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Reactive flame retardant as well as preparation method and application thereof

A reactive flame retardant and solvent technology, used in the field of flame retardants, can solve problems such as fire hazards, and achieve the effects of convenient post-processing, mild conditions and simple preparation methods

Active Publication Date: 2020-05-08
SUZHOU HSM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since there are currently not enough substitutes to replace all halogen-containing flame retardants, at the same time, Europe and Japan have completely banned the use of halogen-containing flame retardants, which has led some manufacturers to face "environmental issues" and cost issues. Double take, use of flame retardants has been discontinued
Therefore, the manufacturer's practice of reducing production costs and "responsive to environmental protection regulations" has caused serious fire hazards, making non-flame-retardant devices continue to burn with a very small ignition source

Method used

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  • Reactive flame retardant as well as preparation method and application thereof
  • Reactive flame retardant as well as preparation method and application thereof
  • Reactive flame retardant as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 25mL of tetrahydrofuran as a solvent to a 100mL three-neck flask equipped with a reflux condenser, a thermometer, and a stirring rod, and then add 3mL of xylene, heat to 80°C and stir evenly, then add 16.4g of TDCA (0.1mol), 37.2g of DMMP (0.3mol), in N 2 The reaction was maintained at 80°C for 5h under the atmosphere. After the reaction, the mixture was filtered, washed and dried to obtain the flame retardant as a white solid with a yield of 91%. The nuclear magnetic phosphorus spectrum of the obtained product is as follows figure 1 As shown, the infrared spectrum is shown in figure 2 As shown, the H NMR spectrum is shown as image 3 shown. Observation of the above drawings can prove that the target product has the structure shown in the above formula (I).

[0049]Mix 22 parts of the flame retardant prepared in this example with 78 parts of EP (product model 4926), and make a composite material by twin-screw extruder at 190°C.

[0050] Referring to the Ameri...

Embodiment 2

[0060] Add 62.5mL of acetonitrile as a solvent to a 250mL three-necked flask equipped with a reflux condenser, a thermometer and a stirring rod, then add 7.5mL of xylene, heat to 80°C and stir evenly, then add 41g of TDCA (0.25mol), 93g of DMMP (0.75mol), in N 2 The reaction was maintained at 80°C for 5h under the atmosphere. After the reaction, the mixture was filtered, washed and dried to obtain the flame retardant as a white solid with a yield of 79%.

[0061] Mix 22 parts of the flame retardant obtained in this example with 78 parts of EP (product model 4926), and make a composite material by twin-screw extruder at 190°C.

[0062] The above composite material is made into UL94 1.6mm standard sample in an injection molding machine, and the standard test is carried out on a horizontal and vertical combustion instrument and an oxygen index tester. After testing, the flame retardant grade of the sample is: UL94 1.6mm V-0 grade, oxygen index 30.

[0063] The above-mentioned ...

Embodiment 3

[0066] Add 250ml tetrahydrofuran as a solvent to a 1000mL three-necked flask equipped with a reflux condenser, a thermometer, and a stirring rod, then add 30mL of trimethylbenzene, heat to 80°C and stir evenly, then add 164g (1mol) of TDCA and 372gDMMP (3mol), in N 2 The reaction was maintained at 80°C for 5h under the atmosphere. After the reaction, the mixture was filtered, washed and dried to obtain a white solid with a yield of 84%.

[0067] Mix 22 parts of the flame retardant obtained in this example with 78 parts of EP (product model 4926), and make a composite material by twin-screw extruder at 190°C.

[0068] The above composite material is made into UL94 1.6mm standard sample in an injection molding machine, and the standard test is carried out on a horizontal and vertical combustion instrument and an oxygen index tester. After testing, the flame retardant grade of the sample is: UL94 1.6mm V-0 grade, oxygen index 30.

[0069] The above-mentioned composite material...

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Abstract

The invention discloses a reactive flame retardant as well as a preparation method and application thereof. The structural formula of the reactive flame retardant is shown in the following formula (I), the preparation method comprises the following steps: mixing dimethyl methylphosphate, terephthalaldehyde, a catalyst and a solvent, carrying out a reaction in nitrogen or an inert atmosphere, and carrying out post-treatment to obtain the reactive flame retardant, wherein the catalyst is selected from at least one of xylene, 2, 3-dichlorotoluene and trimethylbenzene, and the solvent is selectedfrom tetrahydrofuran and / or acetonitrile. The preparation method disclosed by the invention is simple, mild in condition, easy to control and high in product purity, and the prepared reactive flame retardant has the advantages of novel structure, high flame retardant efficiency, environmental protection and low toxicity; and especially, the prepared reactive flame retardant has excellent flame retardant property in an epoxy resin matrix.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a reactive flame retardant and its preparation method and application. Background technique [0002] Epoxy resin is a kind of thermosetting synthetic resin with excellent performance. Many fields such as plastics and composite materials have been widely developed and applied. However, the biggest disadvantage in the application of epoxy resin is the problem of flammability, which is also a problem with most polymer materials. Due to its flammability, the application range of epoxy resin is greatly limited. Therefore, the research on the flame retardancy of epoxy resin is of great significance for expanding its application in various fields. [0003] In recent years, the most popular topic in the flame retardant academic circle is the problem of environmental pollution caused by halogen-containing materials, and the search for suitable new flame retardants ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5333C07F9/40C08L63/00
CPCC08K5/5333C07F9/4025C08L2201/02C08L63/00
Inventor 台启龙胡颐阳何明山
Owner SUZHOU HSM TECH CO LTD
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