CN102964879A - Method for preparing surface modification nano-magnesium hydroxide - Google Patents
Method for preparing surface modification nano-magnesium hydroxide Download PDFInfo
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- CN102964879A CN102964879A CN2012104916817A CN201210491681A CN102964879A CN 102964879 A CN102964879 A CN 102964879A CN 2012104916817 A CN2012104916817 A CN 2012104916817A CN 201210491681 A CN201210491681 A CN 201210491681A CN 102964879 A CN102964879 A CN 102964879A
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Abstract
The invention discloses a method for preparing surface modification nano-magnesium hydroxide. Firstly, phosphate ester compound solution with the mass fraction of 5-20% is adopted to carry out surface modification on magnesium hydroxide, and then, terminal amino polyhydric alcohol ester solution with the mass fraction of 10-20% is adopted to carry out secondary modification through a dry modification method. The prepared modified magnesium hydroxide is applied to the high filling modification of macromolecular materials, and the processing fluidity and flame retardant property of the materials can be obviously improved.
Description
Technical field:
Technical solution of the present invention relates to a kind of preparation method of fire retardant, is specifically related to a kind of preparation method of surface modified nano magnesium hydroxide.
Background technology:
Magnesium hydroxide and aluminium hydroxide are the most frequently used inorganic combustion inhibitors, but the decomposition temperature of magnesium hydroxide is higher about 100 ℃ than aluminium hydroxide, and the magnesium oxide that decomposition generates in combustion processes becomes the charcoal effect will significantly be better than decomposing the aluminum oxide that produces by aluminium hydroxide.Therefore, magnesium hydroxide is highly suitable for the demanding fire retardant material of temperature resistant grade.Although it is large that nano-sized magnesium hydroxide has specific surface area, flame retarding efficiency is advantages of higher relatively, and a large amount of strong polarity oh groups are contained on its surface, and bad dispersibility in macromolecular material is reunited easily; Because loading level is large, mechanical property and the processing fluidity of material are all had a strong impact on simultaneously.Therefore, need to carry out consistency and the processing fluidity that surface modification treatment improves nano-sized magnesium hydroxide and macromolecular material to nano-sized magnesium hydroxide.
Phosphate compounds itself has certain flame retardant effect, and has certain fire-retardant synergistic effect with magnesium hydroxide, but has the undesirable defective of surface modification effect.End amido polyhydric alcohol ester cpds has good covered effect owing to self have than polyfunctional group to mineral fillers such as magnesium hydroxides.The present invention improves flame retarding efficiency by at first adopting phosphate compounds that nano-sized magnesium hydroxide is carried out the first layer surface modification treatment, then adopt end amido polyhydric alcohol ester cpds to carry out second layer surface modification treatment and improve consistency with macromolecular material, to reach the effect that improves simultaneously its flame retarding efficiency and consistency.
Summary of the invention:
For solving in order to solve the deficiencies in the prior art, technical problem to be solved by this invention provides the preparation method of surface modified nano magnesium hydroxide.
The object of the present invention is achieved like this:
At first in homogenizer, nano-sized magnesium hydroxide was stirred preheating 30-40 minute under 90-120 ℃, then adopt phosphate compounds solution to add in the nano-sized magnesium hydroxide with the high-pressure fog form, 100-120 ℃ of lower the stirring 1-2 hour, organic solvent evaporation is removed; Adopt at last end amido polyhydric alcohol ester solution to add in the good nano-sized magnesium hydroxide of phosphate compound surface treatment by the high-pressure fog mode, 100-120 ℃ of lower the stirring 1-2 hour, organic solvent evaporation is removed.
Described magnesium hydroxide: phosphate compound: the mass ratio of end amido polyhydric alcohol ester is 100:(1-3): (0.5-2).
Described homogenizer stir speed (S.S.) is 1000-3000 rev/min.
Described magnesium hydroxide particle diameter is at 10-500nm.
Described phosphate compounds is triphenylphosphate, tricresyl phosphate nonyl phenyl ester, a kind of in the tetraphenyl diphenol A diphosphonate; Described solvent is dehydrated alcohol, acetone, tetrachloromethane, a kind of in ethyl acetate or the butylacetate; The phosphate compound massfraction is 5-15%.
Described end amido polyhydric alcohol ester model is the LK-G02FX of chemical industry company limited of Nanjing Netac; Described solvent is dehydrated alcohol, acetone, tetrachloromethane, a kind of in ethyl acetate or the butylacetate; End amido polyhydric alcohol ester massfraction is 15-20%.
With respect to prior art, beneficial effect of the present invention is embodied as:
1, the nano-sized magnesium hydroxide polarity of the present invention's preparation is low, and activation rate is higher than 98%, and oil-absorption(number) is lower than 35ml/100g.
2, nano-sized magnesium hydroxide and the macromolecular material consistency of the present invention's preparation are good, and flame retarding efficiency is high, can significantly improve mechanical property, processing fluidity and the oxygen index of polymer composite.
3, the present invention has very high cost performance, can be applicable to high-end high-temperature resistant grade flame retardant products and reduces cost.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
Ultrasonic agitation in 10 kilograms of dehydrated alcohols of 1.5 kilograms of triphenylphosphates addings is even, ultrasonic agitation in 8 kilograms of dehydrated alcohols of 1 kilogram of end amido polyhydric alcohol ester LK-G02FX adding is even.100 kilograms of nano-sized magnesium hydroxides are added in the homogenizers 110 ℃ stir preheating 30 minutes.At first the mode of 11.5 kilograms of triphenylphosphate solution with high-pressure fog slowly added at the top in the nano-sized magnesium hydroxide, stirred 2 hours at 120 ℃, boil off organic solvent.Then 9 kilograms of end amido polyhydric alcohol ester LK-G02FX solution are slowly added at the top in the high-pressure fog mode, 120 ℃ of lower stirrings 1.5 hours boil off organic solvent, obtain the high flame retardant surface modified nano magnesium hydroxide.
Embodiment 2:
Ultra-sonic dispersion in 9 kilograms of dehydrated alcohols of 1 kilogram of triphenylphosphate adding is even, ultra-sonic dispersion in 8 kilograms of dehydrated alcohols of 2 kilograms of end amido polyhydric alcohol ester LK-G02FX addings is even.100 kilograms of nano-sized magnesium hydroxides are added in the homogenizers 120 ℃ stir preheating 40 minutes.At first the mode of 10 kilograms of triphenylphosphate solution with high-pressure fog slowly added at the top in the nano-sized magnesium hydroxide, stirred 1.5 hours at 120 ℃, boil off organic solvent.Then 10 kilograms of end amido polyhydric alcohol ester LK-G02FX solution are slowly added at the top in the high-pressure fog mode, 120 ℃ of lower stirrings 2 hours boil off organic solvent, obtain the high flame retardant surface modified nano magnesium hydroxide.
Embodiment 3:
Ultra-sonic dispersion in 8.5 kilograms of acetone of 1.5 kilograms of tricresyl phosphate nonyl phenyl esters addings is even, ultra-sonic dispersion in 8.2 kilograms of acetone of 1.8 kilograms of end amido polyhydric alcohol ester LK-G02FX addings is even.100 kilograms of nano-sized magnesium hydroxides are added in the homogenizers 120 ℃ stir preheating 35 minutes.At first the mode of 10 kilograms of tricresyl phosphate nonyl benzene ester solutions with high-pressure fog slowly added at the top in the nano-sized magnesium hydroxide, stirred 1.5 hours at 120 ℃, boil off organic solvent.Then 10 kilograms of end amido polyhydric alcohol ester LK-G02FX solution are slowly added at the top in the high-pressure fog mode, 120 ℃ of lower stirrings 2 hours boil off organic solvent, obtain the high flame retardant surface modified nano magnesium hydroxide.
Embodiment 4:
Ultra-sonic dispersion in 8 kilograms of acetone of 2 kilograms of tetraphenyl diphenol A diphosphonates addings is even, ultra-sonic dispersion in 8.8 kilograms of acetone of 1.2 kilograms of end amido polyhydric alcohol ester LK-G02FX addings is even.100 kilograms of nano-sized magnesium hydroxides are added in the homogenizers 120 ℃ stir preheating 40 minutes.At first the mode of 10 kilograms of tetraphenyl diphenol A diphosphonate solution with high-pressure fog slowly added at the top in the nano-sized magnesium hydroxide, stirred 2 hours at 120 ℃, boil off organic solvent.Then 10 kilograms of end amido polyhydric alcohol ester LK-G02FX solution are slowly added at the top in the high-pressure fog mode, 120 ℃ of lower stirrings 1.5 hours boil off organic solvent, obtain the high flame retardant surface modified nano magnesium hydroxide.
Adopt the method for embodiment 1 to prepare high flame retardant surface modified nano magnesium hydroxide of the present invention.
To the performance test of embodiment 1-4 high flame retardant surface modified nano magnesium hydroxide, concrete data see the following form:
Undoubtedly, the present invention can also have multiple conversion and remodeling, is not limited to the concrete structure of above-mentioned embodiment.In a word, protection scope of the present invention should comprise those to those skilled in the art apparent conversion or alternative and remodeling.
Claims (6)
1. the preparation method of a surface modified nano magnesium hydroxide is characterized in that: comprise the steps:
(1) at first under 90-120 ℃, in homogenizer, nano-sized magnesium hydroxide was stirred preheating 30-40 minute;
(2) then adopt phosphate compounds solution to add in the nano-sized magnesium hydroxide with the high-pressure fog form, 100-120 ℃ of lower the stirring 1-2 hour, organic solvent evaporation is removed;
(3) adopt at last end amido polyhydric alcohol ester solution to add in the good nano-sized magnesium hydroxide of phosphate compound surface treatment by the high-pressure fog mode, 100-120 ℃ of lower the stirring 1-2 hour, organic solvent evaporation is removed.
2. such as the preparation method of right 1 described a kind of surface modified nano magnesium hydroxide, it is characterized in that: described magnesium hydroxide: phosphate compound: the mass ratio of end amido polyhydric alcohol ester is 100:1-3:0.5-2.
3. such as the preparation method of right 1 described a kind of surface modified nano magnesium hydroxide, it is characterized in that: described homogenizer stir speed (S.S.) is 1000-3000 rev/min.
4. such as right 1 described nano-sized magnesium hydroxide, it is characterized in that: described magnesium hydroxide particle diameter is at 10-500nm.
5. such as right 1 described phosphate compounds solution, it is characterized in that: described phosphate compounds is a kind of in triphenylphosphate, tricresyl phosphate nonyl phenyl ester or the tetraphenyl diphenol A diphosphonate; Described solvent is a kind of in dehydrated alcohol, acetone, tetrachloromethane, ethyl acetate or the butylacetate; The phosphate compound massfraction is 5-15%.
6. such as right 1 described end amido polyhydric alcohol ester solution, it is characterized in that: described end amido polyhydric alcohol ester model is the LK-G02FX of chemical industry company limited of Nanjing Netac; Described solvent is a kind of in dehydrated alcohol, acetone, tetrachloromethane, ethyl acetate or the butylacetate; End amido polyhydric alcohol ester massfraction is 15-20%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965656A (en) * | 2014-05-05 | 2014-08-06 | 山东华研新材料有限公司 | Method for preparing modified magnesium hydroxide flame retardant |
Citations (4)
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|---|---|---|---|---|
| CN1219550A (en) * | 1997-10-17 | 1999-06-16 | 协和化学工业株式会社 | Acid-resistant, thermoplastic resin composition containing magnesium hydroxide and its use |
| CN101845165A (en) * | 2009-03-24 | 2010-09-29 | 新疆科艺达铝塑制造有限公司 | Method for preparing flame-retardant wood-flour composite macromolecular thermoplastic resin material |
| CN102417653A (en) * | 2011-11-23 | 2012-04-18 | 福建陶金峰新材料有限公司 | Low smoke, zero halogen and flame retardant plastic and production method thereof |
| CN102675726A (en) * | 2012-05-09 | 2012-09-19 | 合肥市诚信热缩材料制品厂 | Low-smoke zero-halogen antiflaming thermal contraction material and preparation method thereof |
-
2012
- 2012-11-27 CN CN2012104916817A patent/CN102964879A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1219550A (en) * | 1997-10-17 | 1999-06-16 | 协和化学工业株式会社 | Acid-resistant, thermoplastic resin composition containing magnesium hydroxide and its use |
| CN101845165A (en) * | 2009-03-24 | 2010-09-29 | 新疆科艺达铝塑制造有限公司 | Method for preparing flame-retardant wood-flour composite macromolecular thermoplastic resin material |
| CN102417653A (en) * | 2011-11-23 | 2012-04-18 | 福建陶金峰新材料有限公司 | Low smoke, zero halogen and flame retardant plastic and production method thereof |
| CN102675726A (en) * | 2012-05-09 | 2012-09-19 | 合肥市诚信热缩材料制品厂 | Low-smoke zero-halogen antiflaming thermal contraction material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965656A (en) * | 2014-05-05 | 2014-08-06 | 山东华研新材料有限公司 | Method for preparing modified magnesium hydroxide flame retardant |
| CN103965656B (en) * | 2014-05-05 | 2015-07-01 | 山东华研新材料有限公司 | Method for preparing modified magnesium hydroxide flame retardant |
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Application publication date: 20130313 |