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Triazine ring-containing phosphorus-nitrogen-silicon compound and preparation method thereof

A technology of silicon compound and triazine ring, which is applied in the field of phosphorus-nitrogen-silicon compound containing triazine ring and its preparation, and can solve the problems of complex synthesis process, poor washing resistance, poor thermal stability, etc.

Inactive Publication Date: 2014-08-13
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of poor thermal stability, high addition amount, poor washing resistance and complex synthesis process of existing intumescent flame retardants for cotton, the present invention , the problem of high energy consumption, a phosphorus-nitrogen-silicon compound containing a triazine ring and a preparation method thereof are provided

Method used

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  • Triazine ring-containing phosphorus-nitrogen-silicon compound and preparation method thereof
  • Triazine ring-containing phosphorus-nitrogen-silicon compound and preparation method thereof
  • Triazine ring-containing phosphorus-nitrogen-silicon compound and preparation method thereof

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Effect test

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 h, remove the salt by suction filtration, remove the 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 At the same time, dropwise add sodium bicarbonate aqueous solution to neutralize the hydrogen chloride produced, adjust the pH value to 7, react for 1.5 h, remove the salt by suction filtration,...

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Abstract

The invention relates to a reactive flame retardant and particularly relates to a triazine ring-containing phosphorus-nitrogen-silicon compound and a preparation method thereof. The preparation method comprises the following steps: S1, dissolving paraformaldehyde in methanol; adding a potassium carbonate solid; cooling the solution to 0 DEG C; stirring and adding dimethyl phosphate drop by drop; and S2, rising to room temperature, filtering out potassium carbonate after 1 hour, and decompressing and removing methanol from the filtrate to obtain colorless grease, namely an intermediate I. Compared with the prior art, the triazine ring-containing phosphorus-nitrogen-silicon compound provided by the invention has the beneficial effects that 1, three flame retardant elements phosphorus-nitrogen-silicon are integrated in one molecule, so that the heat stability, the charcoal forming property and the flame retardant synergic effect are improved; 2, the synthetic technological conditions are stable, the reaction process is easy to control and the production cost is low, and the compound has a good flame retardant effect under the condition of a small addition amount and can be used for flame retardant treatment of various fabrics.

Description

technical field [0001] The invention relates to a reactive flame retardant, in particular to a phosphorus-nitrogen-silicon compound containing a triazine ring and a preparation method thereof. Background technique [0002] Flame retardants are a class of additives that prevent materials from igniting or inhibit the spread of flames. With the continuous development of flame retardant technology, the society has higher and higher requirements for the comprehensive index of intumescent flame retardant materials. It must not only meet the prescribed flame retardant level, but also have good physical and mechanical properties. They are all trying to synthesize a new type of three-source integrated intumescent flame retardant. One-component intumescent flame retardants chemically combine compounds containing functional groups such as acid source, carbon source and gas source to the same macromolecule, which fundamentally solves the problem of each flame retardant of compound int...

Claims

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Application Information

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