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Organic phosphinate flame retardant and preparation method thereof

An organic phosphite and flame retardant technology, applied in the chemical industry, can solve the problems of high equipment and safety requirements, complex processes, high reaction pressure, and achieve good thermal stability of products, cheap and easy-to-obtain raw materials, and high reaction pressure. mild conditions

Inactive Publication Date: 2014-10-29
JIANGSU DAMING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, Chinese patent CN201010217750 discloses a method for preparing an alkyl phosphinate polymer, which is formed by free radical addition of alkynes, alkenes and hypophosphorous acid (salt) in sequence under the action of an initiator Alkyl phosphinate polymers, and then undergo metathesis reactions with aluminum salts to produce polymerized aluminum alkyl phosphinates, etc. This process needs to be reacted at relatively high temperature and pressure, which requires high production safety and can The consumption is also large, the 2-step free radical addition reaction is difficult to control, and the product purity is low; patent CN201010613835 discloses a preparation method of dialkylphosphinate, which uses Grignard reagent and diethyl phosphite to react Dialkyl phosphorus oxide is generated, and then reacted with an oxidant and acidified to obtain a dialkylphosphinate. This method uses a Grignard reagent as a raw material, and the operation is dangerous and the process is complicated, and monoalkylphosphonous acid, dioxane Mixed systems such as base phosphinic acid and hypophosphorous acid have many by-products, are difficult to separate, and have low yield and purity; The method for preparing dialkylphosphinate by reacting with ethylene with radical initiation has the following defects: monoalkylphosphinate by-products will be generated, free radicals are easily quenched and deactivated, resulting in reduced reaction speed and high reaction pressure. High requirements on equipment and safety, difficult solvent recovery and utilization, high energy consumption

Method used

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  • Organic phosphinate flame retardant and preparation method thereof
  • Organic phosphinate flame retardant and preparation method thereof
  • Organic phosphinate flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0030] Transfer the material to a hydrolysis kettle, add 2Kg deionized water, raise the temperature to 105°C, and use the reflux rectification method to hydrolyze the methanol. The hydrolyzed product methanol is purified by a rectification tower and recovered for other purposes. After the hydrolysis is completed, the material is cooled and transferred to 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 ...

Embodiment 2

[0034] Put 3.3Kg of dimethyl phosphite into a dry 5L reaction kettle, start stirring, feed 1,3-butadiene gas, keep the pressure in the kettle at 0.4MPa, and drop 30% (mass percent concentration) of Sodium methoxide solution was 100g, and cooling water was passed into the jacket to control the temperature in the reactor to be 35-40°C. When the 1,3-butadiene gas flow rate reached 810g, keep the reaction for 1 hour, and then turn off the gas source. Transfer the material to the hydrolysis kettle, add 2Kg deionized water, raise the temperature to 108°C, and use the reflux rectification methanol method to hydrolyze. The hydrolyzed product methanol is purified by a rectification tower and recovered for other use. After the hydrolysis is completed, the material is cooled and transferred to 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 a white solid was preci...

Embodiment 3

[0038] The solution obtained after hydrolysis in Example 1 was transferred to a neutralization kettle, and the temperature was raised to 75°C, and then 9.15Kg of 40% (mass percent concentration) calcium chloride aqueous solution was added dropwise, and a white solid was precipitated, which was filtered, washed with water, After drying, 3918.2 g of organic calcium phosphinate was obtained, with a yield of 98.2%, a purity of 98.8%, and a phosphorus content of 23.17%.

[0039] The product structure formula is:

[0040]

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PUM

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Abstract

The invention discloses an organic phosphinate flame retardant. The chemical formula of the organic phosphinate flame retardant is as shown in the specification, wherein M is selected from any one of metal ions such as Mg, Al, Fe, Zn, Ca, Sn and the like, and x is 2 to 4. The invention also discloses a preparation method of the organic phosphinate flame retardant. The preparation method is simple in process, low-cost and available in raw materials, mild in reaction conditions, easy to operate, small in equipment investment, safe and environment-friendly; the prepared organic phosphinate flame retardant is high in purity, high in product yield, good in product thermal stability of and high in content of phosphorus; when the organic phosphinate flame retardant is applied to engineering plastics, the organic phosphinate flame retardant is relatively good in flame retardant effect, mechanical property and electrical property.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to an organic phosphonite flame retardant and a preparation method thereof. Background technique [0002] Brominated flame retardants have excellent cost performance and are widely used in various engineering plastics, but their harm to the environment and human health cannot be ignored, and are increasingly being replaced by various environmentally friendly halogen-free flame retardants , organophosphine flame retardants are considered to be one of the most promising flame retardants to replace brominated flame retardants. [0003] Organic phosphonate flame retardants have both the flame retardant effect of phosphorus flame retardants in the gas phase and condensed phase and the smoke suppression function of metal cations. They have good thermal stability, low dosage, high flame retardant efficiency, good color and low smoke density. , good mechanical properties, high ...

Claims

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Application Information

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IPC IPC(8): C08K5/5317C07F9/38C08L67/02C08L77/06
Inventor 潘小明嵇颖耀李雪飞仇国才
Owner JIANGSU DAMING TECH
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