Novel fire retardant tri(1,3-dioxa-2-phospho hetero-2-oxo-1,2-indane) m-cresyl phosphate and preparation method thereof

A technology of phloroglucinol phosphate and indane, which is applied in the field of phloroglucinol triphosphate and its preparation, can solve the problems of poor flame retardant effect and high cost, and achieve good flame retardant effect and low cost. Inexpensive, good degradability effect

Inactive Publication Date: 2013-05-15
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cost of most of the existing halogen-free phosphorus-containing flame retardants is relatively high, and the flame retardant effect is not very good.

Method used

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  • Novel fire retardant tri(1,3-dioxa-2-phospho hetero-2-oxo-1,2-indane) m-cresyl phosphate and preparation method thereof
  • Novel fire retardant tri(1,3-dioxa-2-phospho hetero-2-oxo-1,2-indane) m-cresyl phosphate and preparation method thereof
  • Novel fire retardant tri(1,3-dioxa-2-phospho hetero-2-oxo-1,2-indane) m-cresyl phosphate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] All glassware used in the experiment was cleaned and dried. Put 1.10 g (0.01 mol) of catechol into a 250 ml three-necked flask, and then dissolve catechol with 5 ml of chloroform. 5.05 g (0.05 mol) of triethylamine and 4.56 g (0.03 mol) of phosphorus oxychloride were respectively placed in a constant-pressure dropping funnel, and slowly added dropwise to the three-necked flask after being heated to 70 degrees. After the dropwise addition was completed, the reaction was continued for 1 hour. Then, distillation under reduced pressure was carried out. Below 65 degrees, vacuum distillation was performed for 30 minutes to remove excess phosphorus oxychloride, and then 0.50 g (0.004 mol) of phloroglucinol and 3 ml of chloroform were added while hot. Then take 3.03 g (0.04 mol) of triethylamine and 3 ml of chloroform into the dropping funnel, slowly add it dropwise, control the temperature at 40 degrees, and react for 5 hours. Below 70 degrees, vacuum distillation was perfo...

Embodiment 2

[0028] All glassware used in the experiment was cleaned and dried. 1.10 g (0.01 mol) of catechol was put into a 250 ml three-necked flask, and then 6 ml of chloroform was used to dissolve catechol. Take 8.08 g (0.08 mol) of triethylamine and 6.84 g (0.045 mol) of phosphorus oxychloride and place them in a constant pressure dropping funnel, respectively, and add the temperature to the three-necked flask slowly dropwise at 35 degrees. After the dropwise addition, the reaction was continued for 4 hours. Then, distillation under reduced pressure was carried out. Below 100 degrees, vacuum distillation was performed for 10 minutes to remove excess phosphorus oxychloride, and then 1.26 g (0.01 mol) of phloroglucinol and 4 ml of chloroform were added while hot. Then take 2.02 g (0.02 mol) of triethylamine and 4 ml of chloroform into the dropping funnel, slowly add it dropwise, control the temperature at 60 degrees, and react for 3 hours. The temperature was controlled below 70 degr...

Embodiment 3

[0030] All glassware used in the experiment was cleaned and dried. Put 1.10 g (0.01 mol) of catechol into a 250 ml three-necked flask, and then dissolve catechol with 5 ml of chloroform. Take 2.02 g (0.02 mol) of triethylamine and 1.672 g (0.011 mol) of phosphorus oxychloride and place them in a constant pressure dropping funnel, respectively, and slowly add dropwise to the three-necked flask at a temperature of 10 degrees. After the dropwise addition was completed, the reaction was continued for 10 hours. Then, distillation under reduced pressure was carried out. Below 65 degrees, vacuum distillation was performed for 30 minutes to remove excess phosphorus oxychloride, and then 1.51 g (0.012 mol) of phloroglucinol and 3 ml of chloroform were added while hot. Then take 4.04 g (0.04 mol) of triethylamine and 5 ml of chloroform into the dropping funnel, slowly drop it, control the temperature at 10 degrees, and react for 9 hours. The temperature was controlled below 70 degree...

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Abstract

The invention provides a novel fire retardant tri(1,3-dioxa-2-phospho hetero-2-oxo-1,2-indane) m-cresyl phosphate and a preparation method thereof. The novel fire retardant is characterized in that the structural formula of the novel fire retardant is shown in a formula I. By using the preparation method, the novel halogen-free phosphorus fire retardant is synthesized, the novel halogen-free phosphorus fire retardant has the advantages of good antiflaming effect, environment friendliness and no pollution as well as good degradability. Simultaneously, the fire retardant is simple and availablein raw material, is low in cost, and has strong practicability.

Description

technical field [0001] The invention relates to the field of flame retardant synthesis, in particular to tris(1,3-dioxa-2-phospha-2-oxo-1,2-dihydroindene) phloroglucinol phosphate and preparation thereof method. Background technique [0002] With the continuous development and upgrading of science and technology and the continuous improvement of people's living standards, chemical plastic products and organic polymer materials are more and more widely used in various fields of life, such as construction, transportation, electronics, communication and daily life. supplies, etc. Since most of these synthetic materials are flammable, the resulting fire hazard has become a social problem that cannot be ignored. At this stage, people mainly solve such problems by reducing their flammability and slowing down their burning speed, so as to reduce or even eliminate fire hazards as much as possible, which expands a huge space for the use of flame retardants. Flame retardants are ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/527C08L21/00
Inventor 胡思泉刘继延
Owner JIANGHAN UNIVERSITY
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