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

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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 phosphoru

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

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Effect test

Example Embodiment

[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...

Example Embodiment

[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...

Example Embodiment

[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]

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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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