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A kind of calixarene-containing module and cyclic phosphate flame retardant and its preparation method and application

A technology of cyclic phosphate ester and calixarene, which is applied in the field of flame retardants, can solve the problems of lack of phosphorus-based flame retardants, achieve high flame retardant efficiency, high thermal stability, and improve flame retardant performance

Active Publication Date: 2019-09-24
CHINESE PEOPLES ARMED POLICE FORCE ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no relevant record about phosphorus-based flame retardants containing calixarene modules in the prior art

Method used

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  • A kind of calixarene-containing module and cyclic phosphate flame retardant and its preparation method and application
  • A kind of calixarene-containing module and cyclic phosphate flame retardant and its preparation method and application
  • A kind of calixarene-containing module and cyclic phosphate flame retardant and its preparation method and application

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preparation example Construction

[0028] The present invention also provides a method for preparing the calixarene-containing module and the cyclic phosphate ester flame retardant described in the above technical scheme, comprising the following steps:

[0029] In an inert gas, a compound containing a calixarene module having a structure shown in formula R1, a cyclic phosphate ester having a structure shown in formula R2, a catalyst and an organic solvent are dechlorinated in an ice-water bath to obtain a compound having a structure shown in formula I Calixarene-containing module and cyclic phosphate flame retardant with the structure shown;

[0030]

[0031] In formula R1, X is -NH 2 or -CH 2 OH; Z in the formula R2 is -CH 3 or -CH 2 Br.

[0032] In the present invention, the structural formula of the compound containing the calixarene module having the structure shown in formula R1 is as follows:

[0033]

[0034] In the present invention, the structural formula of the cyclic phosphate ester havin...

Embodiment 1

[0056] Take 0.01 mol of structure 1 and 0.04 mol of structure 3 into a three-necked flask, protect it with nitrogen, and dissolve it in 200 mL of dichloromethane with magnetic stirring, and put it in an ice-water bath. Slowly add triethylamine dropwise to the three-necked flask under ice-bath conditions. During the dropwise addition process, white mist will be generated. Raise the temperature to 40°C and keep stirring at this temperature for 8 hours. The reaction solution was washed three times with saturated sodium chloride solution, added with anhydrous magnesium sulfate and left to dry, filtered after clarification, and the solvent was removed by vacuum suspension evaporation to obtain orange-red crystals containing calixarene modules and cyclic phosphate flame retardants, producing The rate is 85.39%.

[0057] The calixarene-containing module and cyclic phosphate flame retardant were characterized, and the H NMR spectrogram data are as follows, 1 H-NMR (CDCl 3 , δ / ppm): ...

Embodiment 2

[0060] Take 0.04 mol of structure 2 and 0.01 mol of structure 3 into a three-necked flask, nitrogen protection, magnetically stir and dissolve in 200mL chloroform, ice-water bath, slowly drop triethylamine into the three-necked flask under ice-bath conditions, during the dropping process It will be accompanied by the generation of white mist, the temperature is raised to 50°C, and the temperature is maintained for 8 hours with continuous stirring. The reaction solution was washed three times with saturated sodium chloride solution, added with anhydrous calcium carbonate and left to dry, filtered after clarification, and the solvent was removed by vacuum suspension evaporation to obtain orange-red crystals containing calixarene modules and cyclic phosphate flame retardants, producing The rate is 81.28%.

[0061] Mix 750g of polypropylene and 250g of the calixarene-containing module and cyclic phosphate flame retardant prepared above, and mix evenly; then add it to a twin-screw ...

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Abstract

The invention provides a calixarene-containing module and a cyclic phosphate flame retardant, belonging to the technical field of flame retardants. In the present invention, the calixarene module and the cyclic phosphate have higher thermal stability and can improve the flame retardancy of the high polymer material. The data of the embodiment shows that the calixarene-containing module and the cyclic phosphate flame retardant provided by the present invention have higher flame retardant efficiency, and when used in high polymers, using 30wt% of the flame retardant can make The limiting oxygen index (LOI) of polypropylene increased from 19 to 31.5.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a calixarene-containing module and cyclic phosphate flame retardant as well as its preparation method and application. Background technique [0002] With the improvement of technology, polymer materials are widely used in various fields of industry and life due to their excellent performance and low cost. Polymers are everywhere, from plastic products for food and clothing, to transportation and construction industries for housing, to aviation and military fields related to national defense forces. However, most polymer materials are extremely flammable, causing immeasurable losses to human property and life and health. Therefore, it is imminent to improve the flame retardancy of polymers. [0003] Phosphorus-based flame retardants have high flame retardant efficiency, and the flame retardant performance of the flame retardant system with a unit phosphorus content is be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/527C08L63/10C08L23/12
Inventor 卢林刚王会娅钱小东杨守生金静
Owner CHINESE PEOPLES ARMED POLICE FORCE ACAD