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Phosphorus-nitrogen-silicon compound containing triazine ring and its preparation method

A technology of silicon compound and triazine ring, which is applied in the field of phosphorus-nitrogen-silicon compound and its preparation, can solve the problems of high energy consumption, high addition amount, complex synthesis process, etc.

Inactive Publication Date: 2016-04-20
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a triazine ring-containing Phosphorus-nitrogen-silicon compound and preparation method thereof

Method used

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  • Phosphorus-nitrogen-silicon compound containing triazine ring and its preparation method
  • Phosphorus-nitrogen-silicon compound containing triazine ring and its preparation method
  • Phosphorus-nitrogen-silicon compound containing triazine ring and its preparation method

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Embodiment 1

[0045] The preparation method of the phosphorus-nitrogen-silicon compound containing triazine ring is:

[0046] In the first step, 1.75g ​​(55mmol) of paraformaldehyde was dissolved in 50mL of methanol, 0.63g (4.54mmol) of potassium carbonate solid was added, the solution was cooled to 0°C, and 5.0g (45.4mmol) of diphosphite was added dropwise while stirring Methyl ester, then warmed up to room temperature, potassium carbonate was filtered off after 1h, and methanol was removed from the filtrate under reduced pressure to obtain a colorless oil, which was Intermediate I;

[0047] In the second step, dissolve 3.69g (0.02mol) cyanuric chloride in 70mL acetone, stir well, keep the solution temperature between 0-5°C, slowly add 5.6mL (0.024mol) γ-aminopropyl triethyl Oxysilane, while adding sodium carbonate aqueous solution dropwise to neutralize the hydrogen chloride produced, adjust the pH value to 7, react for 1h, remove the salt by suction filtration, remove the acetone from th...

Embodiment 2

[0050] The preparation method of the phosphorus-nitrogen-silicon compound containing triazine ring is:

[0051] In the first step, 1.75g ​​(55mmol) of paraformaldehyde was dissolved in 50mL of methanol, 0.63g (4.54mmol) of potassium carbonate solid was added, the solution was cooled to 0°C, and 5.0g (45.4mmol) of diphosphite was added dropwise while stirring Methyl ester, then warmed up to room temperature, potassium carbonate was filtered off after 1h, and methanol was removed from the filtrate under reduced pressure to obtain a colorless oil, which was Intermediate I;

[0052] In the second step, dissolve 3.69g (0.02mol) cyanuric chloride in 70mL acetonitrile, stir well, keep the solution temperature between 0-5°C, slowly add 4.7mL (0.02mol) γ-aminopropyl triethyl At the same time, dropwise add sodium hydroxide aqueous solution to neutralize the hydrogen chloride produced, adjust the pH value to 6, react for 2 hours, remove the salt by suction filtration, remove acetonitrile...

Embodiment 3

[0055] The preparation method of the phosphorus-nitrogen-silicon compound containing triazine ring is:

[0056] In the first step, 6.61g (0.22mol) of paraformaldehyde was dissolved in 200mL of methanol, 2.76g (0.02mol) of potassium carbonate solid was added, the solution was cooled to 0°C, and 22.0g (0.2mol) of phosphorous acid was added dropwise while stirring Dimethyl ester, then warmed up to room temperature, potassium carbonate was filtered off after 1h, and methanol was removed from the filtrate under reduced pressure to obtain a colorless oily substance, which was intermediate Ⅰ;

[0057] In the second step, dissolve 3.69g (0.02mol) cyanuric chloride in 70mL tetrahydrofuran, stir well, keep the solution temperature between 0-5°C, slowly add 5.6mL (0.024mol) γ-aminopropyl triethyl Oxysilane, while adding dropwise sodium bicarbonate aqueous solution to neutralize the hydrogen chloride produced, adjust the pH value to 7, react for 1.5h, remove the salt by suction filtration...

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Abstract

The invention relates to a reactive flame retardant, specifically a phosphorus-nitrogen-silicon compound containing a triazine ring and a preparation method thereof. In the first step, paraformaldehyde is dissolved in methanol, potassium carbonate solid is added, and the solution is cooled To 0°C, add dimethyl phosphite dropwise while stirring, then warm up to room temperature, filter off potassium carbonate after 1h, and remove methanol from the filtrate under reduced pressure to obtain a colorless oil, which is intermediate Ⅰ. Compared with the prior art, the phosphorus-nitrogen-silicon compound containing triazine rings of the present invention has the following beneficial effects: 1. The phosphorus, nitrogen, and silicon three flame-retardant elements are concentrated in one molecule, which improves the flame retardant Thermal stability, char formation and flame retardant synergistic effect; 2. The synthesis process conditions are stable, the reaction process is easy to control, the production cost is low, and it has good flame retardant effect when the amount of addition is small, and can be used for various fabrics flame retardant treatment.

Description

Technical field [0001] The present invention involves a reactive flame retardant, which is specifically a phosphor-nitrogen-silicon compound and its preparation method with a triazine-containing ring. Background technique [0002] Flame retardants are additives that can prevent materials from igniting or inhibiting flame transmission.With the continuous development of flame retardant technology, the requirements of the society's comprehensive indicators of expansion and flame retardant materials are getting higher and higher. It is necessary to meet the prescribed flame retardant level and have good physical mechanical properties. Therefore, many scholars at home and abroad are currentlyThey are all trying to synthesize the new three -source integrated expansion flame retardant.A single -group expansion flame retardant combines compounds containing acid sources, carbon sources, and gas sources in a chemical method to the same major molecule, which fundamentally solves the flame r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6521D06M13/513
Inventor 张志毅刘亚青刘胜男赵贵哲赵培华
Owner ZHONGBEI UNIV
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