Intumescent flame retardant containing phosphorus, nitrogen and sulfur and preparation method of intumescent flame retardant

An intumescent flame retardant, nitrogen-sulfur technology, applied in the field of halogen-free flame retardant, can solve the problems of low flame retardant efficiency, single flame retardant element, complex preparation process, etc., to achieve improved flame retardant performance, good water resistance, and preparation The effect of simple method

Inactive Publication Date: 2016-07-27
HEFEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the defects of complex preparation process, single flame retardant element and low flame retardant efficiency in the prior art, and provide a phosphorus, nitrogen and sulfur intumescent flame retardant and its preparation method

Method used

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  • Intumescent flame retardant containing phosphorus, nitrogen and sulfur and preparation method of intumescent flame retardant
  • Intumescent flame retardant containing phosphorus, nitrogen and sulfur and preparation method of intumescent flame retardant
  • Intumescent flame retardant containing phosphorus, nitrogen and sulfur and preparation method of intumescent flame retardant

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Effect test

Embodiment 1

[0021] Put 1.77 g of thiocyanuric acid, 3.04 g of triethylamine and 50 ml of tetrahydrofuran in a three-necked flask. Under the conditions of ice bath and nitrogen, add 7.10 g of diphenylphosphinyl chloride dropwise. The reaction was continued for 1 hour under the bath and nitrogen conditions, then the temperature was raised to 60°C, and the reaction was conducted under nitrogen conditions for 6 hours. Finally, the resulting product was filtered to remove the precipitation and the solvent was removed. The obtained light yellow solid powder is the phosphorus-containing nitrogen-sulfur expansion of the present invention Type flame retardant.

[0022] Attached figure 1 The proton nuclear magnetic resonance spectrum ( 1 HNMR, CDCl 3 , Δ, ppm, TMS), it can be seen that TTCA has a single peak at the chemical shift value of 1.5 ppm, which is attributed to the H of the sulfhydryl (-SH) in TTCA, while the single peak in the hydrogen spectrum of TTC-DPP weakens even The disappearance indic...

Embodiment 2

[0027] Put 1.77 g of thiocyanuric acid, 2.37 g of pyridine and 50 ml of N,N-dimethylformamide in a three-necked flask, and add 7.10 g of diphenylphosphinyl chloride dropwise under ice bath and nitrogen conditions. After the dripping is completed, the reaction is continued for 2 hours under ice bath and nitrogen conditions, then the temperature is raised to 50°C, and the reaction is carried out under nitrogen conditions for 8 hours. Finally, the obtained product is filtered to remove the precipitate and the solvent is removed. The obtained light yellow solid powder is the present invention. Intumescent flame retardant containing phosphorus, nitrogen and sulfur.

Embodiment 3

[0029] Put 1.77 g of thiocyanuric acid, 2.97 g of pyridine and 50 ml of N,N-dimethylformamide in a three-necked flask, add 4.22 g of diethylphosphinyl chloride dropwise under ice bath and nitrogen conditions, After the addition is completed, the reaction is continued for 3 hours under ice bath and nitrogen conditions, then the temperature is raised to 40°C, and the reaction is carried out under nitrogen conditions for 9 hours. Finally, the resulting product is filtered to remove the precipitate and the solvent is removed. The obtained light yellow solid powder is the invention Intumescent flame retardant containing phosphorus, nitrogen and sulfur.

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Abstract

The invention belongs to the technical field of halogen-free flame retarding, and particularly relates to an intumescent flame retardant containing phosphorus, nitrogen and sulfur and a preparation method of the intumescent flame retardant.The molecular structural formula of the flame retardant is as follows (please see the formula in the description), wherein R represents an ethyl group or phenyl group.The preparation method comprises the steps that trithiocyanuric acid is dissolved in organic solvent, an acid binding agent is added, phosphinic chloride is added under the ice bath and nitrogen protecting conditions, reacting continues under the ice bath condition, then reacting under heating is performed under the nitrogen condition, and filtering is performed to remove precipitates and then remove the solvent, wherein the molar ratio of the acid binding agent to phosphinic chloride is (1.0-1.5):1, and the molar ratio of phosphinic chloride to trithiocyanuric acid is 3:1.According to the intumescent flame retardant containing phosphorus, nitrogen and sulfur, the contents of phosphorus, nitrogen and sulfur are all high, phosphorus, nitrogen and sulfur have the synergistic flame retarding effect, therefore, the composite material can quickly promote carbonization of a polymer in the heated or combustion process, oxygen and heat insulation is achieved, and releasing of combustible gas and toxic flue gas is reduced; meanwhile, the flame retardance of the composite material can be further improved by cooperating with a small quantity of a flame retardant synergist.

Description

Technical field [0001] The invention belongs to the technical field of halogen-free flame retardant, and specifically relates to a phosphorus-containing nitrogen-sulfur intumescent flame retardant and a preparation method thereof. Background technique [0002] Polymer materials include plastics, rubber, fibers, films, adhesives and coatings. Among them, plastic, synthetic fiber and synthetic rubber, which are called the three major synthetic materials of modern polymers, have become important materials indispensable for the construction of the national economy and people's daily lives. However, most of the polymer materials are combustible, and the polymer materials will generate a large amount of smoke and toxic gases during the heating or burning process, which makes their application areas more restricted. At present, the flame retardants used in polymer materials are mainly halogen-containing systems. Although halogen-containing flame retardants have high flame retardant eff...

Claims

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Application Information

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IPC IPC(8): C07F9/6521C08K5/5398
CPCC07F9/6521C08K5/5398
Inventor 杨伟胡琪杭赵申鲁红典杨本宏
Owner HEFEI UNIV
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