Rear earth organic phosphonate flame retardant, synthesizing method and use thereof

A technology of rare earth organic phosphate and organic phosphonic acid, which is applied in the fields of fine chemicals and polymer materials, and achieves the effects of high phosphorus content, effective and feasible process, and wide synergy.

Active Publication Date: 2011-06-08
广东华南精细化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the field of flame retardants, there is no precedent for the application of rare earth elements. How to combine rare earth elements and halogen-free flame retardants to meet the requirements of low toxicity, low smoke and harmlessness while taking into account the flame retardant effect is an update. research topic

Method used

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  • Rear earth organic phosphonate flame retardant, synthesizing method and use thereof
  • Rear earth organic phosphonate flame retardant, synthesizing method and use thereof
  • Rear earth organic phosphonate flame retardant, synthesizing method and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0064] Example 1. Synthesis of Lanthanum Dimethylphosphonate

[0065] Add 94g of dimethylphosphonic acid and 500ml of ethanol aqueous solution with a concentration of 15% into the reactor. The structural formula of dimethylphosphonic acid is as shown in general formula (IV), R 1 , R 2 For methyl. Under stirring, a 20% sodium hydroxide aqueous solution containing 44 g of sodium hydroxide was added and reacted at 70° C. for 2 hours. Then, a 20% lanthanum chloride aqueous solution containing 245.5 g of lanthanum chloride was added, and then the pH value of the solution was adjusted to 7-8 with sodium hydroxide solution, and the solution was stirred at 20-30°C for 2 hours. After the reaction, it was filtered, dried and crushed to obtain 244.2 g of lanthanum bismethylphosphonate with a yield of 91.8%.

Embodiment 2

[0066] Example 2. Synthesis of Gadolinium Di-tert-butylphosphonate

[0067] Add 178g of bis-tert-butylphosphonic acid and 1000ml of ethanol aqueous solution with a concentration of 15% into the reactor. The structural formula of bis-tert-butylphosphonic acid is shown in general formula (IV), R 1 , R 2 It is tert-butyl. Under stirring, a 20% sodium hydroxide aqueous solution containing 44 g of sodium hydroxide was added and reacted at 60°C for 2 hours. Then a 20% gadolinium chloride aqueous solution containing 263.75 g of gadolinium chloride was added, and the pH value of the solution was adjusted to 7-8 with sodium hydroxide solution, and the solution was stirred at 60° C. for 2 hours. After the reaction is completed, it is filtered, dried and pulverized to obtain 332.2 g of gadolinium bis-tert-butylphosphonate with a yield of 90.2%.

Embodiment 3

[0068] Example 3. Synthesis of bisethoxy lanthanum phosphate

[0069] Add 154g of bisethoxy phosphoric acid and 800ml of isopropanol solution with a concentration of 15% in the reactor. The structural formula is as shown in general formula (IV), R 1 , R 2 It is ethoxy. Under stirring, a 20% sodium hydroxide aqueous solution containing 44 g of sodium hydroxide was added and reacted at 60° C. for 1 hour. Then, a 15% lanthanum chloride aqueous solution containing 245.5 g of lanthanum chloride was added, and then the pH value of the solution was adjusted to 7-8 with sodium hydroxide solution, and the solution was stirred at 60°C for 2 hours. After the reaction, it is filtered, dried and crushed to obtain 297.3 g of bisethoxy lanthanum phosphate with a yield of 91.2%.

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Abstract

The invention relates to organic phosphonic (phosphoric) acid rare-earth salt fire retardant and a synthetic method and application thereof, which belongs to the fields of fine chemical and macromolecular materials. The low-toxic, low-smoke, environment-friendly and efficient fire retardant is formed by combining with rare earth elements in organic phosphonic (phosphoric) acid structure. Comparedwith the organic phosphorous compound, the fire retardant has extremely high stability at normal temperature and plastic processing temperature; moreover, the use of rare earth elements ensures that the fire retardant and other components in macromolecular material are formed into a combination having better effects than Van Der Waals Force, hydrogen bond and the like; particularly, when mixed with other components of inflatable composite fire retardant, the fire retardant can obtain better synergic effects than currently used phosphinates such as aluminum phosphinate, zinc phosphinate and the like; moreover, the obtained macromolecular material can maintain better physical and mechanical properties.

Description

Technical field: [0001] The invention relates to the fields of fine chemicals and polymer materials, in particular to a phosphorus-based flame retardant applied to polymers and a synthesis method thereof. Background technique: [0002] 1. Development of flame retardants [0003] Polymer materials are materials formed by long carbon chain molecules mainly composed of carbon and hydrogen elements, and are flammable, especially polymers such as polyethylene (PE), polypropylene (PP), and polyvinyl chloride (PVC). While burning, it not only caused a lot of losses, but also released a large amount of smoke and poisonous gas to varying degrees, causing casualties. This makes flame retardants one of the necessary functional additives for polymer materials. At present, the amount of flame retardants used is second only to plasticizers dedicated to PVC in terms of quality and value. [0004] Flame retardants are divided into inorganic flame retardants and organic flame retardants....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5317C07F9/30C07F9/11C07F9/12
Inventor 陈宇王朝晖
Owner 广东华南精细化工研究院有限公司
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