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Phosphor-nitrogen expansion type combustion inhibitor and method of producing the same

A technology of nitrogen expansion and flame retardant, which is applied in the field of phosphorus-nitrogen expansion flame retardant and its preparation, can solve the problems of low thermal stability, easy decomposition, and limited application of compounds, and achieve low equipment requirements and environmental protection The effect of less pollution and less viscosity

Inactive Publication Date: 2009-05-13
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the thermal stability of this compound is not very high, and it is easy to decompose in the process of polymer flame retardant processing, which limits its application in the field of polymer materials

Method used

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  • Phosphor-nitrogen expansion type combustion inhibitor and method of producing the same
  • Phosphor-nitrogen expansion type combustion inhibitor and method of producing the same
  • Phosphor-nitrogen expansion type combustion inhibitor and method of producing the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 0.1 mol of p-chlorobenzaldehyde and 0.2 mol of isobutyraldehyde were mixed and placed in a 250 ml four-necked flask equipped with a thermometer, a magnetic stirrer, a reflux condenser, and a constant pressure dropping funnel. Dissolve 0.1 mol of potassium hydroxide in 90 ml of absolute ethanol, and slowly drop it into a four-necked flask with a constant pressure dropping funnel. The reaction is exothermic, and the temperature is controlled by a water bath at 50°C, and the reaction is stirred for 4 hours. After the reaction is completed, it is naturally cooled, and the reaction product is precipitated and then subjected to suction filtration. The filter cake is washed several times with n-heptane, and 19.70 g of white crystals are obtained. The product (I) has a yield of 91.84% and a melting point of 99-100°C.

[0028] Add intermediate product (I) 0.1mol, phosphoric acid 0.1mol, p-toluenesulfonic acid 0.22g, 85.8g toluene in the 250ml four-necked flask that thermometer, ...

Embodiment 2

[0031] 0.1mol of p-chlorobenzaldehyde and 0.22mol of isobutyraldehyde were mixed and placed in a 250ml four-necked flask equipped with a thermometer, a magnetic stirrer, a reflux condenser, and a constant pressure dropping funnel. Dissolve 0.12 mol of potassium hydroxide in 120 ml of absolute ethanol, and slowly drop it into a four-necked flask with a constant pressure dropping funnel. The reaction is exothermic, and the temperature is controlled by a water bath at 54°C, and the reaction is stirred for 5 hours. After the reaction is completed, it is cooled naturally, and the reaction product is precipitated and then filtered with suction. The filter cake is washed several times with n-heptane to obtain 19.75g of white crystals, namely The product (I) has a yield of 92.07% and a melting point of 98-99.5°C.

[0032] Add 0.1mol of intermediate product (I), 0.12mol of phosphoric acid, 0.43g of benzoic acid, and 108g of benzene in a 250ml four-neck flask equipped with a thermometer...

Embodiment 3

[0035] 0.1 mol of p-chlorobenzaldehyde and 0.23 mol of isobutyraldehyde were mixed and placed in a 250 ml four-necked flask equipped with a thermometer, a magnetic stirrer, a reflux condenser, and a constant pressure dropping funnel. Dissolve 0.13 mol of sodium hydroxide in 143 ml of absolute ethanol, and slowly drop it into a four-necked flask with a constant pressure dropping funnel. The reaction is exothermic, and the temperature is controlled by a water bath at 57°C, and the reaction is stirred for 5.5 hours. After the reaction is completed, it is naturally cooled, and the reaction product is precipitated and then filtered with suction. The filter cake is washed several times with n-hexane to obtain 18.90 g of white crystals, namely The product (I) has a yield of 88.11% and a melting point of 97-99.5°C.

[0036]Add intermediate product (I) 0.1mol, phosphoric acid 0.16mol, sodium p-toluenesulfonate 0.53g, 118g dimethylbenzene in the 250ml four-necked flask that thermometer,...

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Abstract

The invention discloses a phosphorus-nitrogen swelling type fire retardant and a method for preparing the same. The chemical name of the fire retardant is 5, 5-dimethyl-4-p-chlorophenyl-1, 3, 2-dioxaphosphorinane phosphonate melamine salt. The preparation method comprises the following steps: (1) p-chlorobenzaldehyde and iso-butyraldehyde react with alkali ethanol solution, are cooled down and filtered to obtain an intermediate product (I); (2) the intermediate product (I) and phosphoric acid are added to solvent, and added with paratoluenesulfonic acid or benzoic acid or sodium salt of benzoic acid; and the mixing solution is distilled after reaction to reclaim the solvent to obtain an intermediate product(II); and (3) melamine and the intermediate product(II) are added to water for reaction, cooled down and filtered to obtain a filter cake; and the filter cake is dried to obtain phosphorus-nitrogen swelling type fire retardant. The phosphorus-nitrogen swelling type fire retardant has the advantages of high thermal stability, good compatibility, no halogen, less smoke and environmental protection. The preparation method has the advantages of materials available, simple process, mild reaction conditions, small viscosity of reaction liquid, low requirement on equipment and little environmental pollution.

Description

technical field [0001] The invention relates to a phosphorus-nitrogen intumescent flame retardant and a preparation method thereof, in particular to a novel flame retardant 5,5-dimethyl-4-p-chlorophenyl-1,3,2-di Melamine oxaphosphorinyl phosphate and a preparation method thereof. Background technique [0002] In recent years, in the development and application of flame retardants, phosphorus-nitrogen-based flame retardants have sprung up. Due to the synergistic and synergistic effects between phosphorus and nitrogen, this type of compound has good flame-retardant properties, and has a small amount of smoke and is toxic. The amount of gas generated is small, and it will become a direction for the development of flame retardants in the future. There is also a kind of intumescent flame retardant in the phosphorus nitrogen flame retardant. When the polymer added with this kind of flame retardant is heated, a layer of uniform carbon foam layer can be formed on the surface. Smok...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/12C07F9/6574C07D251/54
Inventor 闫晓红孟烨赵庭栋
Owner SHANDONG TIANYI CHEM
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