Flame retardant, flame-retardant thermoplastic resin and preparation method thereof

Abstract

The invention discloses a flame retardant, flame-retardant thermoplastic resin and a preparation method thereof. The preparation method of the flame retardant comprises the following steps: (1) mixing hydroxyethylidene-1, 1-diphosphonic acid, glucose, a catalyst, absolute ethyl alcohol and deionized water to prepare a solution A; and (2) cooling, washing and filtering the solution A to obtain the hydroxyethylidene-1, 1-diphosphonic acid-glucose type flame retardant. The invention innovatively synthesizes the flame-retardant thermoplastic resin and the preparation method thereof, the flame-retardant thermoplastic resin has good flame retardant property, and the technical problem that the flame retardant property of the thermoplastic resin in the prior art is limited is solved.

Description

Technical Field

[0001] The present invention relates to the field of flame - retardant polymer materials, and specifically to a flame retardant, a flame - retardant thermoplastic resin, and a preparation method thereof. Background Art

[0002] Thermoplastic resins are widely used polymer resins. Thermoplastic resins have good fatigue resistance, relatively good heat resistance, excellent dimensional stability and other advantages. However, most thermoplastic materials have varying degrees of flammability. With the development of technology and the improvement of the living standards of humans, in the fields of civil use, transportation, electric power, aerospace, etc., the requirements for the flame - retardant performance of materials are getting higher and higher. Some components need to reach the V - 0 level, and it is necessary to further modify thermoplastic resins to improve their flame - retardant performance.

[0003] In view of these deficiencies, the present invention innovatively synthesizes a flame - retardant thermoplastic resin composite material, which has good flame - retardant performance and is of great significance for expanding the application fields of thermoplastic resin composite materials. Summary of the Invention

[0004] In view of this, the present invention provides a flame retardant, a flame - retardant thermoplastic resin, and a preparation method thereof to solve the problems raised in the above - mentioned background art. It innovatively synthesizes a flame - retardant thermoplastic resin and its preparation method, which has good flame - retardant performance and solves the technical problem of the limited flame - retardant performance of thermoplastic resins in the prior art.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] The first aspect of the present invention discloses a preparation method of a flame retardant, including the following steps:

[0007] (1) Mix hydroxyethylidene diphosphonic acid, glucose, a catalyst, absolute ethanol, and deionized water, and stir - react at 60 - 80 °C for 8 - 16 h to prepare solution A;

[0008] (2) Cool, wash, and filter solution A to obtain a flame retardant of the hydroxyethylidene diphosphonic acid - glucose type.

[0009] As a further scheme of the present invention: the mass ratio of hydroxyethylidene diphosphonic acid, glucose, catalyst, absolute ethanol, and deionized water in step (1) is (30 - 40):(24 - 30):(0.2 - 0.4):(50 - 60):(100 - 160).

[0010] As a further scheme of the present invention: the catalyst is tert - butyl hydroperoxide.

[0011] The second aspect of the present invention discloses a flame retardant prepared by the above - mentioned preparation method.

[0012] The third aspect of the present invention discloses a flame-retardant thermoplastic resin composite, which is composed of the following components in parts by weight:

[0013] Thermoplastic resin: 91 parts - 111 parts,

[0014] Flame retardant: 20 parts - 24 parts,

[0015] Antioxidant: 0.1 part - 0.5 part;

[0016] The flame retardant used is the above-mentioned flame retardant.

[0017] As a further scheme of the present invention: The antioxidant is at least one of bis(2,4-dicumylphenyl)pentaerythritol diphosphite, pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], and N,N'-bis(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl)hexamethylenediamine.

[0018] As a further scheme of the present invention: The thermoplastic resin is at least one of polyethylene, polypropylene, polystyrene, polybutylene terephthalate, and polyamide 6.

[0019] The fourth aspect of the present invention discloses a preparation method of the above-mentioned flame-retardant thermoplastic resin composite, which includes the following steps:

[0020] Weigh the thermoplastic resin, flame retardant, and antioxidant in parts by weight, mix and stir evenly to obtain a mixture;

[0021] Add the mixture into a twin-screw extruder for extrusion granulation to obtain the flame-retardant thermoplastic resin composite.

[0022] Compared with the prior art, the beneficial effects of the present invention are:

[0023] (1) In the present invention, the bio-based materials hydroxyethylidene diphosphonic acid and glucose undergo an esterification reaction under certain conditions. Through the reaction of the phosphate group of hydroxyethylidene diphosphonic acid with the -OH of glucose, a flame retardant of the hydroxyethylidene diphosphonic acid-glucose type is generated. The specific chemical equation is as follows:

[0024]

[0025] (2) When the flame retardant of the hydroxyethylidene diphosphonic acid-glucose type decomposes upon heating, phosphorus-containing oxides are generated, forming a carbon layer protective film on the surface. Glucose itself can serve as a carbon source, and the two constitute an intumescent flame retardant system, improving the flame retardant performance of the thermoplastic resin. In addition, when hydroxyethylidene diphosphonic acid-glucose burns, small bubbles will form on the surface, and these bubbles can play a role in blocking oxygen and protecting the thermoplastic resin, which also makes the flame retardant performance of the thermoplastic resin better. Detailed implementation manners

[0026] To facilitate the understanding of the present invention, the present invention will be described more comprehensively below in conjunction with specific embodiments. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.

[0027] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field to which the present invention belongs. The terms used in the description of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0028] The specific information of the raw materials used in the following examples and comparative examples is as follows:

[0029] Polybutylene terephthalate (PBT), model L08XM, Jiangsu Heshili;

[0030] Polypropylene (PP), model Z30S, Maoming Petrochemical;

[0031] Polyethylene (PE), model 5070, Panjin Ethylene;

[0032] Polyamide 6 (PA6), model J2500, Hangzhou Juheshun;

[0033] Polystyrene (PS) model 350, Taiwan Guochiao;

[0034] 1-Hydroxyethylidene-1,1-diphosphonic acid, Jinan Xinying Chemical Co., Ltd.;

[0035] Glucose, Shandong Siyang Biotechnology Co., Ltd.;

[0036] tert-Butyl hydroperoxide, Jinan Xinquan Chemical Technology Co., Ltd.;

[0037] Absolute ethanol, Changzhou Lanzhou Chemical Co., Ltd.;

[0038] Deionized water, Xiamen Aoquan Environmental Protection Technology Co., Ltd.;

[0039] Flame retardant WR02, Suzhou Anhongtai New Materials Co., Ltd.; Antioxidant S9228, Dow Chemical of the United States; Antioxidants (Irganox1010, Irganox1098), BASF of Germany.

[0040] All materials are commercially available conventional and commonly used products.

[0041] The test instruments used in the present invention are as follows:

[0042] ZSK30 twin-screw extruder, produced by W&P Company in Germany; JL-1000 tensile testing machine, produced by Guangzhou Guangcai Experimental Instrument Company; HTL900-T-5B injection molding machine, produced by Haitai Plastic Machinery Co., Ltd.; XCJ-500 impact testing machine, produced by Chengde Testing Machine Factory; QT-1196 tensile tester, produced by Dongguan Gaotai Testing Instrument Co., Ltd.; QD-GJS-B12K high-speed mixer, produced by Beijing Heng'ao Instrument Co., Ltd.

[0043] Preparation Example 1

[0044] (1) Weigh 300 g of hydroxyethane diphosphonic acid, 240 g of glucose, 2 g of catalyst, 500 g of absolute ethanol, and 1.0 kg of deionized water, add them to a reaction vessel, and stir and react at 60 °C for 8 h to prepare Solution A.

[0045] (2) Cool, wash, and filter Solution A to obtain the flame retardant M1 of the hydroxyethane diphosphonic acid-glucose type.

[0046] Example 1

[0047] (1) Weigh 91 parts of PP, 20 parts of flame retardant M1, and 0.1 part of Irganox 1010, mix and stir evenly to obtain a mixture.

[0048] (2) Extrude and pelletize the mixture obtained in step (1) from the twin-screw extruder to obtain the PP composite material P1.

[0049] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 170 °C, the temperature of the second temperature zone is 220 °C, the temperature of the third temperature zone is 220 °C, the temperature of the fourth temperature zone is 220 °C, the temperature of the fifth temperature zone is 220 °C, the temperature of the sixth temperature zone is 220 °C, the head temperature of the twin-screw extruder is 220 °C, and the screw speed is 220 r / min.

[0050] Comparative Example 1

[0051] (1) Weigh 91 parts of PP and 0.1 part of Irganox 1010, mix and stir evenly to obtain a mixture.

[0052] (2) Extrude and pelletize the mixture obtained in step (1) from the extruder to obtain the PP composite material D1.

[0053] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 170 °C, the temperature of the second temperature zone is 220 °C, the temperature of the third temperature zone is 220 °C, the temperature of the fourth temperature zone is 220 °C, the temperature of the fifth temperature zone is 220 °C, the temperature of the sixth temperature zone is 220 °C, the head temperature of the twin-screw extruder is 220 °C, and the screw speed is 220 r / min.

[0054] Comparative Example 2

[0055] (1) Weigh 91 parts of PP, 20 parts of commercially available flame retardant WR02, and 0.1 part of Irganox1010, mix and stir evenly to obtain a mixed material.

[0056] (2) Extrude and pelletize the mixed material obtained in step (1) from the twin-screw extruder to obtain the PP composite material D1.

[0057] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 170 °C, the temperature of the second temperature zone is 220 °C, the temperature of the third temperature zone is 220 °C, the temperature of the fourth temperature zone is 220 °C, the temperature of the fifth temperature zone is 220 °C, the temperature of the sixth temperature zone is 220 °C, the head temperature of the twin-screw extruder is 220 °C, and the screw speed is 220 r / min.

[0058] The PP composite materials prepared in Example 1 and Comparative Examples 1-2 above were made into splines for testing with an injection molding machine, and the test data are shown in Table 1 below.

[0059] Table 1

[0060] Test Items Test Standards Unit P1 D1 D2 Flame Retardant Rating UL 94 / V-0 HB V-1

[0061] As can be seen from Table 1 above, the flame retardant properties of Example 1 are better than those of Comparative Examples 1-2.

[0062] Preparation Example 2

[0063] (1) Weigh 400 g of hydroxyethylidene diphosphonic acid, 300 g of glucose, 4 g of catalyst, 600 g of absolute ethanol, and 1.6 kg of deionized water, add them to a reaction vessel, and stir and react at 80 °C for 16 h to prepare solution A.

[0064] (2) Cool, wash, and filter solution A to obtain the flame retardant M2 of the hydroxyethylidene diphosphonic acid-glucose type.

[0065] Example 2

[0066] (1) Weigh 111 parts of PBT, 24 parts of flame retardant M2, 0.1 part of antioxidant Irganox1010, 0.2 part of antioxidant S9228, and 0.2 part of antioxidant Irganox1098, mix them and stir evenly to obtain a mixed material;

[0067] (2) Extrude and pelletize the mixed material obtained in step (1) from a twin-screw extruder to obtain the PBT composite material P2.

[0068] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 200 °C, the temperature of the second temperature zone is 230 °C, the temperature of the third temperature zone is 230 °C, the temperature of the fourth temperature zone is 230 °C, the temperature of the fifth temperature zone is 230 °C, the temperature of the sixth temperature zone is 230 °C. The head temperature of the twin-screw extruder is 230 °C, and the screw speed is 300 r / min.

[0069] Comparative Example 3

[0070] (1) Weigh 111 parts of PBT, 0.1 part of antioxidant Irganox1010, 0.2 part of antioxidant S9228, and 0.2 part of antioxidant Irganox1098, mix them and stir evenly to obtain a mixed material;

[0071] (2) Extrude and pelletize the mixed material obtained in step (1) from an extruder to obtain the PBT composite material D3.

[0072] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 200 °C, the temperature of the second temperature zone is 230 °C, the temperature of the third temperature zone is 230 °C, the temperature of the fourth temperature zone is 230 °C, the temperature of the fifth temperature zone is 230 °C, the temperature of the sixth temperature zone is 230 °C. The head temperature of the twin-screw extruder is 230 °C, and the screw speed is 300 r / min.

[0073] Comparative Example 4

[0074] (1) Weigh 111 parts of PBT, 24 parts of commercially available flame retardant WR02, 0.1 part of antioxidant Irganox1010, 0.2 part of antioxidant S9228, and 0.2 part of antioxidant Irganox1098, mix them and stir evenly to obtain a mixed material;

[0075] (2) Extrude and pelletize the mixed material obtained in step (1) from a twin-screw extruder to obtain the PBT composite material D4.

[0076] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 200 °C, the temperature of the second temperature zone is 230 °C, the temperature of the third temperature zone is 230 °C, the temperature of the fourth temperature zone is 230 °C, the temperature of the fifth temperature zone is 230 °C, the temperature of the sixth temperature zone is 230 °C, the head temperature of the twin-screw extruder is 230 °C, and the screw speed is 300 r / min.

[0077] The PBT composites prepared in the above Example 2 and Comparative Examples 3-4 were made into splines for testing with an injection molding machine, and the test data are shown in Table 2 below.

[0078] Table 2

[0079] Test Items Test Standards Unit P2 D3 D4 Flame Retardant Rating UL 94 / V-0 HB V-1

[0080] As can be seen from the above table, the flame retardancy of Example 2 is better than that of Comparative Examples 3-4.

[0081] Preparation Example 3

[0082] (1) Weigh 350 g of hydroxyethylidene diphosphonic acid, 270 g of glucose, 3 g of the catalyst tert-butyl hydroperoxide, 550 g of absolute ethanol, and 1.3 kg of deionized water, add them to a reaction vessel, and stir and react at 70 °C for 12 h to prepare Solution A.

[0083] (2) Cool, wash, and filter Solution A to obtain the flame retardant M3 of the hydroxyethylidene diphosphonic acid-glucose type.

[0084] Example 3

[0085] (1) Weigh 100 parts of PE, 22 parts of flame retardant M3, 0.1 part of antioxidant S9228, and 0.2 part of antioxidant Irganox1010, mix and stir evenly to obtain a mixture;

[0086] (2) Extrude and pelletize the mixture obtained in step (1) from a twin-screw extruder to obtain the PE composite material P3.

[0087] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 120 °C, the temperature of the second temperature zone is 180 °C, the temperature of the third temperature zone is 180 °C, the temperature of the fourth temperature zone is 180 °C, the temperature of the fifth temperature zone is 180 °C, the temperature of the sixth temperature zone is 180 °C, the head temperature of the twin-screw extruder is 180 °C, and the screw speed is 300 r / min.

[0088] Comparative Example 5

[0089] (1) Weigh 100 parts of PE, 0.1 part of antioxidant S9228, and 0.2 part of antioxidant Irganox1010, mix and stir evenly to obtain a mixture;

[0090] (2) Extrude and pelletize the mixture obtained in step (1) from a twin-screw extruder to obtain the PE composite material P3.

[0091] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 120 °C, the temperature of the second temperature zone is 180 °C, the temperature of the third temperature zone is 180 °C, the temperature of the fourth temperature zone is 180 °C, the temperature of the fifth temperature zone is 180 °C, the temperature of the sixth temperature zone is 180 °C. The head temperature of the twin-screw extruder is 180 °C, and the screw speed is 300 r / min.

[0092] Comparative Example 6

[0093] (1) Weigh 100 parts of PE, 22 parts of commercially available flame retardant WR02, 0.1 part of antioxidant S9228, and 0.2 part of antioxidant Irganox1010, mix and stir evenly to obtain a mixture.

[0094] (2) Extrude and pelletize the mixture obtained in step (1) from a twin-screw extruder to obtain the PE composite material D6.

[0095] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 120 °C, the temperature of the second temperature zone is 180 °C, the temperature of the third temperature zone is 180 °C, the temperature of the fourth temperature zone is 180 °C, the temperature of the fifth temperature zone is 180 °C, the temperature of the sixth temperature zone is 180 °C. The head temperature of the twin-screw extruder is 180 °C, and the screw speed is 300 r / min.

[0096] The PE composite materials prepared in the above Example 3 and Comparative Examples 5-6 were made into splines for testing by an injection molding machine, and the test data are shown in Table 3 below.

[0097] Table 3

[0098] Test Items Test Standards Unit P3 D5 D6 Flame Retardant Rating UL 94 V-0 HB V-1

[0099] As can be seen from the above table, the flame retardancy of Example 3 is better than that of Comparative Examples 5-6.

[0100] Preparation Example 4

[0101] (1) Weigh 395 g of hydroxyethylidene diphosphonic acid, 285 g of glucose, 3.5 g of catalyst tert-butyl hydroperoxide, 515 g of absolute ethanol, and 145 g of deionized water, add them to a reaction vessel, and stir and react at 75 °C for 15 h to prepare solution A.

[0102] (2) Cool, wash, and filter solution A to obtain the flame retardant M4 of the hydroxyethylidene diphosphonic acid-glucose type.

[0103] Example 4

[0104] (1) Weigh 95 parts of PA6, 23 parts of flame retardant M4, 0.1 part of antioxidant Irganox1010, and 0.2 part of antioxidant Irganox1098, mix them evenly and stir well to obtain a mixed material;

[0105] (2) Extrude and pelletize the mixed material obtained in step (1) from a twin-screw extruder to obtain the PA6 composite material P4.

[0106] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 210°C, the temperature of the second temperature zone is 260°C, the temperature of the third temperature zone is 260°C, the temperature of the fourth temperature zone is 260°C, the temperature of the fifth temperature zone is 260°C, the temperature of the sixth temperature zone is 260°C. The head temperature of the twin-screw extruder is 260°C, and the screw speed is 320 r / min.

[0107] Comparative Example 7

[0108] (1) Weigh 95 parts of PA6, 0.1 part of antioxidant Irganox1010, and 0.2 part of antioxidant Irganox1098, mix them evenly and stir well to obtain a mixed material;

[0109] (2) Extrude and pelletize the mixed material obtained in step (1) from a twin-screw extruder to obtain the PA6 composite material D7.

[0110] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 210°C, the temperature of the second temperature zone is 260°C, the temperature of the third temperature zone is 260°C, the temperature of the fourth temperature zone is 260°C, the temperature of the fifth temperature zone is 260°C, the temperature of the sixth temperature zone is 260°C. The head temperature of the twin-screw extruder is 260°C, and the screw speed is 320 r / min.

[0111] Comparative Example 8

[0112] (1) Weigh 95 parts of PA6, 23 parts of commercially available flame retardant WR02, 0.1 part of antioxidant Irganox1010, and 0.2 part of antioxidant Irganox1098, mix them evenly and stir well to obtain a mixed material;

[0113] (2) Extrude and pelletize the mixed material obtained in step (1) from an extruder to obtain the PA6 composite material D4.

[0114] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 210°C, the temperature of the second temperature zone is 260°C, the temperature of the third temperature zone is 260°C, the temperature of the fourth temperature zone is 260°C, the temperature of the fifth temperature zone is 260°C, the temperature of the sixth temperature zone is 260°C, the head temperature of the twin-screw extruder is 260°C, and the screw speed is 320 r / min.

[0115] The PA6 composite materials prepared in the above Example 4 and Comparative Examples 7-8 were made into splines for testing by an injection molding machine, and the test data are shown in Table 4 below:

[0116] Table 4

[0117] Test Items Test Standards Unit P4 D7 D8 Flame Retardant Rating UL 94 / V-0 HB V-1

[0118] As can be seen from the above table, the flame retardancy of Example 4 is better than that of Comparative Examples 7-8.

[0119] Preparation Example 5

[0120] (1) Weigh 325 g of hydroxyethylidene diphosphonic acid, 255 g of glucose, 2.5 g of the catalyst tert-butyl hydroperoxide, 535 g of absolute ethanol, and 1.25 kg of deionized water, add them to a reaction vessel, and stir and react at 75°C for 9 h to prepare Solution A.

[0121] (2) Cool, wash, and filter Solution A to obtain the flame retardant M5 of the hydroxyethylidene diphosphonic acid-glucose type.

[0122] Example 5

[0123] (1) Weigh 105 parts of PS, 23.5 parts of the flame retardant M5, 0.1 part of the antioxidant Irganox1010, and 0.1 part of the antioxidant S9228, mix and stir evenly to obtain a mixed material;

[0124] (2) Extrude and pelletize the mixed material obtained in step (1) from a twin-screw extruder to obtain the PS composite material P5.

[0125] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 180°C, the temperature of the second temperature zone is 220°C, the temperature of the third temperature zone is 220°C, the temperature of the fourth temperature zone is 220°C, the temperature of the fifth temperature zone is 220°C, the temperature of the sixth temperature zone is 220°C, the head temperature of the twin-screw extruder is 220°C, and the screw speed is 280 r / min.

[0126] Comparative Example 9

[0127] (1) Weigh 105 parts of PS, 0.1 part of antioxidant Irganox1010, and 0.1 part of antioxidant S9228, mix them and stir evenly to obtain a mixed material;

[0128] (2) Extrude and pelletize the mixed material obtained in step (1) from a twin-screw extruder to obtain PS composite material D9.

[0129] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 180 °C, the temperature of the second temperature zone is 220 °C, the temperature of the third temperature zone is 220 °C, the temperature of the fourth temperature zone is 220 °C, the temperature of the fifth temperature zone is 220 °C, the temperature of the sixth temperature zone is 220 °C, the head temperature of the twin-screw extruder is 220 °C, and the screw speed is 280 r / min.

[0130] Comparative Example 10

[0131] (1) Weigh 105 parts of PS, 23.5 parts of commercially available flame retardant WR02, 0.1 part of antioxidant Irganox1010, and 0.1 part of antioxidant S9228, mix them and stir evenly to obtain a mixed material;

[0132] (2) Extrude and pelletize the mixed material obtained in step (1) from a twin-screw extruder to obtain PS composite material D10.

[0133] Among them, the twin-screw extruder includes six temperature zones arranged in sequence. The temperature of the first temperature zone is 180 °C, the temperature of the second temperature zone is 220 °C, the temperature of the third temperature zone is 220 °C, the temperature of the fourth temperature zone is 220 °C, the temperature of the fifth temperature zone is 220 °C, the temperature of the sixth temperature zone is 220 °C, the head temperature of the twin-screw extruder is 220 °C, and the screw speed is 280 r / min.

[0134] Make the PS composite materials prepared in the above Example 5 and Comparative Examples 9-10 into splines for testing with an injection molding machine. The test data are shown in Table 5 below.

[0135] Table 5

[0136] Test Items Test Standards Unit P5 D9 D10 Flame Retardant Rating UL 94 / V-0 HB V-1

[0137] As can be seen from the above table, the flame retardancy of Example 5 is better than that of Comparative Examples 9-10.

[0138] It is understood that the above raw materials and reagents are only examples of some specific embodiments of the present invention to make the technical solutions of the present invention clearer, and do not represent that the present invention can only adopt the above reagents. Specifically, it shall be subject to the scope in the claims. In addition, the "parts" mentioned in the examples and comparative examples refer to parts by weight unless otherwise specified.

[0139] Any range described in the present invention includes the end values, any numerical value between the end values, and any sub-range constituted by any numerical value between the end values or the end values.

[0140] Although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

[0141] Therefore, the above is only the preferred embodiment of the present application and is not used to limit the scope of implementation of the present application; that is, all equivalent transformations made according to the scope of the claims of the present application are within the protection scope of the claims of the present application.

Claims

1. A method for preparing a flame retardant, characterized in that, It includes the following steps: (1) Mix hydroxyethane diphosphonic acid, glucose, a catalyst, absolute ethanol, and deionized water, and stir and react at 60 - 80 °C for 8 - 16 h to prepare solution A; (2) Cool, wash, and filter solution A to obtain a flame retardant of the hydroxyethane diphosphonic acid - glucose type.

2. The preparation method according to claim 1, wherein The mass ratio of hydroxyethane diphosphonic acid, glucose, the catalyst, absolute ethanol, and deionized water in step (1) is (30 - 40):(24 - 30):(0.2 - 0.4):(50 - 60):(100 - 160).

3. The preparation method according to claim 1, wherein The catalyst is tert - butyl hydroperoxide.

4. A flame retardant prepared by the preparation method according to any one of claims 1 - 3.

5. A flame-retardant thermoplastic resin composite, characterized in that, It is composed of the following components by weight: 91 parts - 111 parts of thermoplastic resin, 20 parts - 24 parts of flame retardant, 0.1 parts - 0.5 parts of antioxidant; The flame retardant is the flame retardant according to claim 4.

6. The flame-retardant thermoplastic resin composite according to claim 1, wherein The antioxidant is at least one of bis(2,4 - di - tert - butylphenyl)pentaerythritol diphosphite, pentaerythritol tetra[β-(3,5 - di - tert - butyl - 4 - hydroxyphenyl)propionate], and N,N’ - bis(3-(3,5 - di - tert - butyl - 4 - hydroxyphenyl)propionyl)hexanediamine.

7. The flame-retardant thermoplastic resin composite according to claim 1, characterized in that, The thermoplastic resin is at least one of polyethylene, polypropylene, polystyrene, polybutylene terephthalate, and polyamide 6.

8. The preparation method of a flame-retardant thermoplastic resin composite according to any one of claims 6-7, characterized in that, It includes the following steps: Weigh the thermoplastic resin, flame retardant, and antioxidant by weight, mix and stir evenly to obtain a mixture; Add the mixture into a twin - screw extruder for extrusion granulation to obtain a flame - retardant thermoplastic resin composite material.

Images