CN105645369A - Preparation method of Al(H2PO4)3 crystal powder - Google Patents
Preparation method of Al(H2PO4)3 crystal powder Download PDFInfo
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- CN105645369A CN105645369A CN201610213649.0A CN201610213649A CN105645369A CN 105645369 A CN105645369 A CN 105645369A CN 201610213649 A CN201610213649 A CN 201610213649A CN 105645369 A CN105645369 A CN 105645369A
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- dihydrogen phosphate
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- aluminium dihydrogen
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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
- C01B25/36—Aluminium phosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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Abstract
An efficient preparation method of Al(H2PO4)3 crystal powder is characterized by comprising steps as follows: (1) a solution is prepared from a phosphoric acid solution, ammonia water and distilled water, and then aluminum nitrate and urea are added to the solution; (2) iodine (I2) powder and cetyl ethyl morpholine ethyl ammonium sulfate are added to the solution; (3) the solution is heated to 85-98 DEG C, continuously stirred, then naturally cooled to the room temperature, left to stand and age for 3 h, filtered and separated, a product is washed with absolute ethyl alcohol and dried for 2-4 h, and thus the Al(H2PO4)3 crystal powder with excellent water solubility is prepared. The yield of Al(H2PO4)3 prepared with the method is up to 93.6wt% at most, and the economic and social value is very high.
Description
Technical field
The present invention is to provide the aluminium dihydrogen phosphate (Al (H that a kind of efficient water soluble characteristic is excellent2PO4)3) preparation method of crystalline solid powder, belong to technical field of preparation for inorganic material.
Background technology
Aluminium dihydrogen phosphate (Al (H2PO4)3) application in the industrial production is widely, there is the advantages such as high temperature resistant, anti-strip, anti-vibration, and there is excellent ultraviolet absorption ability, insulating properties, INFRARED ABSORPTION performance, electrical insulation capability, fire resistances etc., can be used as the binding agent of refractory material and ceramic material, the reinforcing agent of ceramic material, the intumescent paints of fiber, timber, paper etc., high temperature insulation goods etc. Aluminium dihydrogen phosphate generally exists in liquid or powder form. But, the aluminium dihydrogen phosphate of liquid can not be used alone, and expensive, is not easy to long-distance transport, this strongly limits the application of liquid phosphoric acid aluminum dihydrogen and popularization. Pulverous aluminium dihydrogen phosphate is less costly, it is simple to packaging and long-distance transport, is conducive to application and promotes. But, aluminium dihydrogen phosphate is soluble in water, the easy moisture absorption, it is difficult to dry, is difficult to produce desirable product by current production method. Japanese plum is prepared for the aluminium dihydrogen phosphate of paste entirely, then utilizes vacuum drying method to prepare biphosphate aluminium powder (prepare the research of water-soluble powder high-temperature agglomerant aluminium dihydrogen phosphate, " inorganic chemicals industry ", the 9th phase in 1984,10-11 page). But, the method is owing to have employed excessive phosphate, and in final product, meeting nubbin phosphoric acid and (or) phosphate, affect performance and the application of aluminium dihydrogen phosphate. In addition, Zhang Zhen emerging grade (production of material level aluminium dihydrogen phosphate and application, print during chemical industry, 9th phase in 2011,20-22 page) utilize hot blast centrifugal spray drying method to be prepared for aluminium dihydrogen phosphate powdery solid, but the method requires material moment rapid draing at 480-520 DEG C of temperature, and the requirement of equipment, process conditions is harsher.
Dry to overcome aluminium dihydrogen phosphate to be difficult to, process of vacuum drying is prone to residual impurity, and hot blast centrifugal spray drying to technological requirement harsh etc. the problem of problem, the preparation method that invention provides a kind of efficient, simple, safe and reliable, easily operated, with low cost, purity is high, water soluble characteristic is excellent biphosphate aluminium powder, the party's ratio juris is: generate aluminium dihydrogen phosphate crystalline solid first in the solution, it is then passed through filter, washing, dries, the highly purified biphosphate aluminium powder of excellent water-solubility can be prepared.
Summary of the invention
The preparation method that this technology provides a kind of efficient, simple, safe and reliable, easily operated, with low cost, purity is high, water soluble characteristic is excellent biphosphate aluminium powder, its technical scheme is:
A kind of efficient aluminium dihydrogen phosphate (Al (H2PO4)3) preparation method of crystalline solid powder, it is characterised in that adopt following steps: (1) concentration to be the phosphoric acid solution of 80wt%, concentration the be ammonia of 30wt% with distilled water by volume proportions for 10:3:5 become solution;Then aluminum nitrate, carbamide being joined in solution, wherein the mol ratio of aluminum nitrate, phosphoric acid and carbamide is: 1:3:1 ~ 4; (2) iodine (I is added in the solution2) powder, cetyl ethyl morpholine ethyl sulfuric acid ammonium, and control iodine powder, the addition of cetyl ethyl morpholine ethyl sulfuric acid ammonium is the 0.015% of solution quality, 0.1% respectively; (3) solution is heated to 85 ~ 98 DEG C, and by agitator continuous stirring 5 ~ 8 hours; Stirring naturally cools to room temperature solution after terminating, then static, ageing 3 hours, it is filtered again, separates, and with absolute ethanol washing product 3 times, then at 60 ~ 80 DEG C dry 2 ~ 4 hours, namely prepare the aluminium dihydrogen phosphate crystalline solid powder that water soluble characteristic is excellent.
Fig. 1 is the aluminium dihydrogen phosphate prepared of the technology of the present invention crystalline solid photo in the solution; As we can see from the figure: aluminium dihydrogen phosphate crystalline solid deposits to the bottom of container, and the boundary line between supernatant is perfectly clear.
The present invention compared with prior art, has the advantage that
1. the technology of the present invention is using iodine powder and cetyl ethyl morpholine ethyl sulfuric acid ammonium as crystallization medium, effectively facilitate the generation of aluminium dihydrogen phosphate crystalline solid, and the output capacity of the aluminium dihydrogen phosphate prepared by the technology of the present invention is high, can reach about 93.6wt%, there is high economy and social value;
2. the aluminium dihydrogen phosphate prepared by this technological invention has excellent water soluble characteristic, and there is fabulous stability, namely just can be configured to the as clear as crystal aluminium dihydrogen phosphate aqueous solution that concentration is 50wt% under room temperature, and after static 24 hours, find no aluminium dihydrogen phosphate or other materials precipitate out;
3. the technology of the present invention absolute ethanol washing aluminium dihydrogen phosphate crystalline solid, can effectively remove the impurity remained on aluminium dihydrogen phosphate crystalline solid, such as a small amount of unreacted phosphate anion, aluminium ion, nitrate ion etc., the purity of the aluminium dihydrogen phosphate crystalline solid therefore prepared is high, is substantially free of impurity;
4. the technology of the present invention absolute ethanol washing aluminium dihydrogen phosphate crystalline solid, can effectively remove the moisture of the overwhelming majority that aluminium dihydrogen phosphate crystalline solid surface is adsorbed, and ethanol is volatile, therefore biphosphate aluminium powder can be dried easily, and after sealed package, it is suitable for long-distance transport and long term storage. Additionally, the biphosphate aluminium powder that washing with alcohol is crossed, it is also possible to need not dry as required, but directly pack, have no effect on the convenience of its long-distance transport.
Detailed description of the invention
Embodiment 1
The ammonia of concentration to be the phosphoric acid solution of 80wt%, concentration be 30wt% with distilled water by volume proportions for 10:3:5 become solution; Then aluminum nitrate and carbamide are joined in solution, wherein aluminum nitrate, carbamide addition be 1/3 and 1 times of molal quantity of phosphoric acid respectively; Add iodine (I in the solution2) powder, cetyl ethyl morpholine ethyl sulfuric acid ammonium, and control iodine powder, the addition of cetyl ethyl morpholine ethyl sulfuric acid ammonium is the 0.015% of solution quality, 0.1% respectively; Solution is heated to 98 DEG C, and by agitator continuous stirring 5 hours; Stirring naturally cools to room temperature solution after terminating, then static, ageing 3 hours, then is filtered, separates, and by absolute ethanol washing filtration product 3 times, then dries 4 hours at 60 DEG C. Found by XRD, infrared analysis: the crystalline phase of powder prepared by the present invention is aluminium dihydrogen phosphate crystalline solid; Under room temperature, aluminium dihydrogen phosphate prepared by the present invention is dissolved in water, can be configured to the as clear as crystal aluminium dihydrogen phosphate aqueous solution that concentration is 50wt%, and after static 24 hours, finds no aluminium dihydrogen phosphate or other materials precipitate out;By calculating: the output capacity (actual production is divided by calculated theoretical yield) of aluminium dihydrogen phosphate prepared by the technology of the present invention is 92.8wt%.
Embodiment 2
The ammonia of concentration to be the phosphoric acid solution of 80wt%, concentration be 30wt% with distilled water by volume proportions for 10:3:5 become solution; Then aluminum nitrate, carbamide are joined in solution, wherein aluminum nitrate, carbamide addition be 1/3 and 3 times of molal quantity of phosphoric acid respectively; Add iodine (I in the solution2) powder, cetyl ethyl morpholine ethyl sulfuric acid ammonium, and control iodine powder, the addition of cetyl ethyl morpholine ethyl sulfuric acid ammonium is the 0.015% of solution quality, 0.1% respectively; Solution is heated to 92 DEG C, and by agitator continuous stirring 7 hours; Stirring naturally cools to room temperature solution after terminating, then static, ageing 3 hours, then is filtered, separates, and by absolute ethanol washing filtration product 3 times, then dries 4 hours at 70 DEG C. Found by XRD, infrared analysis: the crystalline phase of powder prepared by the present invention is aluminium dihydrogen phosphate crystalline solid; Under room temperature, aluminium dihydrogen phosphate prepared by the present invention is dissolved in water, is configured to the as clear as crystal aluminium dihydrogen phosphate aqueous solution that concentration is 50wt%, and after static 24 hours, finds no aluminium dihydrogen phosphate or other materials precipitate out; By calculating: the output capacity (actual production is divided by calculated theoretical yield) of aluminium dihydrogen phosphate prepared by the technology of the present invention is 93.1wt%.
Embodiment 3
The ammonia of concentration to be the phosphoric acid solution of 80wt%, concentration be 30wt% with distilled water by volume proportions for 10:3:5 become solution; Then aluminum nitrate and carbamide are joined in solution, wherein aluminum nitrate, carbamide addition be 1/3 and 4 times of molal quantity of phosphoric acid respectively; Add iodine (I in the solution2) powder, cetyl ethyl morpholine ethyl sulfuric acid ammonium, and control iodine powder, the addition of cetyl ethyl morpholine ethyl sulfuric acid ammonium is the 0.015% of solution quality, 0.1% respectively; Solution is heated to 85 DEG C, and by agitator continuous stirring 8 hours; Stirring naturally cools to room temperature solution after terminating, then static, ageing 3 hours, then is filtered, separates, and by absolute ethanol washing filtration product 3 times, then dries 2 hours at 80 DEG C. Found by XRD, infrared analysis: powder prepared by the technology of the present invention is aluminium dihydrogen phosphate crystal; Under room temperature, aluminium dihydrogen phosphate prepared by the technology of the present invention is dissolved in water, is configured to the as clear as crystal aluminium dihydrogen phosphate aqueous solution that concentration is 50wt%, and after static 24 hours, finds no aluminium dihydrogen phosphate or other materials precipitate out; By calculating: the output capacity (actual production is divided by calculated theoretical yield) of aluminium dihydrogen phosphate prepared by the technology of the present invention is 93.6wt%.
Claims (1)
1. an efficient aluminium dihydrogen phosphate (Al (H2PO4)3) preparation method of crystalline solid powder, it is characterised in that adopt following steps: (1) concentration to be the phosphoric acid solution of 80wt%, concentration the be ammonia of 30wt% with distilled water by volume proportions for 10:3:5 become solution; Then aluminum nitrate, carbamide being joined in solution, wherein the mol ratio of aluminum nitrate, phosphoric acid and carbamide is: 1:3:1 ~ 4; ; (2) iodine (I is added in the solution2) powder, cetyl ethyl morpholine ethyl sulfuric acid ammonium, and control iodine powder, the addition of cetyl ethyl morpholine ethyl sulfuric acid ammonium is the 0.015% of solution quality, 0.1% respectively;(3) solution is heated to 85 ~ 98 DEG C, and by agitator continuous stirring 5 ~ 8 hours; Stirring naturally cools to room temperature solution after terminating, then static, ageing 3 hours, it is filtered again, separates, and with absolute ethanol washing product 3 times, then at 60 ~ 80 DEG C dry 2 ~ 4 hours, namely prepare the aluminium dihydrogen phosphate crystalline solid powder that water soluble characteristic is excellent.
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| CN201610213649.0A CN105645369B (en) | 2016-04-08 | 2016-04-08 | A kind of preparation method of aluminium dihydrogen phosphate crystalline solid powder |
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| CN201610213649.0A CN105645369B (en) | 2016-04-08 | 2016-04-08 | A kind of preparation method of aluminium dihydrogen phosphate crystalline solid powder |
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| CN105645369A true CN105645369A (en) | 2016-06-08 |
| CN105645369B CN105645369B (en) | 2017-10-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459024A (en) * | 2017-07-28 | 2017-12-12 | 贵州大学 | The method that submicron-sized particulate aluminium dihydrogen phosphate powder is prepared in pelite |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51128698A (en) * | 1975-05-02 | 1976-11-09 | Teikoku Kako Kk | The manufacturing process of the aluminum phosphate |
| GB2204860A (en) * | 1987-05-19 | 1988-11-23 | China Petrochemical Dev Corp | Preparing aluminium dihydrogen tripolyphosphate dihydrate |
| JPH03146410A (en) * | 1989-11-01 | 1991-06-21 | Teika Corp | Production of aluminum primary tripolyphosphate |
| JP2003063811A (en) * | 2001-08-28 | 2003-03-05 | Central Glass Co Ltd | Method for producing aluminum metaphosphate |
-
2016
- 2016-04-08 CN CN201610213649.0A patent/CN105645369B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51128698A (en) * | 1975-05-02 | 1976-11-09 | Teikoku Kako Kk | The manufacturing process of the aluminum phosphate |
| GB2204860A (en) * | 1987-05-19 | 1988-11-23 | China Petrochemical Dev Corp | Preparing aluminium dihydrogen tripolyphosphate dihydrate |
| JPH03146410A (en) * | 1989-11-01 | 1991-06-21 | Teika Corp | Production of aluminum primary tripolyphosphate |
| JP2003063811A (en) * | 2001-08-28 | 2003-03-05 | Central Glass Co Ltd | Method for producing aluminum metaphosphate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459024A (en) * | 2017-07-28 | 2017-12-12 | 贵州大学 | The method that submicron-sized particulate aluminium dihydrogen phosphate powder is prepared in pelite |
| CN107459024B (en) * | 2017-07-28 | 2020-03-17 | 贵州大学 | Method for preparing ultrafine-grained aluminum dihydrogen phosphate powder in aluminous rock |
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| CN105645369B (en) | 2017-10-10 |
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Granted publication date: 20171010 Termination date: 20180408 |