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Poly-phosphate flame retardant containing DOPO side-chain structure and preparation method thereof

A technology of polyphosphate ester and flame retardant, which is applied in the field of polymeric organic phosphorus flame retardant structure and its preparation, can solve the problems of poor droplet resistance of flame retardants, and achieve easy control, simple preparation method, and cost-effectiveness. good charcoal effect

Inactive Publication Date: 2012-07-04
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the experimental results show that the use of flame retardants containing DOPO structures alone has poor droplet resistance

Method used

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  • Poly-phosphate flame retardant containing DOPO side-chain structure and preparation method thereof
  • Poly-phosphate flame retardant containing DOPO side-chain structure and preparation method thereof
  • Poly-phosphate flame retardant containing DOPO side-chain structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve DOPO216g (1mol) in 600mL ethanol and heat to 70°C, add 90mL of 37% formaldehyde solution within 30min, then reflux for 4h, cool and crystallize, filter and dry to obtain intermediate I. The reaction equation is as follows:

[0026]

Embodiment 2

[0028] Add 24.6 g (0.1 mol) of intermediate I containing DOPO structure and phosphorus oxychloride into the reactor at a molar ratio of 1 / 15, stir at 60° C. under nitrogen protection, and react for 2 hours. After the reaction is over, remove excess phosphorus oxychloride by distillation to obtain reaction intermediate II; add 25g (0.1mol) of bisphenol S into the reactor, heat and stir under nitrogen flow, and then gradually increase the temperature (ΔT=20°C / h) , raised the temperature from 120°C to 220°C, kept at 220°C for 4 hours to ensure that the reaction degree was higher than 0.95, and the product was obtained after cooling. The reaction equation is as follows:

[0029]

[0030] Theoretical phosphorus content: 11.5%; Theoretical sulfur content: 5.9%.

[0031] The TGA and DTG curves of the flame retardant are shown in figure 1 , the chemical structure is given by 1 H-NMR and 31 P-NMR characterization is shown in Figure 2.

Embodiment 3

[0033] Add 36.3g (0.1mol) of reaction intermediate II and 22.8g (0.1mol) of bisphenol A into the reactor, heat and stir under nitrogen flow, then gradually increase the temperature (ΔT=20°C / h), from 120°C to 220°C °C, keep the temperature at 220 °C for 4 hours to ensure that the reaction degree is higher than 0.95, and the product is obtained after cooling. The reaction equation is as follows:

[0034]

[0035] Theoretical phosphorus content: 12.0%.

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Abstract

The invention discloses a poly-phosphate flame retardant containing a DOPO side-chain structure and a preparation method thereof, belonging to the technical field of polymeric organic phosphorus flame retardant structures and the preparation method thereof. The flame retardant is characterized by comprising the following repeating unit structure: wherein n=5-50. The preparation method of the poly-phosphate flame retardant comprises the following steps of: reacting an intermediate I containing the DOPO structure with phosphorus oxychloride to obtain an intermediate II containing phosphorus oxychloride, and fusing and polymerizing the intermediate II and a bisphenol compound to obtain the poly-phosphate flame retardant containing the DOPO side-chain structure. The preparation method is simple, and through adjusting Ar categories and ratios, the phosphorus content can be controlled at 11.5-15.5% and the sulfur content can be controlled at 0-5.9%. The flame retardant has the characteristics of favorable thermal stability, high decomposition temperature, favorable char-forming property, and the like, and can be used for flame retardance modification of materials, such as polyester, polyamide, polycarbonate and blends thereof, and the like, with higher processing temperature.

Description

technical field [0001] The invention belongs to the technical field of polymeric organophosphorus flame retardant structures and preparation methods thereof, and relates to polyphosphate ester flame retardant structures containing DOPO side chain structures and preparation methods thereof. Background technique [0002] With the rapid development of synthetic materials, synthetic plastics, rubber, and fibers are more and more used in various sectors of the national economy and people's production and life, but at the same time, fires caused by ignition of high polymers are also Therefore, people have higher and higher requirements for the flame retardant properties of synthetic materials. Especially in the high-tech field, people not only require flame-retardant materials to have satisfactory flame-retardant properties, but also require materials to have good physical and mechanical properties and electrical properties, processing fluidity, easy recycling of flame-retardant m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6571
Inventor 郑玉斌闫莉郑楠
Owner DALIAN UNIV OF TECH