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Organic phosphorus-based flame retardant and process for producing the same

A technology of organophosphorus and flame retardants, applied in the field of organophosphorus flame retardants and their preparation, can solve the problems of reduced flame retardant effect and thermal stability, low decomposition temperature, and reduced heat resistance, and achieve excellent dispersion And compatibility, excellent flame retardant effect, high decomposition temperature effect

Active Publication Date: 2012-03-14
ID BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the case of halogen-based flame retardants, although it is easy to ensure flame retardancy, they have the following disadvantages: poor compatibility with resins, generation of carbides due to decomposition caused by retention in the extruder, and generation of carbides during processing and When burning, it will produce harmful toxic gases such as hydrobromic acid, dioxin, and benzofuran
However, the raw materials used in the preparation of the organophosphorus compounds mentioned in the above-mentioned documents are expensive, so it is difficult to use them commercially
[0008] And, U.S. Authorized Patent No. 4,086,206 mentions the reaction of DOPO and formaldehyde to prepare DOPO-formaldehyde, and then carry out polycondensation reaction with melamine to prepare a new method of phosphorus flame retardant, but the above-mentioned documents Organophosphorus compounds still have the problem of reduced flame retardant effect and thermal stability due to low decomposition temperature, and there are also difficulties in commercialization
[0009] Therefore, the actual situation is that further improvement is needed in heat resistance. In order to overcome the problems in the prior art such as poor moisture resistance and heat resistance reduction caused by low decomposition temperature, it is necessary to provide a product with excellent heat resistance. organophosphorus flame retardant

Method used

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  • Organic phosphorus-based flame retardant and process for producing the same
  • Organic phosphorus-based flame retardant and process for producing the same
  • Organic phosphorus-based flame retardant and process for producing the same

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preparation example Construction

[0042]In the preparation method of the organophosphorus flame retardant of the present invention, the HPLC used in the analysis step is Waters 2690 high-performance liquid chromatography of Waters (Waters) Company, and the column adopts cosmosil C18 (4.6×150mm) for analysis. Use 10% methanol aqueous solution (A) and 100% methanol (B) as the mobile phase, use 60% A solution and 40% B solution for 5 minutes for elution, then change to 100% B solution for 15 minutes. eluted, then eluted with 100% B solution, and then analyzed.

[0043] 2. Thermogravimetric analysis (TGA, thermogravimetric analyzer)

[0044] In order to determine the decomposition temperature of organophosphorus flame retardants, TGA 2050 from TA Instruments was used, and the flowing gas was helium. determined.

[0045] 3. Nuclear Magnetic Resonance (NMR, nuclear magnetic resonance)

[0046] For nuclear magnetic resonance analysis, a Germini200 from Varian Company of the United States was used, and DMSO-d6 was ...

Embodiment 1

[0048] 105.1 g of sodium hydroxide (NaOH), 300 g of bisphenol A and 426.6 g of formaldehyde aqueous solution (35%) were added into the reactor, and reacted at 45° C. for 15 hours. Analysis was performed by HPLC during the reaction, and the reaction was terminated when the content of tetramethylol bisphenol A reached 75.2% by weight. Then the above mixture was cooled at room temperature for 1 hour, added to 2L of 1-butanol, and then added dropwise to the hydrochloric acid solution obtained by diluting 35% of 267g of concentrated hydrochloric acid solution with 250g of distilled water to make it acidified, and then extract the product layered. After the upper organic layer was washed with distilled water, 2 kg of the reaction product was obtained.

[0049] HPLC analysis: tetramer-(75.2% by weight), trimer-(6.8% by weight), dimer-(1.6% by weight), monomer-(0.6% by weight), oligomer (15.8% by weight )

[0050] After concentrating 2kg of the above reaction product, add 885g of D...

Embodiment 2

[0059] Add 280.34g of sodium hydroxide (NaOH) aqueous solution (50%), 400g of bisphenol A and 601.3g of formaldehyde aqueous solution (35%) into the reactor, and react at 80°C. Analysis was performed by HPLC, and the reaction was terminated when the content of tetramethylol bisphenol A reached 50% by weight. Then the above mixture was cooled at 10°C for 1 hour, then added to 2L of 1-butanol, and then added dropwise to the hydrochloric acid solution obtained by diluting 35% of 267g of concentrated hydrochloric acid solution with 250g of distilled water to make it acidified, and extracted The product was separated. After the upper organic layer was washed with distilled water, 2 kg of the reaction product was obtained.

[0060] HPLC analysis: tetramer-(56.0% by weight), trimer-(5.0% by weight), dimer-(1.4% by weight), monomer-(0.3% by weight), oligomer (37.3% by weight )

[0061] After 2 kg of the above reaction product was concentrated, 787.9 g of DOPO / 900 mL of 1-methoxy-2-...

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Abstract

The present invention relates to an organic phosphorus-based flame retardant and a process for producing the same, and more particularly, relates to a commercial process for producing an organic phosphorus-based flame retardant comprising: a step of reacting bisphenol A with formaldehyde, a step of extracting reaction products by putting the reactants into organic solvent, and a step of condensation-polymerizing the reaction products by adding phosphine-based or phosphite-based compounds.

Description

technical field [0001] The invention relates to an organic phosphorus flame retardant and a preparation method thereof. The organophosphorus flame retardant is controlled by controlling the content of tetramethylol bisphenol A to 50-90% by weight when bisphenol A and formaldehyde are reacted, so that the obtained organophosphorus flame retardant It has excellent dispersibility and compatibility with various synthetic resins. Due to its high decomposition temperature, it has excellent heat resistance, so it will not decompose even at the processing temperature of synthetic resins. Background technique [0002] Flame retardants generally used in synthetic resins include halogen flame retardants and non-halogen flame retardants. [0003] Halogen-based flame retardants mainly use bromine-based flame retardants containing Australia (Br), which are mixed with metal compounds such as antimony trioxide as auxiliary flame retardants. In the case of halogen-based flame retardants, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/12
CPCC07F9/657172C09K21/12C08K5/0066C08K5/53
Inventor 金晟年张鹤淳金寿赞崔宇爀林富圭
Owner ID BIOCHEM
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