CN104130564B - A kind of preparation method of halogen-free flame retardants - Google Patents
A kind of preparation method of halogen-free flame retardants Download PDFInfo
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- CN104130564B CN104130564B CN201410342654.2A CN201410342654A CN104130564B CN 104130564 B CN104130564 B CN 104130564B CN 201410342654 A CN201410342654 A CN 201410342654A CN 104130564 B CN104130564 B CN 104130564B
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Abstract
The preparation method that the invention discloses a kind of halogen-free flame retardants.Preparation method comprises the following steps: Polyethylene Glycol and water are mixed to get Aqueous Solutions of Polyethylene Glycol, by aluminium hydroxide and Aqueous Solutions of Polyethylene Glycol stirring reaction, stops heating, adds polyethylene, continues stirring, be obtained by reacting mixture A；Boric acid is configured to boric acid aqueous solution, the hybrid reaction when nitrogen by boric acid aqueous solution and APP, obtain mixture B；Adding triguaiacyl phosphate and silane coupler at ambient temperature in high-speed emulsifying machine, high speed shear is divided, and obtains emulsion；Emulsion, mixture B and mixture A are placed in reactor, after being sufficiently mixed reaction, vacuum drying, obtain halogen-free flame retardants finished product.Preparation method of the present invention is simple, and not halogen-containing in raw material, the halogen-free flame retardants prepared blazes up smokelessly, pollution-free, environmental protection.
Description
Technical field:
The preparation method that the present invention relates to a kind of halogen-free flame retardants, belongs to fire proofing field.
Background technology:
Fire retardant is flame-retarded technology application in real life, and it is a kind of special auxiliary chemicals for improving flammable combustible material combustibility, is widely used in the fire-retardant processing of all kinds of finishing material.Material after fire retardant is processed, when being subject to extraneous burning things which may cause a fire disaster and attacking, it is possible to effectively stop, delay or terminate flame transmission, thus reaching fire-retardant effect.
What tradition fire proofing adopted is halogen-containing fire retardant, the burning of Halogen fire proofing produces substantial amounts of smog and poisonous etchant gas, secondary can be caused to endanger, a large amount of uses along with Halogen material, soil, air, water body are brought increasing pollution, it is increasingly recognised that the hazardness to human body and environment of traditional halogen series flame retardant material.
Summary of the invention:
The present invention seeks to, for making up the deficiencies in the prior art, and the preparation method that a kind of halogen-free flame retardants is provided.
To achieve these goals, technical scheme is as follows:
A kind of preparation method of halogen-free flame retardants, including following step:
(1) Polyethylene Glycol that molecular weight is 400-600 is mixed for 1:1 with weight ratio with water, obtain Aqueous Solutions of Polyethylene Glycol, by aluminium hydroxide and Aqueous Solutions of Polyethylene Glycol stirring reaction 2-3h when temperature is 50-60 DEG C, obtain mixture, stop heating, add polyethylene, continue stirring reaction 2-3h, after having reacted, obtain mixture A；
(2) boric acid being configured to the boric acid aqueous solution that mass fraction is 2-5%, the hybrid reaction when nitrogen by boric acid aqueous solution and APP, wherein nitrogen flow is 5-8m3/ h, obtains mixture B after reaction 2-3h；
(3) in high-speed emulsifying machine, triguaiacyl phosphate and silane coupler are added at ambient temperature, when 6000-8000r/min, high speed shear dispersion 35-45min, obtain emulsion；
(4) the mixture A obtained in the mixture B obtained in the emulsion obtained in step (3), step (2) and step (1) is placed in reactor, after being sufficiently mixed reaction, vacuum drying, obtain halogen-free flame retardants finished product.
Wherein, raw material in parts by weight respectively, aluminium hydroxide 15-26 part, boric acid 2-6 part, APP 6-18 part, triguaiacyl phosphate 17-25 part, silane coupler 6-12 part, Polyethylene Glycol 20-35 part and polyethylene 15-30 part.
The preparation method of described halogen-free flame retardants, vacuum drying condition is pressure 42-45KPa, and temperature is 60-70 DEG C.
The halogen-free flame retardants that preparation method according to described halogen-free flame retardants obtains.
The using method of described halogen-free flame retardants, mixes halogen-free flame retardants with weight ratio 1:5 with water, is sprayed on and needs fire-retardant article surface.
Beneficial effects of the present invention is as follows:
Preparation method of the present invention is simple, and not halogen-containing in raw material, the halogen-free flame retardants prepared blazes up smokelessly, pollution-free, environmental protection.The halogen-free flameproof plastic cement prepared adopts UL94 standard testing to determine flame retardant rating, and after measured, halogen-free flameproof plastic cement flame retardant rating of the present invention is on V-1.
Detailed description of the invention:
For the technological means making the present invention realize, creation characteristic, reach purpose and effect and be easy to understand, below in conjunction with specific embodiment, the present invention is expanded on further.
Embodiment 1:
In the present embodiment, the preparation method of a kind of halogen-free flame retardants, including following step:
(1) Polyethylene Glycol that molecular weight is 400-600 is mixed for 1:1 with weight ratio with water, obtain Aqueous Solutions of Polyethylene Glycol, by aluminium hydroxide and Aqueous Solutions of Polyethylene Glycol stirring reaction 3h when temperature is 60 DEG C, obtain mixture, stop heating, add polyethylene, continue stirring reaction 2h, after having reacted, obtain mixture A；
(2) boric acid being configured to the boric acid aqueous solution that mass fraction is 5%, the hybrid reaction when nitrogen by boric acid aqueous solution and APP, wherein nitrogen flow is 8m3/ h, obtains mixture B after reaction 3h；
(3) in high-speed emulsifying machine, triguaiacyl phosphate and silane coupler are added at ambient temperature, when 8000r/min, high speed shear dispersion 45min, obtain emulsion；
(4) the mixture A obtained in the mixture B obtained in the emulsion obtained in step (3), step (2) and step (1) is placed in reactor, after being sufficiently mixed reaction, vacuum drying, vacuum drying condition is pressure 42KPa, temperature is 70 DEG C, obtains halogen-free flame retardants finished product.
Wherein, each raw material in parts by weight respectively, aluminium hydroxide 26 parts, boric acid 2 parts, APP 18 parts, triguaiacyl phosphate 17 parts, silane coupler 12 parts, Polyethylene Glycol 20 parts and polyethylene 30 parts.
The halogen-free flame retardants that preparation method according to described halogen-free flame retardants obtains.
The using method of described halogen-free flame retardants, mixes halogen-free flame retardants with weight ratio 1:5 with water, is sprayed on and needs fire-retardant article surface.
Preparation method of the present invention is simple, and not halogen-containing in raw material, the halogen-free flame retardants prepared blazes up smokelessly, pollution-free, environmental protection.The halogen-free flameproof plastic cement prepared adopts UL94 standard testing to determine flame retardant rating, and after measured, halogen-free flameproof plastic cement flame retardant rating of the present invention is V-0.
Embodiment 2:
In this enforcement, the preparation method of a kind of halogen-free flame retardants, including following step:
(1) Polyethylene Glycol that molecular weight is 400-600 is mixed for 1:1 with weight ratio with water, obtain Aqueous Solutions of Polyethylene Glycol, by aluminium hydroxide and Aqueous Solutions of Polyethylene Glycol stirring reaction 2h when temperature is 50 DEG C, obtain mixture, stop heating, add polyethylene, continue stirring reaction 3h, after having reacted, obtain mixture A；
(2) boric acid being configured to the boric acid aqueous solution that mass fraction is 2%, the hybrid reaction when nitrogen by boric acid aqueous solution and APP, wherein nitrogen flow is 5m3/ h, obtains mixture B after reaction 2h；
(3) in high-speed emulsifying machine, triguaiacyl phosphate and silane coupler are added at ambient temperature, when 8000r/min, high speed shear dispersion 35min, obtain emulsion；
(4) the mixture A obtained in the mixture B obtained in the emulsion obtained in step (3), step (2) and step (1) is placed in reactor, after being sufficiently mixed reaction, vacuum drying, vacuum drying condition is pressure 45KPa, temperature is 60 DEG C, obtains halogen-free flame retardants finished product.
Wherein, each raw material in parts by weight respectively, aluminium hydroxide 15 parts, boric acid 6 parts, APP 6 parts, triguaiacyl phosphate 25 parts, silane coupler 6 parts, Polyethylene Glycol 35 parts and polyethylene 15 parts.
The halogen-free flame retardants that preparation method according to described halogen-free flame retardants obtains.
The using method of described halogen-free flame retardants, mixes halogen-free flame retardants with weight ratio 1:5 with water, is sprayed on and needs fire-retardant article surface.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; described in above-described embodiment and description is that principles of the invention is described; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within the claimed scope of the invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (6)
1. the preparation method of a halogen-free flame retardants, it is characterised in that include following step:
(1) Polyethylene Glycol that molecular weight is 400-600 is mixed for 1:1 with weight ratio with water, obtain Aqueous Solutions of Polyethylene Glycol, by aluminium hydroxide and Aqueous Solutions of Polyethylene Glycol stirring reaction 2-3h when temperature is 50-60 DEG C, obtain mixture, stop heating, add polyethylene, continue stirring reaction 2-3h, after having reacted, obtain mixture A；
(2) boric acid being configured to the boric acid aqueous solution that mass fraction is 2-5%, the hybrid reaction when nitrogen by boric acid aqueous solution and APP, wherein nitrogen flow is 5-8m3/ h, obtains mixture B after reaction 2-3h；
(3) in high-speed emulsifying machine, triguaiacyl phosphate and silane coupler are added at ambient temperature, when 6000-8000r/min, high speed shear dispersion 35-45min, obtain emulsion；
(4) the mixture A obtained in the mixture B obtained in the emulsion obtained in step (3), step (2) and step (1) is placed in reactor, after being sufficiently mixed reaction, vacuum drying, obtain halogen-free flame retardants finished product；
Wherein, raw material in parts by weight respectively, aluminium hydroxide 15-26 part, boric acid 2-6 part, APP 6-18 part, triguaiacyl phosphate 17-25 part, silane coupler 6-12 part, Polyethylene Glycol 20-35 part and polyethylene 15-30 part.
2. the preparation method of halogen-free flame retardants according to claim 1, it is characterized in that, each raw material in parts by weight respectively, aluminium hydroxide 26 parts, boric acid 2 parts, APP 18 parts, triguaiacyl phosphate 17 parts, silane coupler 12 parts, Polyethylene Glycol 20 parts and polyethylene 30 parts.
3. the preparation method of halogen-free flame retardants according to claim 1, it is characterized in that, each raw material in parts by weight respectively, aluminium hydroxide 15 parts, boric acid 6 parts, APP 6 parts, triguaiacyl phosphate 25 parts, silane coupler 6 parts, Polyethylene Glycol 35 parts and polyethylene 15 parts.
4. the preparation method of halogen-free flame retardants according to claim 1, it is characterised in that vacuum drying condition is pressure 42-45KPa, and temperature is 60-70 DEG C.
5. the halogen-free flame retardants that the preparation method of the halogen-free flame retardants according to any of the above one claim obtains.
6. the using method of halogen-free flame retardants according to claim 5, it is characterised in that mixed with weight ratio 1:5 with water by halogen-free flame retardants, is sprayed on and needs fire-retardant article surface.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410342654.2A CN104130564B (en) | 2014-07-18 | 2014-07-18 | A kind of preparation method of halogen-free flame retardants |
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| CN104130564B true CN104130564B (en) | 2016-06-29 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468143A (en) * | 2013-08-16 | 2013-12-25 | 安徽快来防水防腐有限公司 | Polymer asphalt waterproof coating |
| CN103773214A (en) * | 2014-01-26 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Waterproof paint and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468143A (en) * | 2013-08-16 | 2013-12-25 | 安徽快来防水防腐有限公司 | Polymer asphalt waterproof coating |
| CN103773214A (en) * | 2014-01-26 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Waterproof paint and preparation process thereof |
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