CN104961150A - Method for preparing multielement nano hydrotalcite by adopting magnesite - Google Patents
Method for preparing multielement nano hydrotalcite by adopting magnesite Download PDFInfo
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- CN104961150A CN104961150A CN201510376531.5A CN201510376531A CN104961150A CN 104961150 A CN104961150 A CN 104961150A CN 201510376531 A CN201510376531 A CN 201510376531A CN 104961150 A CN104961150 A CN 104961150A
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Abstract
The invention belongs to the field of preparation methods of nano hydrotalcite and particularly relates to a method for preparing multielement nano hydrotalcite by adopting magnesite. The method is performed in the following steps: (1) roasting natural magnesite to prepare MgO; (2) reacting MgO with HNO3 to prepare Mg(NO3)2; (3) adding nitrate of divalent or trivalent metal ions and urea into an Mg(NO3)2 solution to prepare a solution I; (4) stirring to obtain a solution II under the oil bath state of the solution; (5) placing the solution II into a vacuum drying box, and standing and crystallizing; (6) filtering the obtained solution and washing till a washing solution is clear to obtain a solid product III; (7) drying the solid product III; (8) grinding the dried solid product III to obtain the target product. The method is low in cost, capable of fully using magnesite dust and easy for realizing industrialized production.
Description
Technical field
The invention belongs to polynary nanometer hydrotalcite preparation method field, particularly relate to a kind of method adopting magnesite to prepare polynary nanometer hydrotalcite.
Background technology
Magnesite is one of the superior resources in Liaoning Province, and Liaoning magnesite reserves account for 1/4 of the world, but magnesite industry is in the situation of " first-class raw material, second-class processing, third-class product, fourth class price ".Therefore, must pay attention to the Study and Development of magnesium chemical products, expand the application of magnesian in fields such as agricultural, building materials, accelerate magnesian industry technology innovation paces, exploitation has novel material, the product innovation of independent intellectual property right.
Hydrotalcite-based compound (being abbreviated as LDHs) is the negatively charged ion lamellar compound that a class has broad prospect of application, in laminate, positively charged ion and interlayer anion have interchangeability, there is special memory function, there is certain weakly alkaline, be the stratified material that a class has actual application value, receive the extensive concern of industry and academic research.The Derived Mixed Oxides obtained for raw material with hydrotalcite-like material obtains growing concern as solid acid alkali catalytic agent, redox catalyst and support of the catalyst.Hydrotalcite-based compound is utilized as high-efficiency anion absorption agent and catalytic carrier in water pollution is administered simultaneously, and shows applications well prospect.Particularly in the research of nano composite material, hydrotalcite is widely used as a kind of common nano lamellar material.In existing research, magnisite breeze is adopted only to synthesize binary magnalium nano hydrotalcite.
Summary of the invention
The object of the present invention is to provide a kind of method adopting magnesite to prepare polynary nanometer hydrotalcite, the method operational path is simple, with low cost, can make full use of magnesite dust, be easy to realize suitability for industrialized production.
For solving the problems of the technologies described above, the present invention realizes like this.
Adopt magnesite to prepare a method for polynary nanometer hydrotalcite, can carry out successively as follows:
(1) the magnisite obtained magnesium oxide after roasting sieved will be ground;
(2) gained magnesium oxide and nitric acid reaction are obtained magnesium nitrate;
(3) in made magnesium nitrate solution, add nitrate and the urea obtained solution I of divalence or trivalent metal ion again;
(4) by solution I oil bath 102 ~ 110 DEG C, temperature under 90 ~ 100 DEG C of conditions, Keep agitation 10 ~ 12 hours, control rotating speed at 200 ~ 400r/min, obtain solution II;
(5) solution II is put into vacuum drying oven, temperature controls at 90 ~ 95 DEG C, static crystallization 16 ~ 20h;
(6) step (5) gained solution is carried out suction filtration, and with deionized water, the solid product after suction filtration is repeatedly washed, to washings clarification, obtain solid product III;
(7) inserted in vacuum drying oven by solid product III and carry out drying, temperature controls at 90 ~ 95 DEG C, time 15 ~ 20h;
(8) namely dried solid product III obtains object product polynary nanometer hydrotalcite after grinding.
As a kind of preferred version, M of the present invention (II) is Mg, Zn or Ni ion etc.; Described M (III) is Al, Fe or Co ion etc.
Further, step of the present invention (1) described magnisite is the magnesite ore of natural output; Wherein: MgCO
3>=96%, foreign matter content≤4%.
Further, in step of the present invention (3), the mol ratio n (urea: nitrate radical)=1 ~ 4 of urea and nitrate radical; The mol ratio n [M (II): M (III)]=1 ~ 4 of M (II) and M (III) in solution; Wherein: M (II) is divalent-metal ion; M (III) is trivalent metal ion.
Further, in step of the present invention (2), the concentration of salpeter solution is 3 ~ 9mol/L.
The present invention makes full use of the feature of the rich magnesium of magnisite, and its preparation method is simple, and cost is low, by rational technological design and optimizing materials proportioning, effectively can utilize the dust of magnesite, successful in resource deep processing and comprehensive utilization, be easy to realize suitability for industrialized production simultaneously.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments the invention will be further described book.Protection scope of the present invention is not only confined to the statement of following content.
When Fig. 1 is n of the present invention (urea/nitrate radical)=3, the hydrotalcite XRD spectra of n (Zn:Mg:Al)=1:1:1 and n (Mg:Al)=2:1.
Fig. 2-1 and Fig. 2-2 is the SEM figure of ternary Zn-Mg-Al hydrotalcite of the present invention.
When Fig. 3 is n of the present invention (urea/nitrate radical)=3, the hydrotalcite XRD spectra of n (Zn:Mg:Al:Fe)=2:2:1:1.
Fig. 4-1 and Fig. 4-2 is the SEM figure of quaternary Zn-Mg-Al-Fe hydrotalcite of the present invention.
Embodiment
Embodiment 1.
In the present embodiment by the concrete steps that magnisite prepares Zn-Mg-Al hydrotalcite be:
(1) by magnisite ore reduction, levigate at main the magnesium oxide of retort furnace calcining;
(2) 0.15mol is about getting the magnesite 6.25g(after calcining containing Mg) react to obtain magnesium nitrate with 6mol/L nitric acid 50ml, and suction filtration obtains filtrate (magnesium nitrate);
(3) made magnesium nitrate and zinc nitrate, aluminum nitrate and urea are pressed following mol ratio: n [(Mg+Zn)/Al]=2; N (urea/nitrate radical)=3, n (Mg/Zn)=1, adds 44.62gZn (NO
3)
26H
2o, 56.2695g Al (NO
3)
39H
2o, urea 189g and deionized water 200ml are mixed to get solution I;
(4) move in encloses container I by solution I, oil bath about 105 DEG C, the hierarchy of control is between 90-100 DEG C, and Keep agitation 11 hours, controls rotating speed at 300r/min, obtain solution II;
(5) solution II is proceeded in container II, puts into vacuum drying oven, control temperature at 95 DEG C, static crystallization 18h;
(6) solution II is carried out suction filtration, and with deionized water, solid product after suction filtration is repeatedly washed, to washings clarification, obtain solid product III;
(7) vacuum drying oven is placed on to solid product III and carries out drying: control temperature 90 DEG C, time 18h;
(8) dried solid product III grinds to obtain Zn-Mg-Al hydrotalcite powder.
See Fig. 1, obviously can see that diffraction peak that ternary Zn-Mg-Al-LDH hydrotalcite is the highest is than the diffraction peak height of binary Mg-Al hydrotalcite, illustrates that the ternary Zn-Mg-Al hydrotalcite that this method is synthesized is better than the crystallization degree of binary Mg-Al hydrotalcite.
As can be seen from Figure 2 the particle diameter of ternary Zn-Mg-Al hydrotalcite is very little, greatly about about 20nm, be lamellar structure, and its entirety is as petal.
Embodiment 2.
In the present embodiment by the concrete steps that magnisite prepares Zn-Mg-Al-Fe hydrotalcite be:
(1) by magnisite ore reduction, levigate at main the magnesium oxide of retort furnace calcining;
(2) 0.15mol is about getting the magnesite 6.25g(after calcining containing Mg) react to obtain magnesium nitrate with 6mol/L nitric acid 50ml, and suction filtration obtains filtrate (magnesium nitrate);
(3) made magnesium nitrate and zinc nitrate, aluminum nitrate, iron nitrate and urea are pressed following mol ratio: n [(Mg+Zn)/(Al+Fe)]=2; N (urea/nitrate radical)=3; N (Mg/Zn)=1; N (Al/Fe)=1 adds 44.6235gZn (NO
3)
26H
2o, 28.1250g Al (NO
3)
39H
2o, 30.3015gFe (NO
3)
39H
2o, urea 189g and deionized water 200ml are mixed to get solution I;
(4) move in encloses container I by solution I, oil bath about 105 DEG C, the hierarchy of control is between 90-100 DEG C, and Keep agitation 11 hours, controls rotating speed at 300r/min, obtain solution II;
(5) solution II is proceeded in container II, puts into vacuum drying oven, control temperature at 95 DEG C, static crystallization 18h;
(6) solution II is carried out suction filtration, and with deionized water, solid product after suction filtration is repeatedly washed, to washings clarification, obtain solid product III;
(7) vacuum drying oven is placed on to solid product III and carries out drying: control temperature 90 DEG C, time 18h;
(8) dried solid product III grinds to obtain Zn-Mg-Al-Fe hydrotalcite powder.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. adopt magnesite to prepare a method for polynary nanometer hydrotalcite, it is characterized in that: carry out successively as follows:
(1) the magnisite obtained magnesium oxide after roasting sieved will be ground;
(2) gained magnesium oxide and nitric acid reaction are obtained magnesium nitrate;
(3) in made magnesium nitrate solution, add nitrate and the urea obtained solution I of divalence or trivalent metal ion again;
(4) by solution I oil bath 102 ~ 110 DEG C, temperature under 90 ~ 100 DEG C of conditions, Keep agitation 10 ~ 12 hours, control rotating speed at 200 ~ 400r/min, obtain solution II;
(5) solution II is put into vacuum drying oven, temperature controls at 90 ~ 95 DEG C, static crystallization 16 ~ 20h;
(6) step (5) gained solution is carried out suction filtration, and with deionized water, the solid product after suction filtration is repeatedly washed, to washings clarification, obtain solid product III;
(7) inserted in vacuum drying oven by solid product III and carry out drying, temperature controls at 90 ~ 95 DEG C, time 15 ~ 20h;
(8) namely dried solid product III obtains object product polynary nanometer hydrotalcite after grinding.
2. employing magnesite according to claim 1 prepares the method for polynary nanometer hydrotalcite, it is characterized in that: described divalent-metal ion is Mg, Zn or Ni ion; Described trivalent metal ion is Al, Fe or Co ion.
3. employing magnesite according to claim 2 prepares the method for polynary nanometer hydrotalcite, it is characterized in that: step (1) described magnisite is the magnesite ore of natural output; Wherein: MgCO
3>=96%, foreign matter content≤4%.
4. employing magnesite according to claim 3 prepares the method for polynary nanometer hydrotalcite, it is characterized in that: in described step (3), the mol ratio n (urea: nitrate radical)=1 ~ 4 of urea and nitrate radical; The mol ratio n [M (II): M (III)]=1 ~ 4 of M (II) and M (III) in solution; Wherein: M (II) is divalent-metal ion; M (III) is trivalent metal ion.
5. employing magnesite according to claim 4 prepares the method for polynary nanometer hydrotalcite, it is characterized in that: in described step (2), the concentration of salpeter solution is 3 ~ 9mol/L.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268572A (en) * | 2016-07-16 | 2017-01-04 | 沈阳理工大学 | A kind of method preparing layered hydroxide for raw material with solid waste |
| CN111217385A (en) * | 2020-02-23 | 2020-06-02 | 武汉工程大学 | Method for preparing calcium-magnesium-aluminum hydrotalcite by using phosphate tailings |
| CN113104871A (en) * | 2021-04-25 | 2021-07-13 | 北京化工大学 | Method for preparing magnesium-aluminum hydrotalcite from magnesite |
| CN113371741A (en) * | 2021-06-08 | 2021-09-10 | 盘锦迪宝催化剂技术有限公司 | Magnesium-aluminum hydrotalcite and preparation method thereof |
-
2015
- 2015-07-01 CN CN201510376531.5A patent/CN104961150A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 张悦等: "菱镁矿制备纳米镁铝水滑石的研究", 《应用化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268572A (en) * | 2016-07-16 | 2017-01-04 | 沈阳理工大学 | A kind of method preparing layered hydroxide for raw material with solid waste |
| CN111217385A (en) * | 2020-02-23 | 2020-06-02 | 武汉工程大学 | Method for preparing calcium-magnesium-aluminum hydrotalcite by using phosphate tailings |
| CN113104871A (en) * | 2021-04-25 | 2021-07-13 | 北京化工大学 | Method for preparing magnesium-aluminum hydrotalcite from magnesite |
| CN113104871B (en) * | 2021-04-25 | 2022-07-26 | 北京化工大学 | Method for preparing magnalium hydrotalcite from magnesite |
| CN113371741A (en) * | 2021-06-08 | 2021-09-10 | 盘锦迪宝催化剂技术有限公司 | Magnesium-aluminum hydrotalcite and preparation method thereof |
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