 70deg.C, 75deg.C, 80deg.C, 85deg.C, 90deg.C, 95deg.C or 100deg.C, etc., or may be any other value within 70-100deg.C.
The reaction time may be 12-48h, such as 12h, 18h, 24h, 30h, 36h, 42h or 48h, or any other value within the range of 12-48h.
If the reaction temperature is lower than 70 ℃ or the reaction time is shorter than 12 hours, the reaction is insufficient or even impossible to react easily; if the reaction temperature is higher than 100 ℃, the reaction is more severe, and the reaction time is not easy to control; if the reaction time is longer than 48 hours, the cost and the energy consumption are greatly increased.
For reference, the above-mentioned phosphorylated chitosan can be obtained by the following steps:
dissolving chitosan, urea and orthophosphoric acid in N, N-Dimethylformamide (DMF), stirring under protective atmosphere for reaction, cooling, separating solid from liquid, washing the separated solid phase, and drying.
The orthophosphoric acid can carry out esterification reaction with hydroxyl on the surface of chitosan, and simultaneously adjust the pH value of the reaction and provide flame retardant elements; urea is mainly used for promoting the esterification reaction of orthophosphoric acid and chitosan hydroxyl; DMF is mainly used to dissolve chitosan. The phosphate radical and hydroxyl contained in chitosan are subjected to substitution reaction to obtain the phosphorylated chitosan.
Wherein, the mass ratio of chitosan, urea and orthophosphoric acid can be 1-4:10:2-3, such as 1:10:2, 1:10:2.5, 1:10:3, 2:10:2, 2:10:2.5, 2:10:3, 3:10:2, 3:10:2.5, 3:10:3, 4:10:2, 4:10:2.5, or 4:10:3, etc., may also be 1-4:10:2-3, and any other value in the range of from 2 to 3.
The protective atmosphere may be a nitrogen atmosphere, an argon atmosphere, a helium atmosphere, or the like, for example.
The reaction temperature of chitosan, urea, orthophosphoric acid and N, N-dimethylformamide can be 140-160 ℃, such as 140 ℃, 145 ℃,150 ℃, 155 ℃ or 160 ℃, and the like, and can be any other value within the range of 140-160 ℃; the corresponding reaction time may be 0.5-3h, such as 0.5h, 1h, 1.5h, 2h, 2.5h or 3h, etc., or any other value within the range of 0.5-3h.
On the premise of bearing, the silver nano particles are prepared by modifying chitosan with phosphoric acid and then reducing in situ, the preparation process is relatively simple, obvious price advantage is achieved, and the size control of the silver particles can be effectively realized by controlling ultrasonic power and reaction time. The phosphorous source is introduced into the phosphorylated chitosan while the nano silver particles improve the antibacterial property of the chitosan, so that the flame retardance of the chitosan can be effectively improved.
The flame retardant can be used in high polymer materials and also can be used in non-high polymer materials (such as wood materials).
As an example, a flame retardant is used for a PET film containing the above flame retardant. By adding the flame retardant into the PET film, the PET film can have good antibacterial property and flame retardance.
In the application, the main component of the PET film is PET material, and the mass ratio of the flame retardant to the PET material in the PET film can be 1-8:100, such as 1:100, 2:100, 3:100, 4:100, 5:100, 6:100, 7:100 or 8:100, and the like, and can also be any other value within the range of 1-8:100.
If the mass ratio of the flame retardant to the PET material is lower than 1:100 (such as 0.5:100), good antibacterial and flame-retardant effects are not good; if the mass ratio of the flame retardant to the PET material is higher than 8:100 (such as 10:100), the improvement of flame retardance and antibacterial property is small, the retention of the mechanical property of the polyester film is not facilitated, and the cost is greatly increased.
The thickness of the PET film may be 50 to 250. Mu.m, such as 50 μm, 100 μm, 150 μm, 200 μm or 250. Mu.m, etc., or may be any other value within the range of 50 to 250. Mu.m. In addition, the PET film may be provided to other thickness as needed.
Correspondingly, the application also provides a preparation method of the PET film, which comprises the following steps: the flame retardant is blended with PET material for casting.
By adopting a blending casting mode, the flame retardant has good dispersibility and uniformity in the PET matrix, and the action effect is improved.
As a reference, the casting temperature may be 260 to 280℃such as 260℃C, 265℃C, 270℃C, 275℃C or 280℃C, etc., or may be any other value within the range of 260 to 280 ℃.
If the casting temperature is lower than 260 ℃, the PET extrusion is not favored; if the casting temperature exceeds 280 ℃, the chitosan main chain may be broken.
The nano silver-phosphorylated chitosan-PET composite film provided by the application not only can obviously improve the antibacterial property and flame retardance of PET, but also can avoid the agglomeration of nano silver and obviously reduce the mechanical property loss of the composite film compared with the case of directly and independently adding nano silver particles. In addition, compared with the mode that the phosphorylated chitosan and the nano silver are directly added into the PET material, the phosphorylated chitosan-based nano silver can improve the antibacterial effect of the composite membrane and act with the negative potential on the surface of the bacterial cell membrane, so that the efficient antibacterial effect is achieved.
The features and capabilities of the present application are described in further detail below in connection with the examples.
Example 1
The embodiment provides a PET film, which is prepared by the following method:
s1: 10g of chitosan powder, 100g of urea and 20g of orthophosphoric acid are weighed and added into 200mL of DMF, and the mixture is stirred and reacted for 1 hour at 150 ℃ under the protection of nitrogen gas. After cooling, the product is filtered, the sediment is completely washed by distilled water, and the sediment is dried by a blast drying oven at 60 ℃ for 24 hours, thus obtaining the phosphorylated chitosan.
S2: 1g of the obtained phosphorylated chitosan is taken and added into 100ml of 0.5mol/L acetic acid solution, and the mixture is stirred for about 10 hours at 70 ℃ until the solution is transparent, thus obtaining the phosphorylated chitosan solution.
S3: under the conditions of ultrasonic power 300W and 90 ℃, 4ml of 1g/L silver nitrate aqueous solution is added into the phosphorylated chitosan solution to react for 24 hours, and a small amount of sodium hydroxide solution is added to adjust the pH to be neutral. The obtained neutral solution is dried for 24 hours in a baking oven at 80 ℃, then is washed by distilled water, and is dried for 24 hours in the baking oven at 80 ℃ to obtain the nano silver particles wrapped by the phosphorylated chitosan, wherein the nano silver particles account for about 0.25 weight percent of the phosphorylated chitosan.
S4: 12g of phosphorylated chitosan-based nano silver particles and 288g of PET chips were mixed in a high-speed mixer for 1 minute (rotation speed of 1500rpm per minute), and the mixture was fed into a casting machine at a casting temperature of 260℃to prepare a PET film having a thickness of 150. Mu.m, the PET film containing 4wt% of flame retardant.
Example 2
This embodiment differs from embodiment 1 in that: the amount of flame retardant contained in the PET film was 1wt% of the PET chips.
Example 3
This embodiment differs from embodiment 1 in that: the amount of flame retardant contained in the PET film was 6% by weight of the PET chips.
Example 4
This embodiment differs from embodiment 1 in that: the amount of flame retardant contained in the PET film was 8% by weight of the PET chips.
Example 5
This embodiment differs from embodiment 1 in that: the mass ratio of the phosphorylated chitosan to the nano silver particles is 100:0.1.
Example 6
This embodiment differs from embodiment 1 in that: the mass ratio of the phosphorylated chitosan to the nano silver particles is 100:2.
Example 7
This embodiment differs from embodiment 1 in that: the ultrasonic power was 100W.
Example 8
This embodiment differs from embodiment 1 in that: the reaction temperature was 70℃and the reaction time was 48h.
Example 9
This embodiment differs from embodiment 1 in that: the reaction temperature is 100 ℃ and the reaction time is 12 hours.
Comparative example 1
The difference between this comparative example and example 1 is that: a PET film was prepared from 300g of PET chips, that is, only PET chips.
Comparative example 2
The difference between this comparative example and example 1 is that: a PET film was prepared by taking 12g of phosphorylated chitosan and 288g of PET chips. I.e. the PET film does not contain nano silver particles.
Comparative example 3
The difference between this comparative example and example 1 is that: a PET film was prepared by taking 11.97g of phosphorylated chitosan, 0.03g of nano silver particles and 288g of PET slices. That is, the phosphorylated chitosan and the nano silver particles are independently present and simply mixed, and the nano silver particles are not generated in situ at the amino position of the phosphorylated chitosan.
Comparative example 4
The difference between this comparative example and example 1 is that: a PET film was prepared by taking 12g of nano silver particles and 288g of PET chips. Namely, the PET film does not contain phosphorylated chitosan.
Comparative example 5
The difference between this comparative example and example 1 is that: the amount of flame retardant contained in the PET film was 0.5wt% of the PET chips.
Comparative example 6
The difference between this comparative example and example 1 is that: the mass ratio of the phosphorylated chitosan to the nano silver particles is 100:0.05.
Comparative example 7
The difference between this comparative example and example 1 is that: the mass ratio of the phosphorylated chitosan to the nano silver particles is 100:5.
Comparative example 8
The difference between this comparative example and example 1 is that: the ultrasonic power was 50W.
Comparative example 9
The difference between this comparative example and example 1 is that: the ultrasonic power was 500W.
Test examples
The PET films prepared in examples 1 to 9 and comparative examples 1 to 9 were subjected to limiting oxygen index test and E.coli antibacterial property test, respectively.
Among them, limiting oxygen index test was performed according to GB/T2406.2-2009.
The E.coli antibacterial test was performed according to the E.coli test method mentioned in GB/T20944.3-2008 shaking method. Specifically, the PET film was cut into 9mm diameter disks, respectivelyThen placed in a suspension (2.1X10) coated with E.coli 5 CFU/mL). The dishes were incubated in a biochemical incubator at constant temperature (37 ℃). After 24 hours, the size of the antibacterial ring was measured.
The test results are shown in Table 1.
Table 1 test results
As can be seen from table 1: the PET film provided by the embodiment of the application has better flame retardance and antibacterial property.
In conclusion, the flame retardant provided by the application has better flame retardant property and antibacterial property, and the corresponding PET film and other materials can also have better antibacterial property and flame retardance.
The above is only a preferred embodiment of the present application, and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (2)

1. The PET film is characterized by comprising PET materials and flame retardants; the PET film has the following characteristics: the mass ratio of the flame retardant to the PET material is 1-8:100; the thickness of the PET film is 50-250 mu m;
the preparation of the flame retardant comprises the following steps: mixing and reacting the solution of the phosphorylated chitosan with the aqueous solution of the silver nitrate under the ultrasonic condition, and then centrifugally washing and drying to obtain the flame retardant for combining the nano silver particles at the amino position of the phosphorylated chitosan; the mass ratio of the phosphorylated chitosan to the nano silver particles is 100:0.1-2;
the preparation of the flame retardant comprises the following characteristics: the solution of the phosphorylated chitosan is prepared by dissolving phosphorylated chitosan in acetic acid solution; wherein the concentration of the acetic acid solution is 0.1-1mol/L; 5-15g of phosphorylated chitosan is correspondingly dissolved in each liter of acetic acid solution; the concentration of the aqueous solution of silver nitrate is 0.5-2g/L;
the reaction conditions include the following features: the ultrasonic power is 100-300W; the reaction temperature is 70-100 ℃; the reaction time is 12-48h;
the phosphorylated chitosan is obtained through the following steps: dissolving chitosan, urea and orthophosphoric acid in N, N-dimethylformamide, stirring for reaction under protective atmosphere, cooling, separating solid from liquid, washing the separated solid phase, and drying;
the preparation of the phosphorylated chitosan comprises the following characteristics: the mass ratio of the chitosan, the urea and the orthophosphoric acid is 1-4:10:2-3; the protective atmosphere is nitrogen atmosphere; the reaction temperature is 140-160 ℃; the reaction time is 0.5-3h.
2. A method for producing the PET film according to claim 1, comprising the steps of: blending and casting the flame retardant and PET material;
the casting temperature is 260-280 ℃.
CN202310619436.8A 2023-05-30 2023-05-30 Flame retardant, preparation method and application thereof Active CN116376565B (en)

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CN110357987A (en) * 2019-08-14 2019-10-22 东南大学 A kind of expansion type flame retardant and preparation method thereof
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