CN104591238A - Preparation method for ammonium-polyphosphate-doped magnesium aluminium hydrotalcite - Google Patents
Preparation method for ammonium-polyphosphate-doped magnesium aluminium hydrotalcite Download PDFInfo
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- CN104591238A CN104591238A CN201410729207.2A CN201410729207A CN104591238A CN 104591238 A CN104591238 A CN 104591238A CN 201410729207 A CN201410729207 A CN 201410729207A CN 104591238 A CN104591238 A CN 104591238A
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- deionized water
- hydrotalcite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a preparation method for ammonium-polyphosphate-doped magnesium aluminium hydrotalcite. The preparation method comprises: fully grinding magnesium sulfate and aluminium nitrate in a mortar, putting the grinded mixed powder into deionized water for dissolving, adding sodium hydroxide and an anhydrous sodium carbonate solution with stirring, keep pH at 9-12, performing magnetic stirring at room temperature for 20 min, then adding urea and deionized water, heating to 50 DEG C and stirring for 1 h, after the reaction is finished, putting the slurry into a microwave extraction instrument, controlling the power to be 500 W, crystallizing at 150 DEG C, drying, grinding into a powder, putting the crystal powder into a reaction flask, adding deionized water and APP, heating to 120 DEG C, slowly stirring, after the reaction is finished, ageing in the pot for 10 h, cooling and drying, so as to obtain ammonium-polyphosphate-doped magnesium aluminium hydrotalcite. The method is economic and practical, low in cost, simple in technology, high in efficiency and high in quality.
Description
Technical field
The invention belongs to field of fine chemical, relate to a kind of preparation method of the ammonium polyphosphate magnesium aluminum-hydrotalcite that adulterates.
Background technology
Hydrotalcite is the two first chance complex metal oxides (LDC) of a kind of layer column.1842 at Switzerland's Late Cambrian hydrotalcite mineral, hydrotalcite has the anion layer structure of laminate structure and the negatively charged ion interchangeability of flaggy positively charged ion collocation property and uniqueness, therefore, by metal ion and the negatively charged ion of modulation, realize unit assembling variation.For many years to the research of hydrotalcite, hydrotalcite is widely used in many fields such as absorption, ion-exchange, catalysis, medicine, oil-field development, coating.Hydrotalcite is because of its special construction, and to water pollutant, especially negatively charged ion has stronger adsorptivity.In recent years because hydrotalcite has huge development prospect, become the focus of research both at home and abroad.Synthetic hydrotalcite common at present has hydrothermal method, electrochemical process, ion exchange method etc., these method complex process, length consuming time, output is little, be not suitable for becoming to produce on a large scale, the present invention discloses a kind of preparation of the ammonium polyphosphate magnesium aluminum-hydrotalcite that adulterates, and method kind method economy uses, with low cost, technique is simple, high-level efficiency, high quality, is easy to industrial production.
Summary of the invention
In order to solve the technical problem existed in prior art, the invention provides a kind of preparation method of the ammonium polyphosphate magnesium aluminum-hydrotalcite that adulterates, this method economy uses, with low cost, and technique is simple, and high-level efficiency, high quality, is easy to industrial production.
In order to reach above-mentioned purpose, the concrete technical scheme of employing is:
1, take the magnesium sulfate of 25.5g, the aluminum nitrate of 37.5 fully grinds 30-60 minute in mortar;
2, in three mouthfuls of reaction flasks, add 100mL deionized water, placed by ground mixed powder and enter to dissolve, limit is stirred and is just added sodium hydroxide and Carbon Dioxide sodium solution, and pH remains on 9-12;
3, at room temperature magnetic force reduces by half 20 minutes, is adding 20g urea and 30mL deionized water, is warming up to 50 DEG C and stirs 1 hour;
4, after reacting completely, slurries are placed in Microwave Extraction Apparatus, 500W, at 150 DEG C, crystallization 5 minutes;
5, taken out by crystalline thing, drying and grinding into powder puts into reaction flask, adds 100mL deionized water, 20mLAPP, be heated to 120 DEG C, slowly stir, ageing 10 hours in pot after reaction terminates, be cooled to room temperature, put into oven for drying, obtain doping ammonium polyphosphate magnesium aluminum-hydrotalcite.
Application method of the present invention is:
1, take the magnesium sulfate of 25.5g, the aluminum nitrate of 37.5 fully grinds 30-60 minute in mortar;
2, in three mouthfuls of reaction flasks, add 100mL deionized water, placed by ground mixed powder and enter to dissolve, add sodium hydroxide and Carbon Dioxide sodium solution while stirring, pH remains on 9-12;
3, at room temperature magnetic force reduces by half 20 minutes, is adding 20g urea and 30mL deionized water, is warming up to 50 DEG C and stirs 1 hour;
4, after reacting completely, slurries are placed in Microwave Extraction Apparatus, 500W, at 150 DEG C, crystallization 5 minutes;
5, taken out by crystalline thing, drying and grinding into powder puts into reaction flask, adds 100mL deionized water, 20mLAPP, be heated to 120 DEG C, slowly stir, ageing 10 hours in pot after reaction terminates, be cooled to room temperature, put into oven for drying, obtain doping ammonium polyphosphate magnesium aluminum-hydrotalcite.
6, appeal doping ammonium polyphosphate magnesium aluminum-hydrotalcite 20g is put into the Congo red dyeing waste water containing 20mL/L, be heated to 45 DEG C 1 hour, concentration Congo red after testing becomes 0.33mL/L, and clearance is 99.9%.
Specific embodiments:
Take the magnesium sulfate of 25.5g, the aluminum nitrate of 37.5 fully grinds 30-60 minute in mortar, 100mL deionized water is added in three mouthfuls of reaction flasks, ground mixed powder is placed enter to dissolve, add sodium hydroxide and Carbon Dioxide sodium solution while stirring, pH remains on 9-12, at room temperature magnetic force reduces by half 20 minutes, adding 20g urea and 30mL deionized water, be warming up to 50 DEG C to stir 1 hour, after reacting completely, slurries are placed in Microwave Extraction Apparatus, 500W, at 150 DEG C, crystallization 5 minutes, crystalline thing is taken out, drying and grinding into powder puts into reaction flask, add 100mL deionized water, 20mLAPP, be heated to 120 DEG C, slow stirring, ageing 10 hours in pot after reaction terminates, be cooled to room temperature, put into oven for drying, obtain doping ammonium polyphosphate magnesium aluminum-hydrotalcite, appeal doping ammonium polyphosphate magnesium aluminum-hydrotalcite 20g is put into the Congo red dyeing waste water containing 20mL/L, be heated to 45 DEG C 1 hour, concentration Congo red after testing becomes 0.33mL/L, clearance is 99.9%.
Example 1
Take the magnesium sulfate of 25.5g, the aluminum nitrate of 37.5 fully grinds 30 minutes in mortar, 100mL deionized water is added in three mouthfuls of reaction flasks, ground mixed powder is placed enter to dissolve, add sodium hydroxide and Carbon Dioxide sodium solution while stirring, pH remains on 9, at room temperature magnetic force reduces by half 20 minutes, adding 20g urea and 30mL deionized water, be warming up to 50 DEG C to stir 1 hour, after reacting completely, slurries are placed in Microwave Extraction Apparatus, 500W, at 150 DEG C, crystallization 5 minutes, crystalline thing is taken out, drying and grinding into powder puts into reaction flask, add 100mL deionized water, 20mLAPP, be heated to 120 DEG C, slow stirring, ageing 10 hours in pot after reaction terminates, be cooled to room temperature, put into oven for drying, obtain doping ammonium polyphosphate magnesium aluminum-hydrotalcite, appeal doping ammonium polyphosphate magnesium aluminum-hydrotalcite 20g is put into the Congo red dyeing waste water containing 20mL/L, be heated to 45 DEG C 1 hour, concentration Congo red after testing becomes 0.39mL/L, clearance is 99.9%.
Example 2
Take the magnesium sulfate of 25.5g, the aluminum nitrate of 37.5 fully grinds 50 minutes in mortar, 100mL deionized water is added in three mouthfuls of reaction flasks, ground mixed powder is placed enter to dissolve, add sodium hydroxide and Carbon Dioxide sodium solution while stirring, pH remains on 11, at room temperature magnetic force reduces by half 20 minutes, adding 20g urea and 30mL deionized water, be warming up to 50 DEG C to stir 1 hour, after reacting completely, slurries are placed in Microwave Extraction Apparatus, 500W, at 150 DEG C, crystallization 5 minutes, crystalline thing is taken out, drying and grinding into powder puts into reaction flask, add 100mL deionized water, 20mLAPP, be heated to 120 DEG C, slow stirring, ageing 10 hours in pot after reaction terminates, be cooled to room temperature, put into oven for drying, obtain doping ammonium polyphosphate magnesium aluminum-hydrotalcite, appeal doping ammonium polyphosphate magnesium aluminum-hydrotalcite 20g is put into the Congo red dyeing waste water containing 20mL/L, be heated to 45 DEG C 1 hour, concentration Congo red after testing becomes 0.37mL/L, clearance is 99.9%.
Example 3
Take the magnesium sulfate of 25.5g, the aluminum nitrate of 37.5 fully grinds 60 minutes in mortar, 100mL deionized water is added in three mouthfuls of reaction flasks, ground mixed powder is placed enter to dissolve, add sodium hydroxide and Carbon Dioxide sodium solution while stirring, pH remains on 12, at room temperature magnetic force reduces by half 20 minutes, adding 20g urea and 30mL deionized water, be warming up to 50 DEG C to stir 1 hour, after reacting completely, slurries are placed in Microwave Extraction Apparatus, 500W, at 150 DEG C, crystallization 5 minutes, crystalline thing is taken out, drying and grinding into powder puts into reaction flask, add 100mL deionized water, 20mLAPP, be heated to 120 DEG C, slow stirring, ageing 10 hours in pot after reaction terminates, be cooled to room temperature, put into oven for drying, obtain doping ammonium polyphosphate magnesium aluminum-hydrotalcite, appeal doping ammonium polyphosphate magnesium aluminum-hydrotalcite 20g is put into the Congo red dyeing waste water containing 20mL/L, be heated to 45 DEG C 1 hour, concentration Congo red after testing becomes 0.33mL/L, clearance is 99.9%.
Claims (1)
1. adulterate the preparation method of ammonium polyphosphate magnesium aluminum-hydrotalcite, it is characterized in that:
(1) take the magnesium sulfate of 25.5g, the aluminum nitrate of 37.5g fully grinds 30-60 minute in mortar;
(2) in three mouthfuls of reaction flasks, add 100mL deionized water, placed by ground mixed powder and enter to dissolve, limit is stirred and is just added sodium hydroxide and Carbon Dioxide sodium solution, and pH remains on 9-12;
(3) at room temperature magnetic force reduces by half 20 minutes, is adding 20g urea and 30mL deionized water, is warming up to 50 DEG C and stirs 1 hour;
(4) after reacting completely, slurries are placed in Microwave Extraction Apparatus, 500W, at 150 DEG C, crystallization 5 minutes;
(5) taken out by crystalline thing, drying and grinding into powder puts into reaction flask, adds 100mL deionized water, 20mLAPP, be heated to 120 DEG C, slowly stir, ageing 10 hours in pot after reaction terminates, be cooled to room temperature, put into oven for drying, obtain doping ammonium polyphosphate magnesium aluminum-hydrotalcite.
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| CN201410729207.2A CN104591238A (en) | 2014-12-04 | 2014-12-04 | Preparation method for ammonium-polyphosphate-doped magnesium aluminium hydrotalcite |
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| CN201410729207.2A CN104591238A (en) | 2014-12-04 | 2014-12-04 | Preparation method for ammonium-polyphosphate-doped magnesium aluminium hydrotalcite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453750A (en) * | 2020-05-29 | 2020-07-28 | 山东长泽新材料科技有限公司 | Clean synthesis process of magnesium aluminum hydrotalcite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003063818A (en) * | 2001-06-12 | 2003-03-05 | Tosoh Corp | Method for producing crystals of hydrotalcite compounds |
| CN101381094A (en) * | 2007-09-03 | 2009-03-11 | 襄樊市油建化工有限公司 | Method for preparing nano magnalium hydrotalcite and equipment thereof |
| CN101386424A (en) * | 2008-10-14 | 2009-03-18 | 中国海洋大学 | method for preparing modification forming magnalium hydrotalcite and application |
-
2014
- 2014-12-04 CN CN201410729207.2A patent/CN104591238A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003063818A (en) * | 2001-06-12 | 2003-03-05 | Tosoh Corp | Method for producing crystals of hydrotalcite compounds |
| CN101381094A (en) * | 2007-09-03 | 2009-03-11 | 襄樊市油建化工有限公司 | Method for preparing nano magnalium hydrotalcite and equipment thereof |
| CN101386424A (en) * | 2008-10-14 | 2009-03-18 | 中国海洋大学 | method for preparing modification forming magnalium hydrotalcite and application |
Non-Patent Citations (1)
| Title |
|---|
| 杨保俊等: "类水滑石的制备与改性及其在聚丙烯阻燃中的应用", 《复合材料学报》, vol. 31, no. 2, 25 November 2013 (2013-11-25) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453750A (en) * | 2020-05-29 | 2020-07-28 | 山东长泽新材料科技有限公司 | Clean synthesis process of magnesium aluminum hydrotalcite |
| CN111453750B (en) * | 2020-05-29 | 2021-09-03 | 山东长泽新材料科技有限公司 | Clean synthesis process of magnesium aluminum hydrotalcite |
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Application publication date: 20150506 |