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Preparation method of combustion inhibitor containing P-S

A flame retardant, P-S technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., to achieve the effect of good carbon formation

Inactive Publication Date: 2009-11-25
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a method for preparing a flame retardant containing P-S. The research results of the thermal properties of the flame retardant (CDZR-2) obtained in the present invention show that it has good char formation and is an excellent flame retardant. ; In the synthesis of thiophenylphosphonic dichloride, use the ionic liquid method to avoid catalyst AlCl in the aftertreatment 3 Problems that cannot be removed

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  • Preparation method of combustion inhibitor containing P-S

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Synthesis of CDZR-1;

[0024] To PCl 3 (34.4g, 0.25mol) and [Et 3 NH]Cl-2AlCl 3 (6.3g, 0.0810mol) benzene was added dropwise to the reflux liquid of (2.84g, 7.0mmol), and the reflux reaction was continued at 78-80°C for 3.5h after the addition was completed for 1h. The mixture was cooled to room temperature and allowed to stand for 30 min. The excess PCl was then distilled off under reduced pressure at 40°C 3 . The residual liquid was cooled to 30°C, and sulfur powder (27.2 g, 0.0850 mol) was added in batches to ensure that the reaction temperature was around 80°C. After the addition was complete, the reaction was continued at 80°C for 1.5h. After cooling the reactant, petroleum ether was added and stirred for 30 min. After the stirring was stopped, the solution was separated into layers, the upper layer was the petroleum ether phase, and the lower layer was the ionic liquid phase. Separate and collect the petroleum ether phase, wash with cold water to remove un...

Embodiment 2

[0028] Synthesis of CDZR-1;

[0029] To PCl 3 (37.84g, 0.275mol) and [Et 3 NH]Cl-2AlCl 3 Add (6.5g, 0.0833mol) benzene dropwise to the reflux liquid of (3.08g, 7.6mmol), and continue the reflux reaction at 78-80°C for 4h after the addition is completed for 1h. The mixture was cooled to room temperature and allowed to stand for 30 min. The excess PCl was then distilled off under reduced pressure at 40°C 3 . The residual liquid was cooled to 30°C, and sulfur powder (28.4g, 0.0887mol) was added in batches to ensure that the reaction temperature was around 80°C. After the addition was complete, the reaction was continued at 80°C for 1.5h. After cooling the reactant, petroleum ether was added and stirred for 30 min. After the stirring was stopped, the solution was separated into layers, the upper layer was the petroleum ether phase, and the lower layer was the ionic liquid phase. Separate and collect the petroleum ether phase, wash with cold water to remove unreacted phenyl...

Embodiment 3

[0033] Synthesis of CDZR-1;

[0034] To PCl 3 (41.28g, 0.30mol) and [Et 3 NH]Cl-2AlCl 3 Add (6.68g, 0.0856mol) benzene dropwise to the reflux liquid of (3.24g, 8.0mmol), and continue the reflux reaction at 78-80°C for 4h after the addition is completed for 1h. The mixture was cooled to room temperature and allowed to stand for 30 min. The excess PCl was then distilled off under reduced pressure at 40°C 3 . The residual liquid was cooled to 30°C, and sulfur powder (29.0 g, 0.0906 mol) was added in batches to ensure that the reaction temperature was around 80°C. After the addition was complete, the reaction was continued at 80°C for 1.5h. After cooling the reactant, petroleum ether was added and stirred for 30 min. After the stirring was stopped, the solution was separated into layers, the upper layer was the petroleum ether phase, and the lower layer was the ionic liquid phase. Separate and collect the petroleum ether phase, wash with cold water to remove unreacted phen...

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Abstract

The invention relates to a preparation method of combustion inhibitor containing P-S, which includes the steps: (1) under the nitrogen gas atmosphere, adding triethylamine hydrochloride and anhydrous aluminium chloride, mixing; (2) adding benzene into refluxing liquid of PCl3 and [Et3NH]Cl-2AlCl3 for refluxing reaction; vacuum distilling, and then adding sulphur powder in batches for continue reaction; adding petroleum ether and stirring, separating and collecting petroleum ether phase on upper layer, washing, drying; pressure reducing and steaming petroleum ether; collecting distillate; dispersing pentaerythritol and pyridine in carrene, dropping sulfo-phenylphosphono with stirring for refluxing reaction, after the reaction ends, rotary steaming, water washing and recrystallizating. The combustion inhibitor provided the invention has good char formation.

Description

technical field [0001] The invention belongs to the field of preparation of flame retardants, in particular to a method for preparing a flame retardant containing P-S. Background technique [0002] Halogen flame retardants are currently one of the largest organic flame retardants in the world, with the advantages of high efficiency, wide application range, and sufficient raw materials. Its thermal decomposition products capture a large number of high-energy hydroxyl radicals and hydrogen radicals in the flame zone, reduce their concentration, thereby inhibiting or interrupting the chain reaction of combustion, and play a flame-retardant role in the gas phase [8] . However, the use of this type of flame retardant reduces the anti-ultraviolet stability of the flame-retardant substrate, and generates more smoke, corrosive gases and toxic gases during combustion. Developed countries and regions have banned the use of such flame retardants in large quantities. [0003] Organop...

Claims

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Application Information

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IPC IPC(8): C09K21/12C07F9/6571
Inventor 蔡再生陈国敏丁佩佩沈为宁张灯青杨玉红时达赵亚萍
Owner DONGHUA UNIV
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