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Phosphate rare earth salt with cagelike structure, synthesis method and application thereof

A technology of phosphate ester and rare earth salt, which is applied in the field of phosphate ester rare earth salt and its synthesis, and preparation of flame retardants. It can solve the problems of less application and high price, and achieve improved flame retardant synergy, good effect, and high phosphorus content. Effect

Active Publication Date: 2014-04-16
广东国望精细化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphorus-based flame retardants are currently the most researched and more advanced flame retardants with a wide range of applications, especially the intumescent flame retardant system with it as one of the core components has become a more respected flame retardant mechanism. and product series, but its price is relatively high, and its application volume is still small

Method used

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  • Phosphate rare earth salt with cagelike structure, synthesis method and application thereof
  • Phosphate rare earth salt with cagelike structure, synthesis method and application thereof
  • Phosphate rare earth salt with cagelike structure, synthesis method and application thereof

Examples

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Effect test

Embodiment 1

[0044] Embodiment 1, the chemical synthesis of phosphate rare earth salt-bis-PEPA phosphate lanthanum with cage structure

[0045] Synthesizing double PEPA phosphate lanthanum with cage structure with the method of the present invention, specifically comprises the following steps:

[0046] 1) Synthesis of intermediate bis-PEPA phosphoric acid chloride: 1-oxophospha-4-hydroxymethyl-2,6,7-trioxabis[2,2,2]octane (i.e. pentaerythritol phosphate, PEPA) 252g (1.4mol), phosphorus oxychloride 64ml (PEPA: phosphorus oxychloride molar ratio is 2: 1), dioxane 1062g (PEPA is 4.2 times of mass consumption), anhydrous magnesium chloride 3.5g (accounting for PEPA is added in the reactor with heating and agitating device according to the 1.4% of mass consumption), then slowly heats up, heats up to 105 ℃, heat preservation reaction 5 hours; 236.2 g of the intermediate bis-PEPA phosphoric acid chloride was obtained, with a yield of 80.5%.

[0047] 2) 220.3g (0.5mol) of the intermediate produc...

Embodiment 2

[0049] Embodiment 2, the chemical synthesis of phosphate rare earth salt-bis(bis-PEPA phosphate) lanthanum with cage structure

[0050] Synthesize two (two PEPA phosphate) lanthanums with cage structure with the method of the present invention, specifically comprise the following steps:

[0051] 1) Synthesis of intermediate bis-PEPA phosphoric acid chloride: 1-oxophospha-4-hydroxymethyl-2,6,7-trioxabis[2,2,2]octane (i.e. pentaerythritol phosphate, PEPA) 528g (2.93mol), phosphorus oxychloride 128ml (PEPA: phosphorus oxychloride molar ratio is 2.1: 1), acetonitrile 1416g (PEPA is 2.68 times of mass consumption), anhydrous aluminum chloride 14.16g (accounts for PEPA 2.68% of the mass dosage) was added into a reactor with a heating and stirring device, then the temperature was raised slowly to 82° C., and the heat preservation reaction was carried out for 6 hours; The intermediate product bis-PEPA phosphoric acid chloride was 520.4g, and the yield was 88.6%.

[0052] 2) 440.6g o...

Embodiment 3

[0054] Embodiment 3, the chemical synthesis of phosphate rare earth salt-bis-PEPA phosphate cerium with cage structure

[0055] The double PEPA phosphate cerium with cage structure is synthesized with the method of the present invention, specifically comprises the following steps:

[0056] 1) Synthesis of intermediate product bis-PEPA phosphoric acid chloride: same as Example 1.

[0057] 2) 220.3 g of the intermediate product bis-PEPA phosphoric acid chloride, 141.0 g of cerium chloride (bis-PEPA phosphoric acid chloride: cerium chloride molar ratio is 1: 1) and 1000 ml of water (4.54 times of the intermediate product by mass consumption) ) into a reactor with a heating and stirring device, the temperature was raised to 90° C., and the insulation reaction was carried out for 1 hour; after the reaction, the temperature was lowered and cooled, and after filtration, washing and drying, 242.4 g of the final product bis-PEPA phosphate cerium was obtained. Yield 81.3%.

[0058] Af...

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Abstract

The invention discloses a phosphate rare earth salt with a cagelike structure, synthesis method and application thereof to preparation of fire retardant. According to the invention, stiff stable cagelike phosphate structure and a light rare-earth element with special electron distribution and corresponding electron cloud density are combined to fully play roles of good heat stability, high phosphorus content, high charcoal forming catalysis efficiency, increase of compatibility and inflaming retarding synergy by rare earth coordination linkage. The phosphate rare earth salt with cagelike structure can be applied to an expanding inflaming retarding system and is a fire retardant with structural innovativeness, safety, high efficiency, synergy and wide application prospects.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a rare earth phosphate salt with a cage structure, its synthesis method and its application in the preparation of flame retardants. Background technique [0002] Development of Phosphorous Flame Retardants [0003] With the successive implementation of domestic and foreign environmental protection regulations, the replacement of halogenated flame retardants is becoming more and more urgent. Phosphorus-based flame retardants are most likely to become the next-generation mainstream flame retardants due to their characteristics in terms of the balance of flame retardant performance and physical and mechanical properties, product variety, and product applicability. [0004] Phosphorus is a variable-valence element, and almost all of its valence compounds have been successfully applied to the field of flame retardancy, such as -1 valence phosphine oxide, 0 valence red ph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08L23/06C08L23/12C08L27/06C08L77/06C08L67/02C08K5/527C08K3/22C08K3/38C08K5/3492
CPCY02P20/52
Inventor 陈宇王朝晖赵欣王磊张妙珍洪伟波
Owner 广东国望精细化学品有限公司
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