CN102225952A - Tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant and preparation method thereof - Google Patents
Tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant and preparation method thereof Download PDFInfo
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- CN102225952A CN102225952A CN2011100948227A CN201110094822A CN102225952A CN 102225952 A CN102225952 A CN 102225952A CN 2011100948227 A CN2011100948227 A CN 2011100948227A CN 201110094822 A CN201110094822 A CN 201110094822A CN 102225952 A CN102225952 A CN 102225952A
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- triazine
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Abstract
The invention discloses a tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant and a preparation method thereof. The fire retardant has characteristics of low cost, sufficient source, and does not contain halogen. The preparation method is characterized in that: the method does not adopt antimony oxide as a synergist; a resulting tris-(N,N-dihydroxyethylamino)-s-triazine compound is subjected to a heating reaction with one compound selected from phosphorus pentoxide, pyrophosphoric acid or polyphosphate to generate the tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant. The tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant has good dispersibility, good physical property, good mechanical property, good heat stability, good fire resistance property, high efficiency, low smoke and no generation of toxic gas.
Description
Technical field
The engineering synthetic technical field that the present invention relates to organise refers to a kind of three (N, N-dihydroxy ethyl amino)-s-triazine phosphate flame retardants and preparation method thereof especially.
Background technology
Fire retardant claims incombustible agent again; flame-proofing agent or fireproofing agent; fire retardant takes place in fire preventing; aspects such as protection people's lives and properties have become indispensable product; through the material after the fire retardant processing; when being subjected to extraneous burning things which may cause a fire disaster and attacking, can stop, delay or stop flame transmission effectively, thereby reach fire-retardant effect.
Application along with modern high-and-new science and technology, single fire retardant can not satisfy market far away to the demand of its performance, emit a large amount of hydrogen halides when the material combustion such as halogen containing flame-retardant, and then suction forms and has the haloid acid of severe corrosive and cause the secondary public hazards.Fire retardant Halogen cry grows to even greater heights now, and halogen containing flame-retardant is difficult in 21 century and obtains large development.
Cyanuric chloride is a kind of nitrogen heterocyclic ring Organic Chemicals, the source is sufficient, cheap, has stable triazine nitrogen heterocyclic chemical structure, utilize the stronger characteristic of its chlorine atom activity, by functional group's displacement and reaction, synthetic a kind of is the fire retardant of main component with phosphorus, nitrogen, not halogen-containing, also not adopting weisspiessglanz is synergist.When the superpolymer that contains fire retardant was heated, the surface can generate the layer of even flame-retardant layer, played heat insulation, oxygen barrier, pressed down the effect of cigarette, and have good flame retardancy.Expansion type flame retardant meets the development trend that requires the few cigarette of fire retardant, low toxicity now, is considered to realize one of non-halogen approach that gets a good chance of of fire retardant.
Summary of the invention
A kind of three (N of the present invention, N-dihydroxy ethyl amino)-the s-triazine phosphate flame retardant and preparation method thereof, it is characterized in that having cheap, source abundance, and it is not halogen-containing, also not adopting weisspiessglanz is synergist, synthetics has good dispersiveness, physics, mechanical property, thermostability and flame retardant properties, and efficient, hangs down cigarette, does not produce toxic gas.
To achieve these goals, technical solution of the present invention is: cyanuric chloride and the reaction of double hydroxyethyl amine, introduce the water soluble ethoxyl amino group, its reaction generates contains the multi-hydroxy ethyl aminocompound and Vanadium Pentoxide in FLAKES carries out esterification, add double hydroxyethyl amine again and carry out esterification and introduce water soluble hydroxy, specifically comprise following steps:
1). with ethanol is solvent, and cyanuric chloride (I) and double hydroxyethyl amine react 5～7h under 60 ℃～90 ℃ under the alkaline catalysts effect, generate compound three (N, N-dihydroxy ethyl amino)-s-triazine (II), and its chemical reaction is:
Further be, described catalyzer carbonic acid sodium, the mol ratio of cyanuric chloride and double hydroxyethyl amine is 1: 3～3.2.2). compound (II) and one or more the reacting by heating 4～6h under 80 ℃～110 ℃ temperature wherein that contain Vanadium Pentoxide in FLAKES, tetra-sodium or polyphosphoric acid generate three (N, N-dihydroxy ethyl amino)-s-triazine organic phosphate flame-retardant immunomodulator compounds.
Further be that described compound (II) is 1: 2～3.3 with the mol ratio of Vanadium Pentoxide in FLAKES, tetra-sodium or polyphosphoric acid.
Embodiment
Embodiment 1
In the reactor that whipping appts, reflux and temperature controller are housed, add 92kg cyanuric chloride (I), 50kg ethanol, 158kg double hydroxyethyl amine, 12kg sodium hydroxide and 62kg yellow soda ash, react 7h down in 70 ℃, reaction mixture in the reactor is cooled to below 100 ℃, after adding 72kg Vanadium Pentoxide in FLAKES and 127kg polyphosphoric acid, to 100 ℃ of insulation reaction 5h, be cooled to below 60 ℃, get final product product.
Embodiment 2
In the reactor that whipping appts, reflux and temperature controller are housed, add 156kg cyanuric chloride (I), 50kg ethanol, 268kg double hydroxyethyl amine, 22kg sodium hydroxide and 100kg yellow soda ash, react 7h down in 70 ℃, reaction mixture in the reactor is cooled to below 100 ℃, after adding 255kg Vanadium Pentoxide in FLAKES and 284kg tetra-sodium, in 90 ℃ of insulation reaction 4h, be cooled to below 60 ℃, get final product product.
The above; embodiment only is that preferred implementation of the present invention is described; be not that scope of the present invention is limited; under the prerequisite of the spirit that does not break away from the technology of the present invention; various distortion and improvement that this area engineering technical personnel make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (2)
1. (N, N-dihydroxy ethyl amino)-the s-triazine phosphate flame retardant and preparation method thereof, it is characterized in that: be solvent with ethanol, cyanuric chloride (I) and double hydroxyethyl amine react 5～7h down in 60 ℃～90 ℃ under the alkaline catalysts effect, generate compound three (N, N-dihydroxy ethyl amino)-s-triazine (II) again with contain Vanadium Pentoxide in FLAKES, tetra-sodium or polyphosphoric acid reacting by heating 4～6h under 80 ℃～110 ℃ temperature, generate three (N, N-dihydroxy ethyl amino)-s-triazine organic phosphate flame-retardant immunomodulator compounds.
2. according to right 1 described a kind of three (N, N-dihydroxy ethyl amino)-s-triazine phosphate flame retardants and preparation method thereof, it is characterized in that: compound (II) with contain in Vanadium Pentoxide in FLAKES, tetra-sodium, the polyphosphoric acid one or more and react.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100948227A CN102225952A (en) | 2011-04-05 | 2011-04-05 | Tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100948227A CN102225952A (en) | 2011-04-05 | 2011-04-05 | Tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant and preparation method thereof |
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| CN102225952A true CN102225952A (en) | 2011-10-26 |
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| CN2011100948227A Pending CN102225952A (en) | 2011-04-05 | 2011-04-05 | Tris-(N,N-dihydroxyethylamino)-s-triazine phosphate ester fire retardant and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643438A (en) * | 2012-05-15 | 2012-08-22 | 福建师范大学 | Solvent-free preparation method for char formation flame-retardant nitrogen and phosphorus-contained hyperbranched polymer |
| CN102660059A (en) * | 2012-05-15 | 2012-09-12 | 福建师范大学 | Preparation method of flame-resistant polyolefin composite |
| CN102702262A (en) * | 2012-05-18 | 2012-10-03 | 广州朗腾聚氨酯有限公司 | Preparation method of melamine polyolphosphateester |
| CN103265577A (en) * | 2013-05-20 | 2013-08-28 | 青岛大学 | Preparation method of novel flame retardant for cotton |
| CN103409995A (en) * | 2013-07-17 | 2013-11-27 | 常州纺织服装职业技术学院 | Phosphorous acid diethanolamine and preparation method thereof |
| CN109705942A (en) * | 2019-02-28 | 2019-05-03 | 盘锦辽河油田大力集团有限公司 | A kind of preparation method of steric hindrance amine type desulfurization and decarburization agent |
-
2011
- 2011-04-05 CN CN2011100948227A patent/CN102225952A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643438A (en) * | 2012-05-15 | 2012-08-22 | 福建师范大学 | Solvent-free preparation method for char formation flame-retardant nitrogen and phosphorus-contained hyperbranched polymer |
| CN102660059A (en) * | 2012-05-15 | 2012-09-12 | 福建师范大学 | Preparation method of flame-resistant polyolefin composite |
| CN102643438B (en) * | 2012-05-15 | 2013-11-20 | 福建师范大学 | Solvent-free preparation method for char formation flame-retardant nitrogen and phosphorus-contained hyperbranched polymer |
| CN102660059B (en) * | 2012-05-15 | 2014-06-18 | 福建师范大学 | Preparation method of flame-resistant polyolefin composite |
| CN102702262A (en) * | 2012-05-18 | 2012-10-03 | 广州朗腾聚氨酯有限公司 | Preparation method of melamine polyolphosphateester |
| CN103265577A (en) * | 2013-05-20 | 2013-08-28 | 青岛大学 | Preparation method of novel flame retardant for cotton |
| CN103265577B (en) * | 2013-05-20 | 2015-05-27 | 青岛大学 | Preparation method of novel flame retardant for cotton |
| CN103409995A (en) * | 2013-07-17 | 2013-11-27 | 常州纺织服装职业技术学院 | Phosphorous acid diethanolamine and preparation method thereof |
| CN109705942A (en) * | 2019-02-28 | 2019-05-03 | 盘锦辽河油田大力集团有限公司 | A kind of preparation method of steric hindrance amine type desulfurization and decarburization agent |
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Free format text: CORRECT: ADDRESS; FROM: 264006 YANTAI, SHANDONG PROVINCE TO: 276826 RIZHAO, SHANDONG PROVINCE Free format text: CORRECT: INVENTOR; FROM: LIU FANGXU TO: SI YINKUI |
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Effective date of registration: 20120625 Address after: 601, room 2, unit 5, building 35, No. five, Haibin Road, Donggang District, Shandong, Rizhao City 276826, China Applicant after: Si Yinkui Address before: 264006, No. 1, building 16, sun rise District, Yantai Development Zone, Shandong, 4 Applicant before: Liu Fangxu |
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Application publication date: 20111026 |