CN112830862B - Novel fluorine-containing flame retardant, synthetic method and application thereof in nylon 6 modification - Google Patents
Novel fluorine-containing flame retardant, synthetic method and application thereof in nylon 6 modification Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
- C07C17/12—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the ring of aromatic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/395—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification of at least one compound
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
Abstract
The invention provides a synthesis method of a novel fluorine-containing flame retardant, which comprises the following steps: and mixing the fluorine gas with the inert gas to obtain the fluorine gas mixed gas. Adding 1, 2-di (phenyl) -tetrafluoroethane into the microreactor, slowly introducing fluorine gas mixed gas, and synthesizing a fluorine-containing flame retardant crude product under the catalysis of anhydrous aluminum chloride. Diluting the crude product of the fluorine-containing flame retardant by water, and then carrying out neutralization, water washing, hot air treatment and high-temperature treatment to obtain the fluorine-containing flame retardant. The synthesis process of the invention has zero emission in the whole process and is environment-friendly and reliable. The invention also provides a fluorine-containing flame retardant, which mainly comprises 1, 2-bis (4-fluorophenyl) -1, 2-tetrafluoroethane, wherein the molecular weight of the fluorine-containing flame retardant is 290.20, the melting point of the fluorine-containing flame retardant is 97 ℃, the boiling point of the fluorine-containing flame retardant is 255-260 ℃, and the density of the fluorine-containing flame retardant is 1.35g/cm 3 . The fluorine-containing flame retardant is safe and reliable. The invention also relates to application of the fluorine-containing flame retardant in nylon 6 modification, and the modified nylon 6 has good flame retardant effect. The fire-retardant rating can reach V-0 level.
Description
Technical Field
The invention relates to the technical field of fluorine-containing flame retardants, and particularly relates to a novel fluorine-containing flame retardant, a synthesis method and application thereof in nylon 6 modification.
Background
Nylon is commonly known as Polyamide (PA), is a high molecular compound containing amide groups (-NHCO-) on the main chain, is also an important engineering resin, and has wide application in daily life and material industry. Among them, nylon 6 (PA 6) is the most widely used and the most productive one. The structure of the nylon enables the PA6 to have high mechanical strength, and meanwhile, the nylon has high melting point, good solvent resistance, excellent heat resistance and amide groups, so that the nylon has certain flame retardance. The test results according to ASTM D635 show that PA6 is of the self-extinguishing type. However, as a widely used material, the environment for using PA6 is much more severe, such as high humidity, high temperature, high voltage, etc., and therefore, the flame retardant property of nylon becomes a crucial factor in many cases. In order to achieve higher flame retardant performance, there is no way to satisfy the requirement of a molecular structure alone, and therefore, it is necessary to further improve the flame retardant performance of PA6 by modification.
Among the most commonly used flame retardants in current flame retardant modifications are red phosphorus and halogen based flame retardants.
Red phosphorus has the advantage of a high available phosphorus content, which releases volatile phosphorus compounds when decomposed by heat. Mass spectrometry analysis shows that the red phosphorus has PO & free radical when heated, and the PO & captures H & lt + & gt, namely PO & lt + & gt & lt HPO, so that the concentration of hydrogen atoms in the flame is greatly reduced. This also indicates that much phosphoric acid is produced upon combustion. Although the nylon can keep better self mechanical property while the red phosphorus is flame-retardant, the red phosphorus is red in color, is easy to cause color pollution, is flammable and difficult to store, and more importantly, the red phosphorus can react with water to generate high-toxicity phosphine, so that the danger coefficient is higher.
The mechanism of action of the halogen flame retardant is to retard or prevent the combustion of nylon 6 (PA 6) through the gas phase. Halogen flame retardants can generate HX (hydrogen halide) and the like at high temperatures. On one hand, the flame retardant is a free radical terminator which can reduce or eliminate active free radicals, thereby slowing or stopping the chain reaction in gas phase combustion and realizing the flame retardant effect. On the other hand, the generated hydrogen halide belongs to a flame retardant gas with higher density, and a large amount of hydrogen halide can not only dilute the oxygen concentration, but also form a gas protection layer between the polymer and the gas phase, thereby blocking the path of combustion.
Currently, the halogen flame retardants on the market are mainly represented by polybrominated diphenyl ethers (PBDE) and polybrominated biphenyls (PBB). The brominated flame retardant has high flame retardant efficiency, small using amount and little influence on the performance of the flame retardant material. However, PBDE is a persistent toxic pollutant, PBB is also a harmful substance, and especially in the preparation process, a large amount of bromide ions are discharged due to the problem of product yield, so that the PBDE is banned from being used in many countries. Therefore, a safer and more reliable flame retardant needs to be developed to minimize the loss and environmental pollution during the production and use process, so as to achieve a more environment-friendly process control and have a better application prospect.
Disclosure of Invention
The invention aims to provide a novel fluorine-containing flame retardant which is safe and reliable and has a good application prospect.
The invention also aims to provide a synthetic method of the novel fluorine-containing flame retardant, which has the advantages of low loss, zero emission in the whole synthetic process, environmental protection and reliability.
The third purpose of the invention is to provide the application of the novel fluorine-containing flame retardant in the modification of nylon 6.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a synthesis method of a novel fluorine-containing flame retardant, which comprises the following steps:
s1, mixing and diluting fluorine gas and inert gas to obtain fluorine gas mixed gas;
s2, adding 1, 2-bis (phenyl) -tetrafluoroethane and anhydrous aluminum chloride into the microreactor, then slowly introducing the fluorine gas mixed gas, and reacting under the catalysis of the anhydrous aluminum chloride to synthesize a fluorine-containing flame retardant crude product;
and S3, diluting the crude product of the fluorine-containing flame retardant by using water, adding an alkali solution for neutralization, and then performing water washing, hot air treatment and high-temperature treatment to obtain the fluorine-containing flame retardant.
The invention provides a novel fluorine-containing flame retardant which is synthesized according to the synthesis method, and the main component of the fluorine-containing flame retardant is 1, 2-bis (4-fluorophenyl)1, 2-tetrafluoroethane having a molecular weight of 290.20, a melting point of 97 ℃, a boiling point of 255 to 260 ℃ and a density of 1.35g/cm 3 。
The invention also provides application of the novel fluorine-containing flame retardant in nylon 6 modification.
The novel fluorine-containing flame retardant, the synthesis method and the application thereof in nylon 6 modification have the following beneficial effects:
the invention adopts a fluorine synthesis method, and directly reacts 1, 2-di (phenyl) -tetrafluoroethane and fluorine gas under the catalysis of anhydrous aluminum chloride to generate the fluorine-containing flame retardant with 1, 2-di (4-fluorophenyl) -1, 2-tetrafluoroethane as a main component. The synthetic method has the advantages of low raw material loss, zero emission in the whole synthetic process, environmental protection and reliability.
In addition, HF generated after the C-F bond is broken can capture free radicals, so that the fluorine-containing flame retardant disclosed by the invention has a good flame retardant effect. Because the bond energy of the C-F bond is strong, the C-F bond is not broken at ordinary temperature. Therefore, although HF is harmful to human body, the fluorine-containing flame retardant does not cause harm to human body at ordinary temperature, and is very safe. Only at extremely high temperature, in order to extinguish the fire in time and ensure the safety of life and property, the C-F bond is broken to play a role of flame retardance, thereby reducing the loss to the minimum. Therefore, the fluorine-containing flame retardant prepared by the synthesis method is safe and reliable, and has a good application prospect. The fluorine-containing flame retardant of the invention can react with Sb 2 O 3 The flame-retardant master batch is prepared by mixing, and the flame-retardant master batch can be melt-mixed with nylon 6 (PA 6) for modifying the nylon 6. The modified nylon 6 is tested by UL 94V-level fire-retardant rating, and the fire-retardant rating can reach V-0 level.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of the novel fluorine-containing flame retardant, the synthesis method and the application thereof in nylon 6 modification.
The synthesis method of the novel fluorine-containing flame retardant provided by the embodiment of the invention comprises the following steps:
s1, mixing and diluting fluorine gas and inert gas to obtain fluorine gas mixed gas. The fluorine gas and the inert gas used in the present invention are commercially available, and for example, the fluorine gas is available from Hiemann Niflon materials Co.Ltd.
Further, in a preferred embodiment of the present invention, the concentration of the fluorine gas in the fluorine gas mixed gas is 15 to 25%.
And S2, adding 1, 2-bis (phenyl) -tetrafluoroethane and anhydrous aluminum chloride into the microreactor, then slowly introducing the fluorine gas mixed gas, and reacting under the catalysis of the anhydrous aluminum chloride to synthesize the fluorine-containing flame retardant crude product. Anhydrous aluminum chloride is used as a catalyst commonly used in organic synthesis and petroleum industry, and can be used for catalyzing 1, 2-bis (4-fluorophenyl) -1, 2-tetrafluoroethane to be synthesized by reacting 1, 2-bis (phenyl) -tetrafluoroethane with fluorine gas. Both the 1, 2-di (phenyl) -tetrafluoroethane and the anhydrous aluminum chloride used in the present invention are commercially available, for example, 1, 2-di (phenyl) -tetrafluoroethane is commercially available from Chengdu chemical Co., ltd. And the anhydrous aluminum chloride is commercially available from Shandong Zibono Industrial Co., ltd.). The reaction process of the invention is as follows:
further, in a preferred embodiment of the invention, the reaction temperature in the microreactor is below 40 ℃. Preferably, the temperature in the microreactor is 15-25 ℃. The invention adopts the reaction temperature of 15-25 ℃, can ensure the reaction of 1, 2-di (phenyl) -tetrafluoroethane and fluorine gas, and is convenient for subsequent production and application. The molar ratio of the fluorine gas to the 1, 2-bis (phenyl) -tetrafluoroethane is 0.8 to 1:1. preferably, the molar ratio of fluorine gas to 1, 2-bis (phenyl) -tetrafluoroethane is 1. The aeration time is 0.8 to 1.2 hours.
And S3, diluting the crude product of the fluorine-containing flame retardant by using water, adding an alkali solution for neutralization, and then performing water washing, hot air treatment and high-temperature treatment to obtain the fluorine-containing flame retardant.
Further, in a preferred embodiment of the present invention, the mass ratio of the water to the crude fluorine-containing flame retardant during the dilution process is 30.
Further, in a preferred embodiment of the present invention, the alkali solution is selected from a NaOH aqueous solution with a mass fraction of 0.5-1.5% or Na with a molar concentration of 0.5-1.5 mol/l 2 CO 3 An aqueous solution. The pH of the neutralized solution is 6.5 to 7.5. Acid impurities in the crude product of the fluorine-containing flame retardant can be removed through the neutralization of the alkali solution, so that a refined product of the fluorine-containing flame retardant can be obtained later. NaOH and Na used in the present invention 2 CO 3 Are commercially available, e.g. NaOH and Na 2 CO 3 All available from Cangzhou Hongjia chemical products, inc.
Further, in the preferred embodiment of the present invention, the hot air treatment temperature is 150-180 ℃ and the hot air treatment time is 2.5-3.5 h. The high-temperature treatment temperature is 170-190 ℃, and the high-temperature treatment time is 23-25 h.
The invention adopts a fluorine synthesis method, and directly reacts 1, 2-di (phenyl) -tetrafluoroethane and fluorine gas under the catalysis of anhydrous aluminum chloride to generate the fluorine-containing flame retardant with 1, 2-di (4-fluorophenyl) -1, 2-tetrafluoroethane as a main component. The synthetic method has the advantages of low raw material loss, zero emission in the whole synthetic process, environmental protection and reliability.
The invention also provides a novel fluorine-containing flame retardant synthesized by the synthesis method, wherein the main component of the fluorine-containing flame retardant is 1, 2-bis (4-fluorophenyl) -1, 2-tetrafluoroethane. The molecular weight is 290.20, the melting point is 97 ℃, the boiling point is 255-260 ℃, and the density is 1.35g/cm 3 . The fluorine-containing flame retardant also contains a small amount of 1, 2-bis (phenyl) -tetrafluoroethane.
The fluorine-containing flame retardant synthesized by the invention is safe and reliable, and has a good application prospect. HF generated after the C-F bond is broken can capture free radicals, so that the fluorine-containing flame retardant has a good flame retardant effect. The bond energy of the C-F bond is strong and does not break at ordinary temperature. Therefore, although HF is harmful to human bodies, the fluorine-containing flame retardant does not cause harm to human bodies at ordinary temperatures, and is very safe. Only at extremely high temperature, in order to extinguish the fire in time and ensure life and property safety, the C-F bond is broken to play a role of flame retardance, thereby reducing the loss to the minimum.
The invention also provides application of the novel fluorine-containing flame retardant in nylon 6 modification.
Further, in a preferred embodiment of the present invention, the nylon 6 modification comprises the following steps:
preparing a flame-retardant master batch: mixing the fluorine-containing flame retardant with Sb 2 O 3 Mixing and processing by a double screw to obtain the flame-retardant master batch. Antimony trioxide Sb 2 O 3 In the initial stage of combustion, the material is first melted to form a protective film on the surface of the material to block air, and the combustion temperature is lowered by an internal endothermic reaction. The antimony trioxide is gasified at high temperature, and the concentration of oxygen and combustible gas in the air can be diluted, so that the flame retardant effect is achieved. The antimony trioxide can also generate a synergistic effect with a halogen-containing flame retardant, so that the flame retardant efficiency is improved.
Further, in a preferred embodiment of the present invention, the fluorine-containing flame retardant and the Sb 2 O 3 The mass ratio of (A) to (B) is 2.
Preparing modified nylon 6: and melting and mixing the flame-retardant master batch and the nylon 6 master batch, and then carrying out spinning processing to obtain the modified nylon 6.
Further, in a preferred embodiment of the present invention, in the melt mixture of the flame-retardant master batch and the nylon 6 master batch, the mass fraction of the flame-retardant master batch is 4 to 6%. The melting temperature is 180-200 ℃, and the spinning processing temperature is 185-215 ℃. The flame retardant 1, 2-bis (4-fluorophenyl) -1, 2-tetrafluoroethane has a wide temperature range for spinning because the upper limit of the boiling point of the flame retardant is 260 ℃. Nylon 6 and Sb for use in the present invention 2 O 3 Is commercially available, for example, nylon 6 canFrom Polychemicals Ltd, sb 2 O 3 Can be purchased from Henan Shiquan chemical products, inc.
The modified nylon 6 contains the fluorine-containing flame retardant with C-F bonds, so that the modified nylon 6 has good flame retardant capability. The modified nylon 6 is tested by UL 94V-level fire-retardant rating, and the fire-retardant rating can reach UL94V-0 level.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The novel fluorine-containing flame retardant provided by the embodiment is synthesized by the following synthesis method:
s1, mixing and diluting fluorine gas and inert gas to obtain fluorine gas mixed gas. Wherein the concentration of the fluorine gas in the fluorine gas mixed gas is 20%.
S2, adding 1, 2-di (phenyl) -tetrafluoroethane in the same molar ratio with the fluorine gas into the microreactor. And then, slowly introducing fluorine gas mixed gas for 1h, and reacting under the catalysis of anhydrous aluminum chloride, wherein the reaction temperature in the reaction process is kept at 25 ℃, so as to obtain a fluorine-containing flame retardant crude product.
And S3, diluting the fluorine-containing flame retardant crude product with water. Wherein the mass ratio of the water to the fluorine-containing flame retardant crude product is 30. Then, naOH aqueous solution with the mass fraction of 1% is added to neutralize the solution until the pH value is 7, and then water washing is carried out. Finally, treating the mixture for 3 hours by hot air at 150 ℃ and for 24 hours at 180 ℃ to obtain the fluorine-containing flame retardant.
Example 2
The novel fluorine-containing flame retardant provided by the embodiment is synthesized by the following synthesis method:
s1, mixing and diluting fluorine gas and inert gas to obtain fluorine gas mixed gas. Wherein the concentration of the fluorine gas in the fluorine gas mixed gas is 22%.
S2, adding 1, 2-di (phenyl) -tetrafluoroethane into the microreactor. Wherein the molar ratio of 1, 2-bis (phenyl) -tetrafluoroethane to fluorine gas was 0.8. And then, slowly introducing fluorine gas mixed gas for 1h, reacting under the catalysis of anhydrous aluminum chloride, and keeping the reaction temperature at 25 ℃ in the reaction process to obtain a fluorine-containing flame retardant crude product.
And S3, diluting the fluorine-containing flame retardant crude product with water. Wherein the mass ratio of water to the fluorine-containing flame retardant crude product is 30. Then, a 1% NaOH aqueous solution was added to neutralize the solution to pH 7, and then the solution was washed with water. Finally, treating the mixture for 3 hours by hot air at 180 ℃ and treating the mixture for 24 hours at 180 ℃ to obtain the fluorine-containing flame retardant.
Example 3
The novel fluorine-containing flame retardant provided by the embodiment is synthesized by the following synthesis method:
s1, mixing and diluting fluorine gas and inert gas to obtain fluorine gas mixed gas. Wherein the concentration of the fluorine gas in the fluorine gas mixed gas is 20%.
And S2, adding 1, 2-di (phenyl) -tetrafluoroethane in the same molar ratio with the fluorine gas into the microreactor. And then, slowly introducing fluorine gas mixed gas for 1h, and reacting under the catalysis of anhydrous aluminum chloride, wherein the reaction temperature in the reaction process is kept at 15 ℃ to obtain a fluorine-containing flame retardant crude product.
And S3, diluting the fluorine-containing flame retardant crude product with water. Wherein the mass ratio of the water to the fluorine-containing flame retardant crude product is 30. Then Na with a molar concentration of 1mol/l is added 2 CO 3 The aqueous solution was neutralized to pH 7 and washed with water. Finally, hot air treatment is carried out for 3h at 180 ℃ and high temperature treatment is carried out for 24h at 180 ℃ to obtain the fluorine-containing flame retardant.
Example 4
This example provides a modified nylon 6, which is prepared by the following method:
preparing a flame-retardant master batch: mixing a fluorine-containing flame retardant with Sb in a mass ratio of 2 2 O 3 Mixing and processing by a double screw to obtain the flame-retardant master batch.
Preparing modified nylon 6: and melting and mixing the flame-retardant master batch and the nylon 6 master batch at 180 ℃. Wherein, in the melt mixture of the flame-retardant master batch and the nylon 6 master batch, the mass fraction of the flame-retardant master batch is 5 percent. Then spinning processing is carried out at 215 ℃ to obtain the modified nylon 6.
After the spinning process is completed, a UL94 flame retardant rating standard is used for testing to verify the flame retardant rating of the modified PA 6. The test result shows that the flame retardant grade standard of the modified nylon 6 can reach UL94V-0 grade.
Example 5
This example provides a modified nylon 6 prepared by the following method:
preparing a flame-retardant master batch: mixing a fluorine-containing flame retardant with Sb in a mass ratio of 5 2 O 3 Mixing and processing by a double screw to obtain the flame-retardant master batch.
Preparing modified nylon 6: and melting and mixing the flame-retardant master batch and the nylon 6 master batch at 200 ℃. Wherein, in the melt mixture of the flame-retardant master batch and the nylon 6 master batch, the mass fraction of the flame-retardant master batch is 5 percent. Then spinning processing is carried out at 185 ℃ to obtain the modified nylon 6.
After the spinning process is completed, a UL94 flame retardant rating standard is used for testing to verify the flame retardant rating of the modified PA 6. The test result shows that the flame retardant grade standard of the modified nylon 6 can reach UL94V-0 grade.
Comparative example 1
This comparative example provides nylon 6, which differs from the modified nylon 6 of example 4 in that the nylon 6 was modified without the addition of the flame-retardant master batch.
Test example 1
The modified nylon 6 of example 4 and the nylon 6 of comparative example 1 were taken, respectively, and the modified nylon 6 and the nylon 6 were divided into 20 specimens, respectively, each having the same size and dimensions. Wherein, 10 samples are modified nylon 6, 10 samples are nylon 6, and each sample is a small strip sample with the length of 127mm, the width of 12.7mm and the maximum thickness of 12.7 mm. Dividing 10 samples of the modified nylon 6 into 2 groups, 5 samples in each group and 10 samples of the modified nylon into 2 groups, 5 samples in each group, and respectively testing the samples by adopting a UL94 flame retardant rating standard, wherein the test results are shown in a table 1:
table 1 ul94 table of flame retardant rating test results
Two times of after flame time tests and one time of after flame time tests are respectively carried out on the modified nylon 6 prepared in the embodiment 4 and the nylon 6 prepared in the comparative example 1, and the above table shows that the first time of after flame time, the second time of after flame time and the second time of after flame time of the modified nylon 6 are all far shorter than the corresponding time of the nylon 6, which indicates that the flame retardant effect of the modified nylon 6 is better than that of the nylon 6.
In conclusion, the modified nylon 6 of the embodiment of the invention can reach UL94V-0 grade through UL 94V-grade fire-proof rating measurement. HF generated after the C-F bond in the modified nylon 6 is broken can capture free radicals, has a good flame retardant effect, and can put out a fire in time, so that the life and property safety is guaranteed, and the loss is reduced to the minimum.
The embodiments described above are some, not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (9)
1. The synthesis method of the novel fluorine-containing flame retardant is characterized by comprising the following steps:
s1, mixing and diluting fluorine gas and inert gas to obtain fluorine gas mixed gas;
s2, adding 1, 2-bis (phenyl) -tetrafluoroethane and anhydrous aluminum chloride into the microreactor, slowly introducing the fluorine gas mixed gas, and reacting under the catalysis of the anhydrous aluminum chloride to synthesize a fluorine-containing flame retardant crude product;
and S3, diluting the crude product of the fluorine-containing flame retardant by using water, adding an alkali solution for neutralization, and then carrying out water washing, hot air treatment and high-temperature treatment to obtain the fluorine-containing flame retardant.
2. The method of synthesizing a novel fluorine-containing flame retardant according to claim 1, wherein in step S1, the concentration of the fluorine gas in the fluorine gas mixed gas is 15 to 25%.
3. The method of synthesizing a novel fluorine-containing flame retardant according to claim 1, wherein in step S2, the reaction temperature in the microreactor is lower than 40 ℃, and the molar ratio of the fluorine gas to the 1, 2-bis (phenyl) -tetrafluoroethane is from 0.8 to 1:1, the aeration time is 0.8 to 1.2 hours.
4. The method for synthesizing the novel fluorine-containing flame retardant according to claim 1, wherein in the step S2, the reaction temperature in the microreactor is 15 to 25 ℃.
5. The method for synthesizing the novel fluorine-containing flame retardant according to claim 1, wherein in the step S3, the mass ratio of the water to the crude fluorine-containing flame retardant is 30; the alkali solution is selected from NaOH aqueous solution with the mass fraction of 0.5-1.5% or Na with the molar concentration of 0.5-1.5 mol/l 2 CO 3 The pH of the aqueous solution after neutralization is 6.5-7.5.
6. The method for synthesizing the novel fluorine-containing flame retardant according to claim 1, wherein in the step S3, the hot air treatment temperature is 150 to 180 ℃, and the hot air treatment time is 2.5 to 3.5 hours; the high-temperature treatment temperature is 170-190 ℃, and the high-temperature treatment time is 23-25 h.
7. The application of the fluorine-containing flame retardant synthesized by the synthesis method of the novel fluorine-containing flame retardant according to any one of claims 1 to 6 in nylon 6 modification.
8. Use according to claim 7, wherein the nylon 6 modification comprises the following steps:
preparation of flame-retardant master batch: mixing the fluorine-containing flame retardant with Sb 2 O 3 Mixing and processing by a double screw to obtain flame-retardant master batch;
preparing modified nylon 6: and melting and mixing the flame-retardant master batch and the nylon 6 master batch, and then carrying out spinning processing to obtain the modified nylon 6.
9. The use according to claim 8, wherein in the step of preparing the flame-retardant masterbatch, the fluorine-containing flame retardant and the Sb are 2 O 3 The mass ratio of (1) to (5) is 2; and preparing modified nylon 6, wherein in the melt mixture of the flame-retardant master batch and the nylon 6 master batch, the mass fraction of the flame-retardant master batch is 4-6%, the melting temperature is 180-200 ℃, and the spinning processing temperature is 185-215 ℃.
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