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Synthesis of nitrogen and sulfur-containing synergistic flame retardant compound and preparation method of intercalated modified hydrotalcite thereof

A technology of synergistic flame retardant and synthesis method, which is applied in the fields of dyeing low-molecular organic compound treatment, organic chemistry, and fibrous fillers. It can solve the problems that the preparation method of composite flame retardant materials has not been reported, and achieve good application value and improve Dispersion, the effect of simple and easy preparation

Active Publication Date: 2019-08-09
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation method of composite flame-retardant materials based on nitrogen-containing sulfur and hydrotalcite has not been reported yet.

Method used

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  • Synthesis of nitrogen and sulfur-containing synergistic flame retardant compound and preparation method of intercalated modified hydrotalcite thereof
  • Synthesis of nitrogen and sulfur-containing synergistic flame retardant compound and preparation method of intercalated modified hydrotalcite thereof
  • Synthesis of nitrogen and sulfur-containing synergistic flame retardant compound and preparation method of intercalated modified hydrotalcite thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 7.52g of dimethylamine water and mix it with 100mL of toluene. Take 9.22g of cyanuric chloride and mix it with 50mL of toluene. Add the above two solutions dropwise into a beaker, and react at 0-5°C for 2h. With hydrochloric acid, NaHCO 3 , washed with deionized water, and rotary evaporated, and the obtained solid was recrystallized with n-hexane, filtered with suction, and dried to obtain a triazine monosubstituted product (NN).

[0036] Take 0.8gNN, 2.1g anhydrous Na 2 SO 4 , and stir well with 100mL 1,4-dioxane in the flask. Dissolve 1.25g of taurine in 50mL of water, drop the taurine solution into the flask, and heat to 60°C for 6h. Rotary steaming, then add 100mL deionized water to the beaker, react at 90°C for 48 hours, rotary steaming, recrystallize the solid with ultrapure water, suction filter, dry to obtain nitrogen-sulfur synergistic flame retardant compound (NNS), the reaction formula is as follows:

[0037]

[0038] Accurately weigh Mg(NO 3 )...

Embodiment 2

[0042] Take 7.52g of dimethylamine water and mix it with 100mL of toluene. Take 9.22g of cyanuric chloride and mix it with 50mL of toluene. Add the above two solutions dropwise into a beaker, and react at 0-5°C for 2h. With hydrochloric acid, NaHCO 3 , washed with deionized water, and rotary evaporated, and the obtained solid was recrystallized with n-hexane, filtered with suction, and dried to obtain a triazine monosubstituted product (NN).

[0043] Take 0.8gNN, 2.1g anhydrous Na 2 SO 4 , and stir well with 100mL 1,4-dioxane in the flask. Dissolve 1.25g of taurine in 50mL of water, drop the taurine solution into the flask, and heat to 60°C for 6h. Rotary evaporation, then add 100mL deionized water to the beaker, react at 90°C for 48h, rotary evaporation, recrystallize the solid with ultrapure water, suction filter, and dry to obtain the nitrogen-sulfur synergistic flame retardant compound (NNS).

[0044] Accurately weigh Zn(NO 3 ) 2 ·6H 2 O and Fe(NO 3 ) 3 9H 2 O ...

Embodiment 3

[0048] Take 7.52g of dimethylamine water and mix it with 100mL of toluene. Take 9.22g of cyanuric chloride and mix it with 50mL of toluene. Add the above two solutions dropwise into a beaker, and react at 0-5°C for 2h. With hydrochloric acid, NaHCO 3 , washed with deionized water, and rotary evaporated, and the obtained solid was recrystallized with n-hexane, filtered with suction, and dried to obtain a triazine monosubstituted product (NN).

[0049] Take 0.8gNN, 2.1g anhydrous Na 2 SO 4 , and stir well with 100mL 1,4-dioxane in the flask. Dissolve 1.25g of taurine in 50mL of water, drop the taurine solution into the flask, and heat to 60°C for 6h. Rotary evaporation, then add 100mL deionized water to the beaker, react at 90°C for 48h, rotary evaporation, recrystallize the solid with ultrapure water, suction filter, and dry to obtain the nitrogen-sulfur synergistic flame retardant compound (NNS).

[0050] Accurately weigh Ni(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O ...

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Abstract

The invention relates to synthesis of a nitrogen and sulfur-containing synergistic flame retardant compound and a preparation method of intercalated modified hydrotalcite thereof. By means of the "structure memory effect" of hydrotalcite, the compound is introduced into the interlayer of hydrotalcite, thus significantly improving the dispersion performance of a hydrotalcite-based flame retardant and enhancing flame retardance to a polymer matrix. Based on the flame-retardant mechanism and high-efficiency flame-retardant properties peculiar to nitrogen-sulfur compounds, the compound is introduced to the interlayer of hydrotalcite by self-assembly reconstruction to prepare a novel organic-inorganic hybrid flame retardant, thus enhancing the hydrophilic properties of the hydrotalcite surface,and also further enhancing the flame-retardant properties. The prepared nitrogen and sulfur-containing synergistic flame retardant compound intercalated hydrotalcite composite flame retardant can significantly improve the flame-retardant effect after filling in the polymer matrix, and has good application value in improving the flame retardance of polyolefins. The preparation of the nitrogen-sulfur synergistic flame retardant compound is simple and practicable, the reaction conditions are easy to control, and the flame retardant efficiency is high.

Description

technical field [0001] The invention relates to a preparation method of a high-efficiency nitrogen-sulfur synergistic flame retardant compound intercalated hydrotalcite flame retardant, which belongs to the field of polymer flame retardant and organic-inorganic hybrid materials. Background technique [0002] Polyolefin polymers are flammable materials, which will be ignited quickly in case of fire, with fast diffusion speed and high calorific value, accompanied by a large number of flammable molten droplets, which will cause fire accidents and cause huge losses to people's lives and property, which greatly limits other It is widely used in fields with high requirements for flame retardancy. [0003] In view of the continuous enhancement of people's awareness of environmental protection and the promulgation of EU WEEE and RoHS directives, it is urgent to develop environmentally friendly halogen-free flame retardants. Hydrotalcites (LDHs), due to their adjustable chemical com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/70C09C1/24C09C1/40C09C3/08C08K5/3492C08K9/04C08K3/22C08L23/12
CPCC07D251/70C08K5/34922C08K9/04C08K3/22C09C1/24C09C1/407C09C3/08C01P2002/82C01P2002/08C08L23/12
Inventor 徐圣李思雨曾虹燕张敏潘勇陈超荣吴昆田贤曜
Owner XIANGTAN UNIV
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