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

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Problems solved by technology

[0004] The invention provides a microencapsulated red phosphorus for polyurethane resin and its prepa

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
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Example Embodiment

[0038] Example 1

[0039] First, red phosphorus pretreatment. After soaking 100 g of crude red phosphorus in 50 g of 30% glycerin aqueous solution for 12 hours, 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 a constant weight for later use.

[0040] Mix 40g of the above-treated red phosphorus, 55g water, and 2.6g polyethylene glycol into a suspension emulsion, grind it twice in a colloid mill, transfer it into a 250ml three-necked flask, add 80g chloroform at a stirring speed of 2000rpm , Stir for 60min to form a milky solution. Reduce the stirring speed to 200rpm and the temperature to 5-10°C, add 22.4g of diphenylmethane diisocyanate solution (wherein diphenylmethane diisocyanate: Tween-80: chloroform is 2: 0.4: 20), maintain the temperature and The stirring speed is unchanged, the reaction is 30min, the filtration is performed, and after washing with chloroform and water three times, it is dri...

Example Embodiment

[0053] Example 2

[0054] 60g of red phosphorus pretreated by the same method as in Example 1 was mixed with 38g of water and 1.6g of ethylenediamine to form an aqueous suspension emulsion. After being ground twice in a colloid mill, it was transferred to a 250ml three-necked flask and added at a stirring speed of 1000rpm. 70g cyclohexanone, stirred for 60min, into a milky solution. Reduce the stirring speed to 400rpm, the temperature is 3~10℃, add 30.4g diphenylmethane diisocyanate solution (wherein diphenylmethane diisocyanate: sodium dodecylbenzene sulfonate: cyclohexanone is 10: 0.4: 20 ), maintaining the temperature and stirring speed unchanged, reacting for 30 minutes, filtering, washing with water three times, and drying 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 releas...

Example Embodiment

[0056] Example 3

[0057] 80g of red phosphorus pretreated by the same method as in Example 1 was mixed with 31g of water and 4.6g of polyvinyl alcohol to form an aqueous suspension emulsion. After grinding twice in a colloid mill, it was transferred into a 250ml three-necked flask and added at a stirring speed of 4000rpm. 60g carbon tetrachloride, stirred for 60min, into a milky solution. Reduce the stirring speed to 400rpm, the temperature is 3~10℃, add 24.4g diphenylmethane diisocyanate solution (where diphenylmethane diisocyanate: sodium oleate: carbon tetrachloride is 4: 0.4: 20), maintain the temperature With the stirring speed unchanged, the reaction was carried out for 30 minutes, filtered, washed with water three times, and dried to constant weight at 50°C 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; phosphi...

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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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