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A kind of flame retardant dihydric alcohol containing phosphaphenanthrene group and preparation method thereof

A phosphaphenanthrene group, diol technology, applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc. Structural asymmetry, etc.

Active Publication Date: 2017-05-17
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a flame-retardant diol containing a phosphaphenanthrene group and a preparation method thereof, which utilizes the active P-H bond in DOPO to undergo an addition reaction with an acrylic ketal ester containing a double bond and then hydrolyzes it. , to prepare flame-retardant diols containing phosphaphenanthrene groups to solve the problems of few types of flame-retardant compounds containing dihydroxyl groups, asymmetric hydroxyl structures, and low reactivity

Method used

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  • A kind of flame retardant dihydric alcohol containing phosphaphenanthrene group and preparation method thereof
  • A kind of flame retardant dihydric alcohol containing phosphaphenanthrene group and preparation method thereof
  • A kind of flame retardant dihydric alcohol containing phosphaphenanthrene group and preparation method thereof

Examples

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Effect test

Embodiment 1

[0020] Embodiment 1: Preparation of flame retardant dihydric alcohol DDOPO

[0021] Add 5 grams of DOPO and 4.3 grams of MEDB into a 500mL three-necked flask, and then add 50mL of toluene as a solvent and 0.03 grams of triethylamine as a catalyst. The reaction system is stirred and heated to 110°C for 24 hours to stop the reaction; wait for the system to cool After reaching room temperature, the product A was obtained by precipitation, filtration, and drying; the product A was then transferred to a 500mL three-necked flask, and a mixed solution of 20mL tetrahydrofuran and 1M hydrochloric acid in a volume ratio of 1:1 was added dropwise, and the reaction was carried out at room temperature for 1 hour Afterwards, tetrahydrofuran and water are removed after vacuum distillation, and the product is a flame-retardant diol 10-(dimethylolpropionate ethyl)-9,10-dihydro-9-oxygen with a symmetrical hydroxyl structure. Hetero-10-phosphaphenanthrene-10-oxide DDOPO; 85% yield.

[0022] att...

Embodiment 2

[0024] Example 2: Application of the flame retardant diol DDOPO prepared by the present invention

[0025] 51 grams of polyadipate-1,4-butylene glycol ester diol (PBA, M n =3200) into a 500mL three-neck flask, dehydrated at 115°C for 1 hour and then cooled to 50°C. Take 22.4 grams of toluene diisocyanate (TDI) into a three-necked flask, stir and react at 80°C for 3 hours, then add 5.6 grams of 1,4-butanediol (BDO), 23 grams of the flame-retardant diol prepared in the above examples DDOPO, 0.01 g of dibutyltin dilaurate and 50 g of N,N-dimethylformamide were stirred and reacted at a constant temperature of 75°C for 4 hours, and then the solvent was distilled off under reduced pressure to prepare phosphorus-based intrinsically flame-retardant polyurethane PU-A.

[0026] For ease of comparison with common polyurethanes without phosphaphenanthrene groups, 51 grams of PBA (M n =3200) into a 500mL three-neck flask, dehydrated at 115°C for 1 hour and then cooled to 50°C. Add 22.4 ...

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Abstract

The invention discloses phosphaphenanthrene group-containing flame retardant dihydric alcohol and a preparation method thereof. The preparation method is characterized by comprising the following steps: carrying out addition reaction on reactive bonds P-H in a 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and double bond-containing acrylate ketal; and hydrolyzing to prepare a reaction type phosphorus flame retardant dihydric alcohol 10-(dimethylolpropionic carbethoxy)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide which has symmetric hydroxyl structures and has a phosphaphenanthrene group. According to the preparation method, the micro molecular dihydric alcohol which is frequently used in the synthesis of polymers such as polyester, polycarbonate, polyether, polyether ester and polyurethane is introduced into the phosphaphenanthrene group through a chemical bonding manner so that the molecular structure of the obtained dihydric alcohol not only has the phosphaphenanthrene group, but also has two symmetric hydroxyl structures with same reaction activity, the micro molecular dihydric alcohol without the inflaming retarding characteristic can be partially or completely replaced and the prepared polymer material has flame retarding characteristic.

Description

technical field [0001] The invention belongs to the technical field of flame retardant compounds, in particular to a flame retardant diol 10-(dimethylol propionate ethyl)-9,10-dihydro-9-oxa-10 containing a phosphaphenanthrene group - Phosphaphenanthrene-10-oxide (DDOPO) and process for its preparation. Background technique [0002] When the organophosphorus flame retardant is decomposed by heat, its product generally has a strong dehydration effect, which can quickly carbonize the surface of the covered organic matter and form a carbon film, so that it has a good flame retardant effect. This type of flame retardant can solve the problems of large smoke and release of toxic and corrosive gases when halogen flame retardants are burned, and can also overcome the shortcomings of the large amount of inorganic flame retardants that easily affect the physical and mechanical properties of materials. The phosphaphenanthrene group has the characteristics of heterocyclic phosphorus-co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6571C08G18/76C08G18/66C08G18/42C08G18/32
Inventor 张兴元贺晨李军配徐路路
Owner UNIV OF SCI & TECH OF CHINA