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Preparation method of microcapsuled red phosphorus for polyurethane resin

A technology for microencapsulating red phosphorus and polyurethane resin, which is applied in the directions of microcapsule preparation, microsphere preparation, etc., can solve the problem that red phosphorus cannot be directly added, and achieves the effect of less addition and low cost

Inactive Publication Date: 2007-07-11
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a microencapsulated red phosphorus for polyurethane resin and its preparation method to solve the problem that red phosphorus cannot be directly added to polyurethane resin

Method used

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  • Preparation method of microcapsuled red phosphorus for polyurethane resin
  • Preparation method of microcapsuled red phosphorus for polyurethane resin
  • Preparation method of microcapsuled red phosphorus for polyurethane resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] First red phosphorus pretreatment. Soak 100g of crude red phosphorus in 50g of 30% glycerol aqueous solution for 12h, grind it twice with a colloid mill, filter, wash the filter cake with absolute ethanol three times, and dry it in an oven at 80°C to constant weight for later use.

[0040] 40 g of the above-mentioned treated red phosphorus, 55 g of water, and 2.6 g of polyethylene glycol were made into an aqueous suspension emulsion, and after being ground twice in a colloid mill, it was moved into a 250 ml three-necked bottle, and 80 g of chloroform was added at a stirring speed of 2000 rpm , Stir for 60min to form a milky solution. Reduce stirring speed to 200rpm, temperature is 5~10 ℃, add 22.4g diphenylmethane diisocyanate solution (wherein diphenylmethane diisocyanate: Tween-80: trichloromethane is 2: 0.4: 20), maintain temperature and Stir at a constant speed, react for 30 minutes, filter, wash with chloroform and water three times, and dry at 50°C to constant we...

Embodiment 2

[0054] Red phosphorus 60g pretreated in the same way as in Example 1 was made into an aqueous suspension emulsion with 38g water and 1.6g ethylenediamine, and after being ground twice in a colloid mill, it was moved into a 250ml three-necked bottle, and at a stirring speed of 1000rpm, adding 70g of cyclohexanone was stirred for 60min to form a milky solution. Reduce the stirring speed to 400rpm, the temperature is 3~10°C, add 30.4g diphenylmethane diisocyanate solution (wherein diphenylmethane diisocyanate: sodium dodecylbenzenesulfonate: cyclohexanone is 10:0.4:20 ), keep the temperature and stirring speed constant, react for 30min, filter, wash with water three times, and dry to constant weight at 50°C to obtain microencapsulated red phosphorus.

[0055] According to the method introduced in Example 1, various indicators were measured: coating rate: 17%; moisture absorption rate: 0.050%; ignition point: 375° C.; phosphine release: 0.21 μg / g·24h.

Embodiment 3

[0057] Red phosphorus 80g pretreated in the same way as in Example 1 was made into an aqueous suspoemulsion with 31g water and 4.6g polyvinyl alcohol. After grinding twice in a colloid mill, move it into a 250ml three-necked bottle, and at a stirring speed of 4000rpm, add Carbon tetrachloride 60g, stirred for 60min, into a milky solution. Reduce the stirring speed to 400rpm, the temperature is 3 ~ 10 ℃, add 24.4g diphenylmethane diisocyanate solution (wherein diphenylmethane diisocyanate: sodium oleate: carbon tetrachloride is 4: 0.4: 20), maintain the temperature With constant stirring speed, the reaction was carried out for 30 minutes, filtered, washed with water three times, and dried at 50°C to constant weight to obtain microencapsulated red phosphorus.

[0058] According to the method introduced in Example 1, various indicators were measured: coating rate: 10%; moisture absorption rate: 0.021%; ignition point: 355° C.; phosphine release: 0.15 μg / g·24h.

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Abstract

The invention discloses a microcapsule red phosphorus and making method of polyurethane resin, which comprises the following steps: immersing red phosphorus in the 25%-35% glycerin deionized water for 10-14h; grinding gel evenly; filtering; washing filter pie through anhydrous alcohol; placing in the baker to toast to constant weight under 60-90 deg. c; blending red phosphorus, water and polyol; grinding the gel evenly; stirring at 1000-5000rpm; adding organic solvent with weight as 1-2 times as red phosphorus; stirring 30-60min continuously; reducing stirring speed to 100-600rpm; adjusting temperature to 2-10 deg. c; adding isocyanate solution; reacting completely; filtering; washing; drying to obtain the product.

Description

(1) Technical field [0001] The invention relates to a microencapsulated red phosphorus for polyurethane resin and a preparation method thereof. (2) Background technology [0002] Red phosphorus is a new type of halogen-free flame retardant that has attracted great attention in recent years. It is non-toxic, odorless, low-smoke and highly efficient. Adding a small amount of red phosphorus to polymers has a significant flame-retardant effect. Its flame retardant mechanism is mainly that red phosphorus is first heated to decompose P n →P 4 →P 2 , red phosphorus can capture oxygen in the polymer or oxygen in the air during the decomposition process, and red phosphorus becomes oxygen-containing phosphoric acid. These oxyphosphoric acids are extremely absorbent and char the surface of the burning polymer. The carbonized layer can reduce the heat of oxidation on the surface of the polymer and at the same time block the release of volatile components in the polymer. In addition...

Claims

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Application Information

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IPC IPC(8): C08K11/00C08L75/04B01J13/02
Inventor 赵亚娟任宝东李新华
Owner WENZHOU UNIVERSITY
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