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Triazine compound, as well as preparation method and application thereof

A compound and triazine technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of low thermal stability of products, large amount of organic solvents, and difficulty in subsequent processing. and other problems, to avoid excessive reaction time, less side reactions, and facilitate industrial production.

Active Publication Date: 2017-06-27
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above preparation methods all have the disadvantages of large amount of organic solvent (mainly acetone), serious environmental pollution, difficult follow-up treatment, low thermal stability of the product, low carbon residue, etc., and the reaction cycle is generally longer, more than 20 hours

Method used

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  • Triazine compound, as well as preparation method and application thereof
  • Triazine compound, as well as preparation method and application thereof
  • Triazine compound, as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 188.0g (1mol) of 2,2'-dihydroxybiphenyl (99.0%), 433.0g of toluene (99.5%) to a 2L four-necked round-bottomed flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, 132.9g (1.3mol) of triethylamine (content 99.0%), start stirring, control the temperature at 10°C, add 155.6g (1mol) (98.5%) of phosphorus oxychloride dropwise for 1.0h, and continue the reaction for 4h. Rotary steam toluene, add 800g water, 37.9g ​​(0.3mol) melamine (99.8%), cool down after 100 ℃ of reflux reaction 3h, filter, dry, obtain product 801.1g, calculate yield 96.0% with phosphorus oxychloride, heat The amount of carbon formed at 500°C by gravimetric analysis is 51.8%, and the thermal decomposition temperature is 305°C.

[0035] figure 1 It is the infrared spectrogram of embodiment 1 gained triazine compound, from figure 1 It can be seen that there are melamine groups (1650~1000cm -1 ), biphenyl group (3500~2800cm -1 ) and phosphorus oxygen group (600~750cm ...

Embodiment 2

[0037] Add 225.6g (1.2mol) of 2,2'-dihydroxybiphenyl (99.0%) and 433.0g of toluene (99.5%) to a 2L four-necked round-bottomed flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel , 112.4g (1.1mol) triethylamine (content 99.0%), start stirring, control the temperature at 10°C, add 155.6g (1mol) (98.5%) of phosphorus oxychloride dropwise for 1.5h, and continue the reaction for 5h. Rotary steam toluene, add 800g of water, 39.1g of melamine (0.31mol) (99.8%), reflux at 100°C for 3.5h, then cool down, filter, and dry to obtain 821.5g of the product, with a yield of 98.5% based on phosphorus oxychloride. According to thermogravimetric analysis, the amount of carbon formed at 500°C is 50.2%, and the thermal decomposition temperature is 304°C.

Embodiment 3

[0039] Add 188.0g (1mol) of 2,2'-dihydroxybiphenyl (99.0%), 433.0g of toluene (99.5%) to a 2L four-necked round-bottomed flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, 102.2g (1mol) of triethylamine (content 99.0%), start stirring, control the temperature at 10°C, add 155.6g (1mol) (98.5%) of phosphorus oxychloride dropwise for 3h, and continue the reaction for 7h. Rotary steam toluene, add 800g of water, 37.9g ​​(0.3mol) of melamine (99.8%), reflux at 100°C for 5h, cool down, filter, and dry to obtain 809.8g of the product, with a yield of 97.1% based on phosphorus oxychloride. According to thermogravimetric analysis, the amount of carbon formed at 500°C is 50.2%, and the thermal decomposition temperature is 304°C.

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Abstract

The invention discloses a triazine compound, as well as a preparation method and application thereof. The novel triazine compound is prepared by taking 2,2'-dihydroxybiphenyl, phosphorus oxychloride, triethylamine and melamine as main raw materials, not only has a carbon source (biphenyl structure), but also has an acid source (phosphoric acid structure) and a gas source (melamine). The carbon forming agent has high carbon forming property, high thermal decomposition temperature, high stability and large residual carbon quantity. According to the preparation method provided by the invention, the reaction condition is mild, the side reaction is less, the operating flow is simple, the reaction cycle is greatly shortened, the used raw materials are safe and easily available, the use of an organic solvent is avoided because water serves as a reaction medium, the aftertreatment process is simplified, and industrialized production is facilitated. The solvent and the mother liquid can be recycled and reused, the operating flow of the process is simple, and the defects that the reaction time is too long and the use amount of the organic solvent is large in the existing process are overcome.

Description

technical field [0001] The invention relates to a new compound, in particular to a triazine compound, a preparation method and an application thereof. It belongs to the field of material technology. Background technique [0002] Intumescent halogen-free flame retardant is a compound flame retardant containing nitrogen and phosphorus, which is mainly used for the flame retardancy of polyolefins. It is the fastest-growing type of halogen-free flame retardant in recent years. When the polymer material containing intumescent halogen-free flame retardant is heated and burned, a uniform foam carbon layer will be formed on the surface of the polymer. The role of molten droplets can effectively prevent the generation and diffusion of toxic smoke and corrosive gases, and it is a very promising new flame retardant. [0003] Generally speaking, intumescent flame retardants include three parts, namely carbon source (usually polyol, such as pentaerythritol), acid source (such as ammoni...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C07D251/54C07D251/56C08K5/3492C08K5/527
CPCC07D251/54C07D251/56C07F9/65744C08K5/34928C08K5/527
Inventor 岳涛邢文国冯维春陈琦魏凤付永丰徐婷王达彤
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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