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A kind of method that utilizes magnesite to prepare magnesium aluminum hydrotalcite

A magnesite, nano-hydrotalcite technology, applied in the directions of hydrotalcite, chemical instruments and methods, nanotechnology for materials and surface science, etc., can solve the problem of large consumption of nitric acid and NaOH waste liquid, incomplete precipitation of magnesium sulfate, Consume large acid and ammonia water, etc., to increase the effective contact area, avoid high temperature and high pressure reaction, and achieve the effect of small particle size

Active Publication Date: 2022-07-26
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

Patent 201210449644.X uses magnesite as raw material, reacts light-burned magnesite with ammonium sulfate to obtain magnesium sulfate solution and ammonia gas, and then passes ammonia gas into magnesium sulfate solution to react to prepare micron-sized magnesium hydroxide, but due to ammonia The gas is a weak base, and the precipitation of magnesium sulfate is not complete, resulting in a low yield of magnesium hydroxide
Patent 201410413211.8 discloses a method of using magnesite to prepare magnesium oxide, dissolving magnesite with sulfuric acid, adding concentrated ammonia water to convert magnesium sulfate into magnesium hydroxide, and then adding CO 2 Gas and concentrated ammonia water are used to prepare magnesium carbonate, and magnesium carbonate is calcined to obtain magnesium oxide, but this method needs to consume a large amount of acid and ammonia water, and produces a large amount of waste liquid
Patent 201010275047.0 uses sulfuric acid to dissolve calcined magnesite powder to prepare magnesium sulfate solution. Magnesium sulfate and ammonium bicarbonate are pyrolyzed to prepare basic magnesium carbonate. However, this method can only produce micron-sized basic magnesium carbonate and consumes a large amount of sulfuric acid.
Patent 201110385334.1 discloses a method for preparing hydrotalcite using natural magnesite, aluminum nitrate, nitric acid and NaOH as raw materials. In this method, magnesite is dissolved with nitric acid to obtain magnesium nitrate, and the solution of magnesium nitrate and aluminum nitrate reacts with NaOH to generate magnesium Aluminum hydrotalcite, but this method needs to consume a large amount of nitric acid and NaOH and produce a large amount of waste liquid
[0005] The purification and transformation of low- and medium-grade magnesite is the basis and key to realize the high-value utilization of magnesium resources. Currently, the purification methods of low- and medium-grade magnesite mainly include carbonization, acid hydrolysis, and ammonium leaching, among which carbonization is the The most commonly used method in industry, and the prepared products are mainly basic magnesium carbonate, magnesium hydroxide and magnesium oxide. There are few reports on the preparation of other magnesium-based functional materials using low-grade magnesite as raw materials

Method used

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  • A kind of method that utilizes magnesite to prepare magnesium aluminum hydrotalcite
  • A kind of method that utilizes magnesite to prepare magnesium aluminum hydrotalcite
  • A kind of method that utilizes magnesite to prepare magnesium aluminum hydrotalcite

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Effect test

Embodiment 1

[0029] Step A: Place 1 kg of magnesite powder (calcium-magnesium molar ratio is 8%) in a muffle furnace, heat to 700° C. for calcination for 2 hours to obtain light-burned magnesite powder; 89 grams of light-burned magnesite Powder (containing 8.96 grams of CaO), 32.6 grams of magnesium chloride hexahydrate and 1 kilogram of deionized water were mixed, and ground with a colloid mill for 10 minutes to obtain a slurry; the slurry was heated to 70 ° C, stirred and reacted for 3 hours, filtered and washed to obtain Mg(OH) 2 Wet cake; Mg(OH) 2 The wet cake was added to 800 g of deionized water and ground with a colloid mill for 4 minutes to obtain Mg(OH) 2 slurry.

[0030] Step B: Combine 286 g (NH 4 ) 2 SO 4 added to Mg(OH) 2 In the slurry, heated to 100 °C, stirring to react to Mg(OH) 2 All dissolved, the solution was filtered to obtain MgSO 4 solution, the resulting ammonia vapor is condensed by a condensing device and combined with CO 2 The gas reacts to give (NH 4 ) ...

Embodiment 2

[0034] Steps A, B and C are the same as in Example 1.

[0035] Step D: the nano-AlOOH wet filter cake (dry weight 30 grams), the hydrated MgCO obtained in step D 3 The wet filter cake and 30 g of acetic acid were added to 1.2 kg of deionized water and ground with a colloid mill for 5 minutes. The slurry was heated to 100°C and reacted under vigorous stirring for 0.5 and 1 hour, respectively. The reaction slurry was ground with a colloid mill for 6 minutes, and the reaction was continued. After 3 hours, 8 grams of lauric acid were added to modify the hydrotalcite, and after stirring for 2 hours, the precipitate was filtered and dried to obtain a lauric acid-modified nano-magnesium-aluminum hydrotalcite [Mg 0.8 Al 0.2 (OH) 2 ](CH 3 COO) 0.2 ·0.6H 2 O.

Embodiment 3

[0037] Steps A, B and C are the same as in Example 1.

[0038] Step D: the nano-AlOOH wet filter cake (dry weight 40 grams), the hydrated MgCO obtained in step C 3 Wet cake and 78.7 g of succinic acid (C 4 H 6 O 4 ) was added to 1.5 kg of deionized water and ground with a colloid mill for 8 minutes, heated to 105°C, and the reaction slurry was ground with a colloid mill for 8 minutes after reacting under vigorous stirring for 0.5 hours, and 10 grams of dodecylbenzene was added after continuing the reaction for 2.5 hours. The hydrotalcite was modified by sulfonic acid, and after stirring for 1 hour, the precipitate was filtered and dried to obtain nano-magnesium-aluminum hydrotalcite modified by dodecylbenzenesulfonic acid [Mg 0.75 Al 0.25 (OH) 2 ](C 4 H 4 O 4 ) 0.125 ·0.75H 2 O.

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Abstract

The invention provides a method for preparing nano-magnesium-aluminum hydrotalcite by utilizing magnesite. The method uses magnesite as raw material, reacts with magnesium salt and ammonium sulfate after roasting to realize separation of magnesium and impurities, and uses the generated magnesium sulfate and ammonium sulfate to separate magnesium and impurities. Ammonium carbonate or ammonium bicarbonate is used as raw material to prepare hydrated magnesium carbonate with uniform size, and then hydrated magnesium carbonate, pseudo-boehmite and functional guest are used as raw materials to prepare magnesium-aluminum hydrotalcite with relatively uniform size. The invention uses the high shear force of the colloid mill to force the micro-mixing of the hydrated magnesium carbonate, the pseudo-boehmite and the functional guest, thereby avoiding the problem of incomplete reaction caused by particle agglomeration. Since the raw material is a wet filter cake, no hard agglomeration occurs, the particle size is small, the specific surface area is large, and the reaction activity is high, and the nano-hydrotalcite can be rapidly reacted by heating under normal pressure, avoiding the high temperature and high pressure reaction. The method adopted in the invention has the advantages of abundant raw material sources, low price, simple preparation process, mild reaction conditions, green environmental protection, easy industrial production and the like.

Description

[0001] Field of study [0002] The invention relates to the field of preparation of inorganic non-metallic functional materials, in particular to a method for preparing nano-magnesium-aluminum hydrotalcite by using magnesite. Background technique [0003] Magnesite is a magnesium carbonate salt with the chemical formula MgCO 3 , my country is rich in magnesite mineral resources, mainly distributed in the Liaoning area, and the proven magnesite resource reserves that can be exploited exceed 3 billion tons. Magnesite is an important magnesium resource and is widely used in metallurgy, magnesium, refractory materials, building materials, chemical industry, agriculture, environmental protection and other fields. Magnesite is mainly used to produce primary products, and the added value of products is low. How to increase the added value of magnesite resources, carry out deep processing of magnesite, and produce high-end products with high added value is an urgent problem to be sol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/785B82Y40/00B82Y30/00
CPCB82Y40/00B82Y30/00C01P2002/22C01P2002/72C01P2004/03C01F7/785C01F7/78
Inventor 唐平贵李殿卿冯拥军
Owner BEIJING UNIV OF CHEM TECH
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