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Intumescent flame retardant and synthesis method thereof

An intumescent flame retardant and a synthesis method technology, applied in the field of flame retardants, can solve the problems of small content of effective flame retardant components, low flame retardant efficiency, unfavorable storage and storage, etc., and achieve good compatibility and easy Control, the effect of low production cost

Inactive Publication Date: 2011-02-16
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, the halogen-free intumescent flame retardants involved in the above patents generally only contain two flame retardant components, phosphorus and nitrogen, and the effective flame retardant components are relatively small, and the flame retardant efficiency is not very high, and many flame retardant products are prone to Water absorption, unfavorable storage and storage, poor compatibility with polymers, high production cost, complex synthesis process, etc.

Method used

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  • Intumescent flame retardant and synthesis method thereof
  • Intumescent flame retardant and synthesis method thereof
  • Intumescent flame retardant and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 8.32g (0.08mol) of neopentyl glycol and 30mL of chloroform into a 100mL four-necked reaction flask equipped with a thermometer, a reflux condenser, a magnetic stirrer, and an exhaust gas absorption device, stir well to dissolve the neopentyl glycol, and then Add 8.32mL (0.08mol) of phosphorous trichloride dropwise to the reaction flask, after 2 hours, the reaction temperature was gradually raised to 50°C, and the reaction was completed for 3 hours, then the reaction was terminated, distilled under reduced pressure, washed with water, and dried in vacuum for 12 hours to obtain a white Solid, 2-thio-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane, yield 75.5%.

[0032]Weigh 36g (0.18mol) of 2-thio-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane and? In a 250mL four-necked reaction flask, add 100mL DMF, stir rapidly to dissolve it, then add 9.54g (0.09mol) of dithiosemicarbazide, 26.01mL (0.18mol) of triethylamine, heat to 50°C, React for 4 hours, stop the reaction, fil...

Embodiment 2

[0034] The molar ratio of neopentyl glycol to phosphorus trichloride in this embodiment is 1.25:1. In the synthesis process, after the phosphorus trichloride is added dropwise, the reaction temperature rises to 75° C., and the reaction time is 4 hours. The rest are the same as in Example 1.

[0035] The yield of 2-thio-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane in this example is 78.6%; N, N'-two (5, The yield of 5-dimethyl-2-phospha-2-thio-1,3-dioxan-2-yl)dithiosemicarbazide was 72.7%.

Embodiment 3

[0037] The molar ratio of neopentyl glycol to phosphorus trichloride in this embodiment is 1.25:1. In the synthesis process, after the addition of thion trichloride is completed, the reaction temperature rises to 75°C, and the reaction time is 6 hours. 2-thio-2-chloro-5,5-dimethyl-1,3,2-di The molar ratio of oxaphosphorinane to dithioaminourea is 2: 1.2, and all the other are the same as in Example 1.

[0038] The yield of 2-thio-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane in this example is 78.6%; N, N'-two (5, The yield of 5-dimethyl-2-phospha-2-thio-1,3-dioxan-2-yl)dithiosemicarbazide was 76%.

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Abstract

The invention discloses an intumescent flame retardant and a synthesis method thereof. The structural formula of the flame retardant is as shown in the figure, and the chemical name of the flame retardant is N,N'-bis(5,5-dimethyl-2-phospha-2-sulfo-1,3-dioxane-2-yl) dithiosemicarbazide. The synthesis method comprises the following steps: adding neopentyl glycol into a reaction vessel filled with a first solvent, dropwise adding phosphorus thiochloride at 50-100 DEG C, reacting for 2-10 h, carrying out reduced pressure distillation, washing with water, and drying to obtain a white solid, namely 2-sulfo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane; and adding the white solid to a second solvent, adding dithiosemicarbazide and acid binding agent, reacting at 40-120 DEG C for 2-10 h, filtering, pouring the filtrate into ice water, dropwise adding a defined amount of inorganic acid until the pH value of the filtrate is 7 and white solid powder is separated out, washing, filtering, and drying to obtain the finished product.

Description

technical field [0001] The invention relates to flame retardant technology, in particular to a novel intumescent flame retardant containing phosphorus, sulfur and nitrogen flame retardant components and a synthesis method thereof. Background technique [0002] Flame retardant is one of the important additives of polymer materials. As people's awareness of environmental protection continues to increase, although traditional halogenated flame retardants have high-efficiency flame-retardant properties, they will not only produce a large amount of corrosive gases, smoke, and Dioxin problems when they are burned, they are widely used in many fields. are restricted. Therefore, the development of environmentally friendly and efficient halogen-free flame retardants is an important topic for researchers today. [0003] Intumescent flame retardant (IFR) contains phosphorus, nitrogen and other main flame retardant elements, and also contains rich acid source, carbon source and gas so...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C07F9/6574
Inventor 任元林程博闻刘晓辉刘玉桂康卫民金银山董二莹
Owner TIANJIN POLYTECHNIC UNIV
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