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Reaction type phosphorus-nitrogen fire retardant and preparation method thereof

A phosphorus-nitrogen flame retardant and reactive technology, applied in the field of reactive phosphorus-nitrogen flame retardants and their preparation, can solve the problem of poor compatibility between small molecule flame retardants and polymers, affecting the mechanical properties of substrates and bonding methods Complicated issues

Active Publication Date: 2012-12-12
THE SECOND RES INST OF CIVIL AVIATION ADMINISTRATION OF CHINA +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0023] (where R is a partially acrylated or partially methacrylated functional group; R' is a nitrogen-containing functional group with two tertiary or secondary amines) because the reactive group in its structure has an active double bond of the R part and The secondary amino group of the R' part, in which the active double bond can only be inserted into the curable resin matrix through ultraviolet radiation, so the bonding process is also relatively complicated and not easy to industrialize
[0024] In addition, since the additive-type flame retardant disclosed above is mixed with the matrix in a physical way, it is easy for the flame retardant to migrate out of the matrix over time, which reduces the flame-retardant grade of the flame-retardant material, and the small-molecule flame retardant and The compatibility of polymers is generally poor, which will affect the mechanical properties of the substrate and affect the use in specific fields
Compared with additive flame retardants, although reactive flame retardants have reactive groups, they can react with monomers or prepolymers, and embed the flame retardant compound structure into the polymer chain, not only does the flame retardant element not migrate, The flame retardant performance is long-lasting, and the problem of compatibility difference can be overcome, and the influence on the mechanical properties of the substrate is small. However, the three reactive phosphorus-nitrogen flame retardants disclosed in the above prior art are not satisfactory, and all of them have reactive groups. Disadvantages of low activity or complex chemical bonding with polymers

Method used

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  • Reaction type phosphorus-nitrogen fire retardant and preparation method thereof
  • Reaction type phosphorus-nitrogen fire retardant and preparation method thereof
  • Reaction type phosphorus-nitrogen fire retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0076] First, 47.4g (0.44mol) of benzaldehyde and 64.0g (0.88mol) of isobutyraldehyde were stirred and mixed, and 24.8g (0.44mol) of potassium hydroxide was dissolved in 400ml of ethanol and slowly added dropwise to the system through a dropping funnel. The reaction is exothermic. When the temperature reaches 70℃, the dripping is stopped. When the temperature of the system is quickly cooled to 50℃ with a water bath, the ethanol solution of potassium hydroxide is added rapidly. After the dripping is completed, the system is heated and kept at 50-60℃ React for 5 hours. After the reaction was completed, the yellow viscous crude product was obtained by rotary evaporation, which was extracted with chloroform / water system. The obtained chloroform layer was dried with anhydrous magnesium sulfate. After drying, the clear liquid was rotary evaporated to remove chloroform, and recrystallized with toluene / n-hexane system to obtain 61.0 g (0.34mol) 1-phenyl-2,2-dimethyl-1,3-propanediol.

[...

Embodiment 2

[0079] The operation steps for the synthesis of 1-phenyl-2,2-dimethyl-1,3-propanediol used in this example are the same as in Example 1. Add 36.0g (0.20mol) of 1-phenyl-2,2-dimethyl-1,3-propanediol to 200ml of xylene to dissolve it, and then slowly add 19.9g (0.13) dropwise through a constant pressure funnel while stirring at room temperature. mol) Phosphorus oxychloride, the hydrogen chloride gas generated by the reaction is absorbed by sodium bicarbonate aqueous solution, and after the dripping is completed, the temperature is raised to 75°C to react for 2h. After the reaction is completed, the xylene is removed by rotary evaporation, and the obtained solids are respectively n-hexane and anhydrous ether After successive washing, 23.4 g (0.09 mol) of 4-phenyl-5,5-dimethyl-1,3,2-dioxacaprolactone phosphoryl chloride was obtained. Dissolve 23.4g (0.09mol) of 4-phenyl-5,5-dimethyl-1,3,2-dioxacaprolone phosphoryl chloride in 150ml of acetonitrile, and then take 9.7g (0.10mol) of t...

Embodiment 3

[0081] The operation steps for the synthesis of 1-phenyl-2,2-dimethyl-1,3-propanediol used in this example are the same as in Example 1. Add 36.0g (0.20mol) of 1-phenyl-2,2-dimethyl-1,3-propanediol to 200ml of acetone to dissolve it, and then add 21.4g (0.14mol) slowly through a constant pressure funnel while stirring at room temperature ) Phosphorus oxychloride, the hydrogen chloride gas generated by the reaction is absorbed with sodium bicarbonate aqueous solution, after the dripping is completed, the temperature is raised to 56°C for 3 hours, and the acetone is removed by rotary evaporation after the reaction. Then 28.6 g (0.11 mol) of 4-phenyl-5,5-dimethyl-1,3,2-dioxacaprolactone phosphoryl chloride was obtained. Dissolve 28.6g (0.11mol) of 4-phenyl-5,5-dimethyl-1,3,2-dioxacaprolone phosphoryl chloride in 150ml of acetone, and then take 11.6g (0.12mol) of thiocyanate Potassium is dissolved in 50ml of acetone, then the temperature is raised to 53℃, and the dissolved potassi...

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Abstract

The invention discloses a reaction type phosphorus-nitrogen fire retardant which has the structural general formula shown in the specification, wherein in the formula (1), R1 is hydrogen atom or phenyl; R2 is oxygen atom or sulphur atom; R3 is nitrogen-containing compounds; and the compounds have one primary amine group and two hydroxyls, the primary amine group and the isothiocyano (-NCS) are reacted with each other, and the two hydroxyls can be used for the follow-up reactive group with a polymer monomer. The invention further discloses a preparation method of the reaction type phosphorus-nitrogen fire retardant. The fire retardant provided by the invention not only can integrate an acid source, a carbon source and a gas source, but also has the two hydroxyls which are very high in reactivity, so that the structure of the fire retardant can be very easily embedded into a polymer chain due to the chemical bonding, the problems caused by the initiator or the optical radiation means adopted in the prior art can be avoided, the effects of the expansion type fire retardant can be well played, and the anti-flaming effect of the high molecular material can be greatly improved. The preparation method is simple and mature, easy in operation, low in reaction temperature, and energy-saving.

Description

Technical field [0001] The invention belongs to the technical field of phosphorus-nitrogen flame retardants and their preparation, and specifically relates to a novel reactive phosphorus-nitrogen flame retardant and a preparation method thereof. Background technique [0002] After the 1950s, the polymer material industry began to develop, but fires caused by the flammability of polymer materials brought people property losses and life-threatening safety. Flame retardant modification of polymer materials became a technology One of the important topics for workers' research. [0003] Traditional flame retardants are halogen-based flame retardants (especially bromine-based) and synergistic flame retardants mixed with halogen-based and other synergistic agents. However, brominated flame-retardant systems are prone to generate more smoke during the combustion process. Corrosive and toxic gases are gradually restricted and prohibited. The halogen-free flame retardant system has gradual...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C08G18/32
Inventor 夏祖西李洁华苏正良陈业中彭华乔谭鸿
Owner THE SECOND RES INST OF CIVIL AVIATION ADMINISTRATION OF CHINA
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