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A kind of spirocyclic phosphate flame retardant containing s-triazine structure, preparation method and application thereof

A technology of spirocyclic phosphate and flame retardant, which is applied in the field of phosphorus-nitrogen synergistic flame-retardant compounds, can solve the problem of high price of spirocyclic phosphate, and achieve the effects of good thermal stability, high phosphorus content, and advanced technology

Inactive Publication Date: 2017-08-29
湖北万锦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to overcome the weak point in the above-mentioned prior art, provide a kind of technique simple, production cost is low, overcome the shortcoming that spirocyclic phosphate price is high, synthesize intermediate IV (spirophosphoric acid ester) by reaction of phosphorus oxychloride and pentaerythritol Cyclic phosphate dichloride), using cyanuric chloride, phenol, and p-hydroxybenzaldehyde to prepare intermediate III, which reacts with intermediate IV to form a combination of acid source, carbon source, and gas source. The flame retardant performance is excellent Novel spirocyclic phosphate flame retardant containing bistriazine structure

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  • A kind of spirocyclic phosphate flame retardant containing s-triazine structure, preparation method and application thereof
  • A kind of spirocyclic phosphate flame retardant containing s-triazine structure, preparation method and application thereof
  • A kind of spirocyclic phosphate flame retardant containing s-triazine structure, preparation method and application thereof

Examples

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Embodiment 1

[0034] A preparation method containing s-triazine and spirocyclic phosphate flame retardant, the steps are:

[0035] Add 18.80g (0.20mol) of phenol, 8.00g (0.20mol) of sodium hydroxide and 300mL of water into the flask, and stir for 30min at room temperature. In another flask, add 18.55g (0.10mol) cyanuric chloride, 100mL acetone-water mixed solution (V 丙酮 :V 水 =1:1). Slowly add the prepared sodium phenate solution into the cyanuric chloride solution dropwise, control the temperature at about 5°C, and keep the temperature for 1 hour after the dropwise addition is completed. Raise the temperature to 25-30°C, react for 2 hours, then raise the temperature to 50°C for 12h. After the reaction, the reaction solution was poured into 500 mL of ice water, and a large amount of white solid was precipitated, which was filtered by suction and dried to obtain Intermediate I with a yield of 90.5%.

[0036] Add 30.0g (0.1mol) of intermediate I, 18.30g (0.15mol) of p-hydroxybenzaldehyde, ...

Embodiment 2

[0047] A preparation method containing s-triazine and spirocyclic phosphate flame retardant, the steps are:

[0048] Add 18.80g (0.20mol) of phenol, 8.00g (0.20mol) of sodium hydroxide and 300mL of water into the flask, and stir for 30min at room temperature. In another flask, add 18.55g (0.10mol) cyanuric chloride, 100mL acetone-water mixed solution (V 丙酮 :V 水 =1:1). Slowly add the prepared sodium phenate solution into the cyanuric chloride solution dropwise, control the temperature at about 5°C, and keep the temperature for 1 hour after the dropwise addition is completed. Raise the temperature to 25-30°C, react for 2 hours, then raise the temperature to 50°C for 12h. After the reaction, the reaction solution was poured into 500 mL of ice water, and a large amount of white solid was precipitated, which was filtered by suction and dried to obtain Intermediate I with a yield of 90.5%.

[0049] Add 30.0g (0.1mol) of intermediate I, 18.30g (0.15mol) of p-hydroxybenzaldehyde, ...

Embodiment 3

[0055] The acid-binding agent triethylamine was replaced by N,N-dimethylaniline, and the others were the same as Example 1, and the yield of the target compound was 80.1%.

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Abstract

The invention discloses a preparation method and application of a spirocyclic phosphate flame retardant with an S-triazine structure. The preparation method comprises the steps of reacting sodium phenolate and cyanuric chloride under the action of an acetone-water solution to generate an intermediate I; reacting the intermediate I and p-hydroxy benzaldehyde to obtain an intermediate II; reducing the intermediate II through sodium borohydride to obtain an intermediate III; and finally, reacting the intermediate III and an intermediate IV (spirocyclic pentaerythritol diphosphate phosphorus chloride) to obtain the spirocyclic phosphate flame retardant with the S-triazine structure, wherein the appearance of the spirocyclic phosphate flame retardant is white solid powder. The initial decomposition temperature of the flame retardant is about 345 DEG C, the weight loss at the temperature of 400 DEG C is 10%, the carbon residual rate of the flame retardant at the temperature of 700 DEG C is up to 56%, the flame retardant is relatively good in thermal stability and high in carbon residual rate, and the flame retardant not only can be used as a reactive-type flame retardant to be connected to thermosetting resin such as epoxy resin, but also can be used as an additive-type flame retardant to meet the halogen-free and flame retardant requirements of ABS with a relatively high heat resistant requirement for the flame retardant.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-nitrogen synergistic flame-retardant compounds, and specifically relates to a spirocyclic phosphate flame retardant containing a bistriazine structure. The flame retardant can be used as a reactive flame retardant to prepare a halogen-free flame-retardant resin. It can also be used as an additive flame retardant in the halogen-free flame retardant of engineering plastics. Background technique [0002] When traditional halogen-containing flame-retardant materials burn, there are secondary hazards such as smoke, toxic or corrosive gas emissions, which pose a serious threat to personal safety. Triazine derivatives are a large class of compounds rich in tertiary nitrogen structures, which have the advantages of being halogen-free, low toxicity, high decomposition temperature, little effect on the physical and mechanical properties of materials, anti-bleeding, and high flame retardant efficiency. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/527C07F9/6574C08L63/00C08L55/02
Inventor 李德江刘义稳谢益碧
Owner 湖北万锦科技有限公司