CN103523765A - Preparation method of aluminum dihydrogen tripolyphosphate - Google Patents
Preparation method of aluminum dihydrogen tripolyphosphate Download PDFInfo
- Publication number
- CN103523765A CN103523765A CN201210241912.9A CN201210241912A CN103523765A CN 103523765 A CN103523765 A CN 103523765A CN 201210241912 A CN201210241912 A CN 201210241912A CN 103523765 A CN103523765 A CN 103523765A
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- CN
- China
- Prior art keywords
- dihydrogen tripolyphosphate
- preparation
- aluminium dihydrogen
- shrend
- tripolyphosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
Abstract
The invention provides a preparation method of aluminum dihydrogen tripolyphosphate. The preparation method comprises the following steps of controlling the mole ratio of P/Al to be (1.7-3.5):1, adding Al(OH)3 into an H3PO4 aqueous solution of which the mass concentration is less than 85%, stirring, and keeping the temperature at 75-100 DEG C for 0.5-3 hours to obtain an intermediate aluminum hydrogen phosphate; calcining the intermediate aluminum hydrogen phosphate at 250-350 DEG C for 1-4 hours to obtain anhydrous aluminum dihydrogen tripolyphosphate. The preparation method of aluminum dihydrogen tripolyphosphate provided by the invention can shorten time and save energy, is easy to operate and realize industrial production, reduces the discharge of acidic wastewater and improves the conversion rate, and the obtained product is high in purity and good in quality.
Description
Technical field
The present invention relates to a kind of preparation method of phosphalugel, relate in particular to a kind of preparation method of aluminium dihydrogen tripolyphosphate.
Background technology
Aluminium dihydrogen tripolyphosphate is a kind of rust-stabilising pigment of high-efficiency environment friendly, is the ideal substitute of the toxic pigments such as red lead and chromic salt.At present, aluminium dihydrogen tripolyphosphate is generally polymerized by aluminum oxide or aluminium hydroxide and phosphoric acid dehydration, and concrete grammar is as follows: first aluminum oxide or aluminium hydroxide are pressed to certain molar ratio reaction with phosphorus aqueous acid, prepare intermediate acid aluminum phosphate; Then by intermediate calcining, obtain anhydrous aluminium dihydrogen tripolyphosphate; Anhydrous aluminium dihydrogen tripolyphosphate, through aquation, grinds, and further it is washed, filters, is dried, is pulverized, and finally obtains purer aluminium dihydrogen tripolyphosphate.The method has the following disadvantages: the production cycle is long, and energy consumption is high, causes production cost high; Be unfavorable for extensive continuous suitability for industrialized production; Reaction process can generate more impurity, and its water-soluble impurity must can be removed through washing, and after washing, the acid waste water of discharge pollutes the environment.
The Chinese patent CN1099719A authorizing on April 18th, 1994 has reported the crystallization that promotes acid aluminum phosphate by adding acid aluminum phosphate crystal seed and ethanol or propyl alcohol etc., by calcining acid phosphatase crystalline aluminophosphate, obtain aluminium dihydrogen tripolyphosphate, wherein calcination time 1.5～2h; Although shortening calcination time, this method makes processing step more complicated.The Chinese patent CA101172596A that on May 7th, 2008 authorizes has reported the method for preparing fast polyphosphoric acid salt by microwave radiation, under microwave condition, only need 30min can obtain polyphosphoric acid aluminum dihydrogen, the method has shortened the time of preparing polyphosphoric acid aluminum dihydrogen greatly, but microwave method is for scale operation, poor controllability.
Therefore, develop a kind of consuming time shortly, the preparation method of aluminium dihydrogen tripolyphosphate pigment who easily realizes suitability for industrialized production is significant.
Summary of the invention
In view of the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of aluminium dihydrogen tripolyphosphate, it can shorten the time, conserve energy.
The preparation method who another object of the present invention is to provide a kind of aluminium dihydrogen tripolyphosphate, it is easy to operate, easily realizes suitability for industrialized production.
Another object of the present invention is to provide a kind of preparation method of aluminium dihydrogen tripolyphosphate, it can reduce sour water discharge.
In order to realize object of the present invention, the invention provides a kind of preparation method of aluminium dihydrogen tripolyphosphate, comprise step: P/Al mol ratio is controlled at (1.7 ~ 3.5): in 1 scope, by Al (OH)
3joining mass concentration is the H below 85%
3pO
4in the aqueous solution, stir, and at 75 ~ 100 ℃ of insulation 0.5 ~ 3h, obtain intermediate acid aluminum phosphate; Intermediate acid aluminum phosphate, in 250 ℃ ~ 350 ℃ calcining 1 ~ 4h, is obtained to anhydrous aluminium dihydrogen tripolyphosphate.
Beneficial effect of the present invention is as follows.
The preparation method of a kind of aluminium dihydrogen tripolyphosphate provided by the invention, it can shorten the time, conserve energy; Easy to operate, be easy to suitability for industrialized production; Reduce sour water discharge; Improve transformation efficiency, the product purity obtaining is high, quality better.
Embodiment
First preparation method according to aluminium dihydrogen tripolyphosphate of the present invention is described.
Preparation method according to aluminium dihydrogen tripolyphosphate of the present invention, comprises step: P/Al mol ratio is controlled at (1.7 ~ 3.5): in 1 scope, by Al (OH)
3joining mass concentration is the H below 85%
3pO
4in the aqueous solution, stir, and at 75 ~ 100 ℃ of insulation 0.5 ~ 3h, obtain intermediate acid aluminum phosphate; Intermediate acid aluminum phosphate, in 250 ℃ ~ 350 ℃ calcining 1 ~ 4h, is obtained to anhydrous aluminium dihydrogen tripolyphosphate.
According in the preparation method of aluminium dihydrogen tripolyphosphate of the present invention, preferably, mass concentration is the H below 85%
3pO
4the aqueous solution is mixed by the pure water of the phosphoric acid that is 85% by mass concentration and 0 ~ 40% phosphoric acid amount.Phosphoric acid can be selected PHOSPHORIC ACID TECH.GRADE.
According in the preparation method of aluminium dihydrogen tripolyphosphate of the present invention, preferably, also can comprise step: the anhydrous aluminium dihydrogen tripolyphosphate obtaining is carried out to shrend, and after shrend, by the product after the filtration of shrend liquid, washing, dry filter.
According in the preparation method of aluminium dihydrogen tripolyphosphate of the present invention, preferably, the shrend liquid of shrend process is dilute phosphoric acid.
According in the preparation method of aluminium dihydrogen tripolyphosphate of the present invention, preferably, shrend temperature is 250 ℃ ~ 350 ℃.
Secondly explanation is according to the preparation method's of aluminium dihydrogen tripolyphosphate of the present invention embodiment.
Embodiment 1
By 200g mass concentration, be 85% industrial H
3pO
4add in the beaker of 500mL, under the condition stirring, in beaker, add 46g industry Al (OH) simultaneously
3, H
3pO
4with Al (OH)
3mol ratio be P/Al=2.9:1;
Above-mentioned mixed solution is heated to 75 ℃, and insulated and stirred 3h, obtains intermediate acid aluminum phosphate;
Intermediate acid aluminum phosphate is placed in to retort furnace, in 350 ℃ of calcining 1h, dehydration, condensation, obtains anhydrous aluminium dihydrogen tripolyphosphate;
Anhydrous aluminium dihydrogen tripolyphosphate is shifted out to retort furnace, be placed in rare H
3pO
4shrend in the time of 350 ℃ in solution;
Shrend liquid is filtered, and the product after washing, dry filter, obtains the dihydrate tripolyphosphate aluminium dihydride powder that median size is less than 10 μ m.
Embodiment 2
By 600g mass concentration, be 85% industrial H
3pO
4, 150g pure water adds in 1L beaker, under the condition stirring, adds 116g industry Al (OH) in beaker simultaneously
3, H
3pO
4with Al (OH)
3mol ratio be P/Al=3.5:1;
Above-mentioned mixed solution is heated to 100 ℃, and insulated and stirred 0.5h, obtains intermediate acid aluminum phosphate;
Intermediate acid aluminum phosphate is placed in to retort furnace, in 300 ℃ of calcining 4h, dehydration, condensation, obtains anhydrous aluminium dihydrogen tripolyphosphate;
Anhydrous aluminium dihydrogen tripolyphosphate is shifted out to retort furnace, be placed in rare H
3pO
4shrend in the time of 300 ℃ in solution;
Shrend liquid is filtered, and the product after washing, dry filter, obtains the dihydrate tripolyphosphate aluminium dihydride powder that median size is less than 10 μ m.
Embodiment 3
By 200g mass concentration, be 85% industrial H
3pO
4, 66g pure water adds in 500mL beaker, under the condition stirring, adds 79g industry Al (OH) in beaker simultaneously
3, H
3pO
4with Al (OH)
3mol ratio be P/Al=1.7:1;
Above-mentioned mixed solution is heated to 80 ℃, and insulated and stirred 2h, obtains intermediate acid aluminum phosphate;
Intermediate acid aluminum phosphate is placed in to retort furnace, in 250 ℃ of calcining 3h, dehydration, condensation, obtains anhydrous aluminium dihydrogen tripolyphosphate;
Anhydrous aluminium dihydrogen tripolyphosphate is shifted out to retort furnace, be placed in rare H
3pO
4shrend in the time of 250 ℃ in solution;
Shrend liquid is filtered, and the product after washing, dry filter, obtains the dihydrate tripolyphosphate aluminium dihydride powder that median size is less than 10 μ m.
Finally provide the preparation method's of the aluminium dihydrogen tripolyphosphate of the present invention detected result of embodiment.
Table 1 has provided the detected result of the final sample obtaining of embodiment 1-3.Detect and adopt XRD.
The detected result of the final sample obtaining of table 1 embodiment 1-3
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Quality product | 164g | 434g | 158g |
| Crest (2 θ angle) | 11.2° | 11.2° | 11.2° |
Claims (5)
1. a preparation method for aluminium dihydrogen tripolyphosphate, comprises step:
P/Al mol ratio is controlled at (1.7 ~ 3.5): in 1 scope, by Al (OH)
3joining mass concentration is the H below 85%
3pO
4in the aqueous solution, stir, and at 75 ~ 100 ℃ of insulation 0.5 ~ 3h, obtain intermediate acid aluminum phosphate;
Intermediate acid aluminum phosphate, in 250 ℃ ~ 350 ℃ calcining 1 ~ 4h, is obtained to anhydrous aluminium dihydrogen tripolyphosphate.
2. the preparation method of aluminium dihydrogen tripolyphosphate according to claim 1, is characterized in that, mass concentration is the H below 85%
3pO
4the aqueous solution is mixed by the pure water of the phosphoric acid that is 85% by mass concentration and 0 ~ 40% phosphoric acid amount.
3. the preparation method of aluminium dihydrogen tripolyphosphate according to claim 1, is characterized in that, also comprises step: the anhydrous aluminium dihydrogen tripolyphosphate obtaining is carried out to shrend, and after shrend, by the product after the filtration of shrend liquid, washing, dry filter.
4. the preparation method of aluminium dihydrogen tripolyphosphate according to claim 3, is characterized in that, the shrend liquid of shrend process is dilute phosphoric acid.
5. the preparation method of aluminium dihydrogen tripolyphosphate according to claim 4, is characterized in that, shrend temperature is 250 ℃ ~ 350 ℃.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210241912.9A CN103523765A (en) | 2012-07-04 | 2012-07-04 | Preparation method of aluminum dihydrogen tripolyphosphate |
| PCT/CN2013/078553 WO2014005498A1 (en) | 2012-07-04 | 2013-07-01 | Method for preparing aluminum dihydrogen tripolyphosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210241912.9A CN103523765A (en) | 2012-07-04 | 2012-07-04 | Preparation method of aluminum dihydrogen tripolyphosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103523765A true CN103523765A (en) | 2014-01-22 |
Family
ID=49881331
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210241912.9A Pending CN103523765A (en) | 2012-07-04 | 2012-07-04 | Preparation method of aluminum dihydrogen tripolyphosphate |
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| CN (1) | CN103523765A (en) |
| WO (1) | WO2014005498A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600766A (en) * | 2016-03-28 | 2016-05-25 | 广西民族大学 | Aluminum dihydrogen tripolyphosphate continuous production method and device |
| CN105621380A (en) * | 2016-04-08 | 2016-06-01 | 山东理工大学 | Simple method for efficiently preparing acicular aluminum dihydrogen phosphate |
| CN108516529A (en) * | 2018-04-24 | 2018-09-11 | 云南云天化以化磷业研究技术有限公司 | A kind of method that one step of polyphosphoric acid prepares aluminium dihydrogen tripolyphosphate |
| CN109534311A (en) * | 2018-12-06 | 2019-03-29 | 江苏申隆锌业有限公司 | A kind of preparation method of zinc aluminum phosphate |
| CN110116998A (en) * | 2018-02-05 | 2019-08-13 | 江苏省国盛稀土有限公司 | A kind of preparation method of high-purity aluminium metaphosphate powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1099719A (en) * | 1994-04-18 | 1995-03-08 | 郑州金岭化工有限公司 | Method for preparing dihydrate tripolyphosphate aluminium dihydride |
| JP2003063811A (en) * | 2001-08-28 | 2003-03-05 | Central Glass Co Ltd | Method for producing aluminum metaphosphate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61286209A (en) * | 1985-06-11 | 1986-12-16 | Teikoku Kako Kk | Production of condensed aluminum phosphate |
-
2012
- 2012-07-04 CN CN201210241912.9A patent/CN103523765A/en active Pending
-
2013
- 2013-07-01 WO PCT/CN2013/078553 patent/WO2014005498A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1099719A (en) * | 1994-04-18 | 1995-03-08 | 郑州金岭化工有限公司 | Method for preparing dihydrate tripolyphosphate aluminium dihydride |
| JP2003063811A (en) * | 2001-08-28 | 2003-03-05 | Central Glass Co Ltd | Method for producing aluminum metaphosphate |
Non-Patent Citations (2)
| Title |
|---|
| 袁爱群: "三聚磷酸二氢铝二水物的合成和表征", 《广西科学》, vol. 7, no. 4, 31 December 2000 (2000-12-31), pages 266 - 269 * |
| 袁爱群: "三聚磷酸二氢铝二水物的合成工艺", 《四川化工与腐蚀控制》, vol. 3, no. 3, 30 June 2000 (2000-06-30), pages 9 - 12 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600766A (en) * | 2016-03-28 | 2016-05-25 | 广西民族大学 | Aluminum dihydrogen tripolyphosphate continuous production method and device |
| CN105600766B (en) * | 2016-03-28 | 2017-06-16 | 广西民族大学 | A kind of aluminium dihydrogen tripolyphosphate continuous producing method and device |
| CN105621380A (en) * | 2016-04-08 | 2016-06-01 | 山东理工大学 | Simple method for efficiently preparing acicular aluminum dihydrogen phosphate |
| CN110116998A (en) * | 2018-02-05 | 2019-08-13 | 江苏省国盛稀土有限公司 | A kind of preparation method of high-purity aluminium metaphosphate powder |
| CN108516529A (en) * | 2018-04-24 | 2018-09-11 | 云南云天化以化磷业研究技术有限公司 | A kind of method that one step of polyphosphoric acid prepares aluminium dihydrogen tripolyphosphate |
| CN108516529B (en) * | 2018-04-24 | 2021-08-27 | 云南云天化以化磷业研究技术有限公司 | Method for preparing aluminum dihydrogen tripolyphosphate by polyphosphoric acid in one step |
| CN109534311A (en) * | 2018-12-06 | 2019-03-29 | 江苏申隆锌业有限公司 | A kind of preparation method of zinc aluminum phosphate |
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| Publication number | Publication date |
|---|---|
| WO2014005498A1 (en) | 2014-01-09 |
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Application publication date: 20140122 |