Organic phosphinate flame retardant and preparation method thereof

[0028] Example 1:

[0029] Put 3.3Kg of dimethyl phosphite into a dry 5L reaction kettle, turn on stirring, feed acetylene gas, keep the pressure in the kettle at 0.3MPa, and dropwise add 100g of 30% (mass percent concentration) sodium methoxide solution, clamp Cooling water was introduced into the jacket to control the temperature in the reactor to be 30-35°C. When the amount of acetylene gas introduced reached 390 g, the reaction was kept for 1 hour, and then the gas source was closed.

[0030] Transfer the material to the hydrolysis kettle, add 2Kg of deionized water, raise the temperature to 105°C, use the reflux rectification methanol method for hydrolysis, and purify the hydrolyzed product methanol through a rectifying tower and then recycle it. After the hydrolysis is completed, the material is cooled and transferred to a In the neutralization kettle, the temperature was raised to 75°C, and then 9.4Kg of 40% (mass percent concentration) aluminum sulfate aqueous solution was added dropwise, and white solids were precipitated. The yield was 97.0%, the purity was 98.2%, and the phosphorus content was 27.72%.

[0031] The structural formula is:

[0032]

[0033] Example 2:

[0034] Put 3.3Kg of dimethyl phosphite into a dry 5L reaction kettle, turn on stirring, feed 1,3-butadiene gas, keep the pressure in the kettle at 0.4MPa, and add 30% (mass percent concentration) dropwise at the same time. 100g of sodium methoxide solution, pass cooling water into the jacket to control the temperature in the reaction kettle to be 35-40°C, when the amount of 1,3-butadiene gas introduced reaches 810g, keep the reaction for 1 hour, and then close the gas source. Transfer the material to the hydrolysis kettle, add 2Kg of deionized water, raise the temperature to 108°C, and use the reflux rectification methanol method to hydrolyze the hydrolysis product. In the neutralization kettle, the temperature was raised to 85°C, and then 9.4Kg of 40% (mass percent concentration) aluminum sulfate aqueous solution was added dropwise, and white solids were precipitated. The yield was 97.6%, the purity was measured to be 98.6%, and the phosphorus content was 24.68%.

[0035] The structural formula is:

[0036]

[0037] Example 3:

[0038] The solution obtained after the hydrolysis of Example 1 was transferred to the neutralization kettle, and the temperature was raised to 75° C. Then 9.15Kg of 40% (mass percent concentration) calcium chloride aqueous solution was added dropwise, and a white solid was precipitated. After filtration, washing, After drying, 3918.2 g of finished product calcium phosphinate was obtained, the yield was 98.2%, the purity was measured to be 98.8%, and the phosphorus content was 23.17%.

[0039] The product structure is:

[0040]