CN102786041A - Method for preparing aluminum hypophosphite - Google Patents
Method for preparing aluminum hypophosphite Download PDFInfo
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- CN102786041A CN102786041A CN2012103024901A CN201210302490A CN102786041A CN 102786041 A CN102786041 A CN 102786041A CN 2012103024901 A CN2012103024901 A CN 2012103024901A CN 201210302490 A CN201210302490 A CN 201210302490A CN 102786041 A CN102786041 A CN 102786041A
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Abstract
The invention relates to a method for preparing aluminum hypophosphite. The method includes the following steps of firstly, preparing sodium hypophosphite solution with concentration of 2-6mol/L, adjusting pH (potential of hydrogen) to be 3-5 preferentially within 3-6.5; secondly, preparing aluminum sulfate solution; and thirdly, subjecting the sodium hypophosphite solution and the aluminum sulfate solution to reaction by heating on the acid condition to generate aluminum hypophosphite. The aluminum sulfate is added into the sodium hypophosphite solution for reaction within a certain temperature range, so that harms caused by volatilization of hypophosphorous acid during preparing of the aluminum hypophosphite are avoided, operation is simplified, yield of products is high, cost is low and industrialization is easy to realize.
Description
Technical field
The present invention relates to a kind of preparation method of compound, relate in particular to a kind of preparation method of hypo-aluminum orthophosphate.
Background technology
Phosphorus content is higher in the hypo-aluminum orthophosphate, and thermostability and stability to hydrolysis are good.It adopts the fire-retardant mode of condensed phase, and the body material is had the catalysis carbon-forming effect, can have complementary advantages with the collaborative use of other fire retardants, strengthens flame retardant properties, is a kind of synergistic flame retardant efficiently.
People such as Cheng Xian great waves in 2011 have reported hypo-aluminum orthophosphate synergistic melamine cyanurate fire-retardant to terpolymer EP rubber; Because its look white; Addition is little, make made fire retardant have better machining property, flame retardant properties and mechanical property (Cheng Xiantao, Jiang Hongwei. the research [J] of hypo-aluminum orthophosphate synergistic MCA fire retardant trielement ethylene-propylene rubber. elastomerics; 2011,21 (3): 59-63).Li Qi in 2011 flies also to have reported that employing acid-base neutralisation method synthesized hypo-aluminum orthophosphate; Studied its fire-retardant to PA6 simultaneously; Research show if a small amount of hypo-aluminum orthophosphate just can make PA6 obtain higher flame retardant effect (Li Qifei. the synthetic and fire-retardant Nylon 6 of hypophosphite fire retardant is studied; Northeast Forestry University, master thesis, 2011).Also there are not other reports now about the hypo-aluminum orthophosphate compound method.
And adopting Hypophosporous Acid, 50 to make reactant, suction Hypophosporous Acid, 50 steam or fog are bigger to the human injury, simultaneously environment and water body are had pollution.
Because the defective that the preparation method of above-mentioned existing hypo-aluminum orthophosphate exists, the design people actively studies innovation, in the hope of founding a kind of preparation method of new hypo-aluminum orthophosphate, makes it have more practicality.
Summary of the invention
Main purpose of the present invention is; Overcome the defective of preparing method's existence of existing hypo-aluminum orthophosphate; And a kind of preparation method of new hypo-aluminum orthophosphate is provided; Technical problem to be solved be make that its preparation process operation is simple, reaction conditions is gentle, the reaction times is short, power consumption is low, corrosion is little, pollution less, product is pure, productive rate is high, thereby be suitable for practicality more, and have the utility value on the industry.
For realizing the object of the invention and solve its technical problem, adopt following technical scheme:
A kind of preparation method of hypo-aluminum orthophosphate comprises following preparation process:
The first step: compound concentration is the sodium hypophosphite solution of 2～6mol/L, and adjusting PH is 3～6.5;
Second step: preparation alum liquor;
The 3rd step: said sodium hypophosphite solution is reacted with said alum liquor mixing post-heating, generate hypo-aluminum orthophosphate.
The mol ratio of aforementioned sodium hypophosphite and Tai-Ace S 150 is 5～9:1.
The Heating temperature in aforementioned the 3rd step is 40～100 ℃, preferred 50～100 ℃.
In the aforementioned the first step, preferably regulating the pH value is 3～5.
The preparation hypo-aluminum orthophosphate mainly adopts the neutralization reaction of Hypophosporous Acid, 50 and white lake to prepare in the prior art, because Hypophosporous Acid, 50 evaporable steam is bigger to human harm, so the present invention adopts the replacement(metathesis)reaction of sodium hypophosphite and Tai-Ace S 150 to prepare.Because the certain activation energy of reaction needed, so temperature can not be too low, but also can not be too high, and the hypo-aluminum orthophosphate of generation also can decompose when being higher than 200 ℃, emits highly toxic substance PH
3The temperature of reaction that the present invention recommends is 50～100 ℃, need control the pH value of sodium hypophosphite solution simultaneously, because of the acidity difference; The different solubility of hypo-aluminum orthophosphate; It is 3～5 that the present invention recommends pH, and this moment, the solubleness of product hypo-aluminum orthophosphate was minimum, the separating of carrying out that helps reacting and product.
Schematic diagram of the present invention is following:
After above-mentioned reaction end, cooling is filtered and is obtained thick product hypo-aluminum orthophosphate, adds water washing, filtration, drying again, just can obtain the higher title product of purity.
Beneficial effect of the present invention is:
1. react through in certain temperature range, Tai-Ace S 150 being added in the sodium hypophosphite solution, avoided the Hypophosporous Acid, 50 volatilization and the harm that brings, simplified operation, yield of product is higher, and cost is low, is easy to industriallization.
2. method products obtained therefrom productive rate of the present invention can reach more than 95% about 90-98% usually.
3. low in raw material cost of the present invention, technology are simple, and the better industrial prospect is arranged.
4. the prepared hypo-aluminum orthophosphate quality of the present invention is good, and purity is high.
5. the present invention is reflected at aqueous phase and carries out, and does not need complicated aftertreatment, and preparation process environmentally safe meets the requirement of Green Chemistry.
Above-mentioned explanation only is the general introduction of technical scheme of the present invention, understands technique means of the present invention in order can more to know, and can implement according to the content of specification sheets, below with preferred embodiment of the present invention specify as after.
Embodiment
Reach technique means and the effect that predetermined goal of the invention is taked for further setting forth the present invention, to its embodiment of preparation method, characteristic and the effect thereof of a kind of hypo-aluminum orthophosphate of proposing according to the present invention, specify as after.
Embodiment 1
, 500 mL, the four neck flasks of dimroth's condensing tube, electric mixer and TM add sodium hypophosphite 7.7 g in being housed, water 110 mL, and stirring and dissolving, dripping sulfuric acid accent pH is 3.
Heating sodium hypophosphite solution to 40 ℃ adds solution afterreaction 2 h that 50 mL contain 8.3 g 18 water Tai-Ace S 150, white precipitate.Filtration, washing, drying can get the white powder product.Yield is 80.9%.
Embodiment 2
, 500 mL, the four neck flasks of dimroth's condensing tube, electric mixer and TM add sodium hypophosphite 7.7 g in being housed, water 110 mL, and stirring and dissolving, transferring pH is 3.
Heating sodium hypophosphite solution to 50 ℃, Dropwise 50 mL contains solution afterreaction 2 h of 8.3 g 18 water Tai-Ace S 150, white precipitate.Filtration, washing, drying can get the white powder product.Yield is 91.9%.
Embodiment 3
, 500 mL, the four neck flasks of dimroth's condensing tube, electric mixer and TM add sodium hypophosphite 7.7 g in being housed, water 110 mL, and stirring and dissolving, transferring pH is 4.
Heating sodium hypophosphite solution to 80 ℃, Dropwise 50 mL contains solution afterreaction 2 h of 8.3 g 18 water Tai-Ace S 150, white precipitate.Filtration, washing, drying can get the white powder product.Yield is 95.9%.
Embodiment 4
, 500 mL, the four neck flasks of dimroth's condensing tube, electric mixer and TM add sodium hypophosphite 7.7 g in being housed, water 110 mL, and stirring and dissolving, transferring pH is 5.
Heating sodium hypophosphite solution to 100 ℃, Dropwise 50 mL contains solution afterreaction 2 h of 8.3 g 18 water Tai-Ace S 150, white precipitate.Filtration, washing, drying can get the white powder product.Yield is 82.9%.
Embodiment 5
, 500 mL, the four neck flasks of dimroth's condensing tube, electric mixer and TM add sodium hypophosphite 7.7 g in being housed, water 50 mL, and stirring and dissolving, transferring pH is 3～5.
Heating sodium hypophosphite solution to 60～70 ℃, Dropwise 50 mL contains solution afterreaction 2 h of 8.3 g 18 water Tai-Ace S 150, white precipitate.Filtration, washing, drying can get the white powder product.Yield is 97.9%.
Embodiment 6
, 500 mL, the four neck flasks of dimroth's condensing tube, electric mixer and TM add sodium hypophosphite 8.8 g in being housed, water 110 mL, and stirring and dissolving, transferring pH is 3～5.
Heating sodium hypophosphite solution to 70～80 ℃, Dropwise 50 mL contains solution afterreaction 2 h of 8.3 g 18 water Tai-Ace S 150, white precipitate.Filtration, washing, drying can get the white powder product.Yield is 96.9%.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limiting the present invention, anyly be familiar with the professional and technical personnel, in not breaking away from technical scheme scope of the present invention; When the technology contents of above-mentioned announcement capable of using is made a little change or is modified to the equivalent embodiment of equivalent variations; In every case be the content that does not break away from technical scheme of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (4)
1. the preparation method of a hypo-aluminum orthophosphate is characterized in that, described method may further comprise the steps:
The first step: compound concentration is the sodium hypophosphite solution of 2～6mol/L, and adjusting PH is 3～6.5;
Second step: preparation alum liquor;
The 3rd step: said sodium hypophosphite solution is reacted with said alum liquor mixing post-heating, generate hypo-aluminum orthophosphate.
2. the preparation method of hypo-aluminum orthophosphate according to claim 1 is characterized in that, the mol ratio of said sodium hypophosphite and said Tai-Ace S 150 is 5～9:1.
3. the preparation method of hypo-aluminum orthophosphate according to claim 1 is characterized in that, the Heating temperature in said the 3rd step is 40～100 ℃.
4. the preparation method of hypo-aluminum orthophosphate according to claim 1 is characterized in that, in the said the first step, the pH of sodium hypophosphite solution is 3～5.
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| CN2012103024901A CN102786041A (en) | 2012-08-24 | 2012-08-24 | Method for preparing aluminum hypophosphite |
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| CN2012103024901A CN102786041A (en) | 2012-08-24 | 2012-08-24 | Method for preparing aluminum hypophosphite |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103101893A (en) * | 2013-02-01 | 2013-05-15 | 河北联合大学 | Preparation method of highly dispersed aluminum orthophosphite crystals |
| CN103146022A (en) * | 2013-03-18 | 2013-06-12 | 南京师范大学 | Preparation method of aluminum phenylphosphinate |
| CN103145110A (en) * | 2013-03-18 | 2013-06-12 | 南京师范大学 | Preparation method of aluminium hypophosphite |
| CN103496681A (en) * | 2013-10-18 | 2014-01-08 | 上海美莱珀化工材料科技有限公司 | Method for preparing aluminum hypophosphite |
| CN103803516A (en) * | 2014-01-25 | 2014-05-21 | 北京理工大学 | Method for micron-scale aluminum hypophosphite by virtue of alcohol-water method |
| CN103879979A (en) * | 2014-03-13 | 2014-06-25 | 广东宇星阻燃新材有限公司 | Method for producing aluminium hypophosphite by adopting reaction extrusion process |
| CN104448948A (en) * | 2014-12-10 | 2015-03-25 | 山东川君化工股份有限公司 | Preparation method of modified aluminium hypophosphite |
| CN104860281A (en) * | 2015-06-01 | 2015-08-26 | 武汉理工大学 | Preparation method of aluminum hypophosphite |
| CN105860594A (en) * | 2016-05-10 | 2016-08-17 | 什邡市太丰新型阻燃剂有限责任公司 | Synthesis method of organosilicone modified superfine aluminum hypophosphite |
| CN106006589A (en) * | 2015-08-24 | 2016-10-12 | 湖北航天化学技术研究所 | Method for joint production of hypophosphite of calcium, magnesium and aluminum |
| CN106986318A (en) * | 2017-04-11 | 2017-07-28 | 四川福思达生物技术开发有限责任公司 | The method that glufosinate-ammonium by-product waste residue prepares hypo-aluminum orthophosphate |
| CN107973281A (en) * | 2017-12-01 | 2018-05-01 | 合肥学院 | Anhydrous tubular metal hypophosphite and preparation method thereof |
| CN111689481A (en) * | 2020-06-28 | 2020-09-22 | 山东泰星新材料股份有限公司 | Aluminum hypophosphite flame retardant ultrafine powder and preparation method and application thereof |
| CN111961254A (en) * | 2020-08-27 | 2020-11-20 | 湖北航天化学技术研究所 | Preparation method of modified aluminum hypophosphite flame retardant |
| CN113979412A (en) * | 2021-10-29 | 2022-01-28 | 湖北航天化学技术研究所 | Synthesis method of fine-particle-size low-cost aluminum hypophosphite flame retardant |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103101893B (en) * | 2013-02-01 | 2015-03-04 | 河北联合大学 | Preparation method of highly dispersed aluminum orthophosphite crystals |
| CN103101893A (en) * | 2013-02-01 | 2013-05-15 | 河北联合大学 | Preparation method of highly dispersed aluminum orthophosphite crystals |
| CN103146022A (en) * | 2013-03-18 | 2013-06-12 | 南京师范大学 | Preparation method of aluminum phenylphosphinate |
| CN103145110A (en) * | 2013-03-18 | 2013-06-12 | 南京师范大学 | Preparation method of aluminium hypophosphite |
| CN103146022B (en) * | 2013-03-18 | 2014-08-20 | 南京师范大学 | Preparation method of aluminum phenylphosphinate |
| CN103496681B (en) * | 2013-10-18 | 2015-09-02 | 上海美莱珀化工材料科技有限公司 | A kind of preparation method of hypo-aluminum orthophosphate |
| CN103496681A (en) * | 2013-10-18 | 2014-01-08 | 上海美莱珀化工材料科技有限公司 | Method for preparing aluminum hypophosphite |
| CN103803516A (en) * | 2014-01-25 | 2014-05-21 | 北京理工大学 | Method for micron-scale aluminum hypophosphite by virtue of alcohol-water method |
| CN103879979A (en) * | 2014-03-13 | 2014-06-25 | 广东宇星阻燃新材有限公司 | Method for producing aluminium hypophosphite by adopting reaction extrusion process |
| CN104448948A (en) * | 2014-12-10 | 2015-03-25 | 山东川君化工股份有限公司 | Preparation method of modified aluminium hypophosphite |
| CN104860281A (en) * | 2015-06-01 | 2015-08-26 | 武汉理工大学 | Preparation method of aluminum hypophosphite |
| CN106006589A (en) * | 2015-08-24 | 2016-10-12 | 湖北航天化学技术研究所 | Method for joint production of hypophosphite of calcium, magnesium and aluminum |
| CN105860594A (en) * | 2016-05-10 | 2016-08-17 | 什邡市太丰新型阻燃剂有限责任公司 | Synthesis method of organosilicone modified superfine aluminum hypophosphite |
| CN106986318A (en) * | 2017-04-11 | 2017-07-28 | 四川福思达生物技术开发有限责任公司 | The method that glufosinate-ammonium by-product waste residue prepares hypo-aluminum orthophosphate |
| CN107973281A (en) * | 2017-12-01 | 2018-05-01 | 合肥学院 | Anhydrous tubular metal hypophosphite and preparation method thereof |
| CN107973281B (en) * | 2017-12-01 | 2019-12-03 | 合肥学院 | Anhydrous tubular metal hypophosphite and preparation method thereof |
| CN111689481A (en) * | 2020-06-28 | 2020-09-22 | 山东泰星新材料股份有限公司 | Aluminum hypophosphite flame retardant ultrafine powder and preparation method and application thereof |
| CN111961254A (en) * | 2020-08-27 | 2020-11-20 | 湖北航天化学技术研究所 | Preparation method of modified aluminum hypophosphite flame retardant |
| CN113979412A (en) * | 2021-10-29 | 2022-01-28 | 湖北航天化学技术研究所 | Synthesis method of fine-particle-size low-cost aluminum hypophosphite flame retardant |
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Application publication date: 20121121 |