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 indene dihydrogenate is applied in the field of phloroglucinol triphosphate and its preparation, which can solve the problems of high cost and poor flame retardant effect, and achieves low cost and flame retardant effect. Good effect and strong practical effect

Inactive Publication Date: 2011-06-08
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] Clean and dry all the glass instruments used in the experiment. Get 1.10 grams (0.01mol) of catechol and put it into a 250ml three-necked flask, then dissolve the catechol with 5ml of chloroform. Take 5.05 g (0.05 mol) of triethylamine and 4.56 g (0.03 mol) of phosphorus oxychloride respectively in a constant pressure dropping funnel, and slowly drop them into a three-necked flask after heating to 70°C. After the dropwise addition was completed, the reaction was continued for 1 hour. Distillation under reduced pressure was then carried out. Below 65°C, distill under reduced pressure for 30 minutes to remove excess phosphorus oxychloride and add 0.50 g (0.004 mol) of phloroglucinol and 3 ml of chloroform while hot. Then take 3.03 g (0.04 mol) of triethylamine and 3 ml of chloroform in the dropping funnel, slowly add dropwise, control the temperature at 40 degrees, and react for 5 hours. Below 70°C, distill under reduced pressure for 45 minutes until the remaining prod...

Embodiment 2

[0028] Clean and dry all the glass instruments used in the experiment. Get 1.10 grams (0.01mol) of catechol and put it into a 250ml three-necked flask, then dissolve the catechol with 6ml of chloroform. Take 8.08 g (0.08 mol) of triethylamine and 6.84 g (0.045 mol) of phosphorus oxychloride respectively in a constant pressure dropping funnel, heat to 35 degrees and slowly drop them into a three-necked flask. After the dropwise addition was completed, the reaction was continued for 4 hours. Distillation under reduced pressure was then carried out. Below 100°C, distill under reduced pressure for 10 minutes to remove excess phosphorus oxychloride and add 1.26 g (0.01 mol) of phloroglucinol and 4 ml of chloroform while hot. Then take 2.02 g (0.02 mol) of triethylamine and 4 ml of chloroform in the dropping funnel, slowly add dropwise, control the temperature at 60 degrees, and react for 3 hours. The temperature was controlled below 70 degrees, and the distillation under reduced...

Embodiment 3

[0030] Clean and dry all the glass instruments used in the experiment. Get 1.10 grams (0.01mol) of catechol and put it into a 250ml three-necked flask, then dissolve the catechol with 5ml of chloroform. Take 2.02 g (0.02 mol) of triethylamine and 1.672 g (0.011 mol) of phosphorus oxychloride respectively in a constant pressure dropping funnel, and slowly drop them into a three-necked flask at a controlled temperature of 10°C. After the dropwise addition was completed, the reaction was continued for 10 hours. Distillation under reduced pressure was then carried out. Below 65°C, distill under reduced pressure for 30 minutes to remove excess phosphorus oxychloride and add 1.51 g (0.012 mol) of phloroglucinol and 3 ml of chloroform while hot. Then take 4.04 g (0.04 mol) of triethylamine and 5 ml of chloroform in the dropping funnel, slowly add dropwise, control the temperature at 10 degrees, and react for 9 hours. The temperature was controlled below 70 degrees, and the vacuum ...

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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, specifically tris(1,3-dioxa-2-phospha-2-oxo-1,2-dihydroindene) phloroglucinol phosphate and its preparation 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, communications and daily life. Supplies etc. Because most of these synthetic materials are flammable, the fire hazards caused by them have become social problems 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 c...

Claims

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Application Information

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