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Preparation method for low-sodium low-iron composite pseudo-boehmite and co-production of ammonium chloride

A technology of pseudo-boehmite and ammonium chloride, applied in the fields of alumina/hydroxide preparation, ammonium chloride, chemical instruments and methods, etc., can solve the problem of increased cost of reverse osmosis membrane, complex process steps, and sodium oxide content High-level problems, to achieve the effect of good iron removal effect, simple process and simple operation steps

Active Publication Date: 2022-05-31
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The kneading method is difficult to control the components, and the mechanical strength is poor
The precipitation method uses alkaline sodium metaaluminate as the aluminum source and the acidic titanium source to undergo a neutralization reaction to form a precipitate to prepare a composite carrier. The raw material cost of this method is low, but due to the introduction of a large amount of Alkali also has the problems of difficult washing and high sodium oxide content in the product. In the prior art, the soluble aluminum salt and soluble titanium salt solution are processed by a strong alkali aqueous solution to form a precipitate and the reverse osmosis membrane is used to remove the basic cations introduced by the strong alkali to obtain Pseudoboehmite-titania composite support with low basic cation content, but the use of reverse osmosis membrane increases the cost
It is also possible to mix alumina, metatitanic acid and a solvent, and then perform high-energy ball milling on the mixture and dry it. The dried product is mixed with acid solution, shaped, dried and roasted to obtain a composite carrier of pseudo-boehmite and alumina. method, but the process steps are complicated, and the alumina material needs to be prepared in advance, which only tends to solve the problem of preparation of titanium oxide
[0006] At present, there is no method for preparing composite pseudo-boehmite by fly ash, especially circulating fluidized bed fly ash. Therefore, the problem to be solved by the present invention is how to use this solid waste of fly ash as raw material, through Simple process to prepare high-quality pseudo-boehmite products, and introduce titanium source in the preparation process, prepare composite pseudo-boehmite and co-produce ammonium chloride, so as to obtain low-cost and high-quality pseudo-boehmite- Titanium oxide composite carrier

Method used

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  • Preparation method for low-sodium low-iron composite pseudo-boehmite and co-production of ammonium chloride

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Embodiment 1

[0025] The present embodiment provides a preparation method of low-sodium and low-iron composite pseudoboehmite and co-production of ammonium chloride, comprising the following steps:

[0026] a) Leaching: the circulating fluidized bed fly ash adopts wet magnetic separation to remove iron: the fly ash and boron mud are pulverized to 200 mesh, and water is added to prepare a slurry with a solid content of 20wt% to 40wt%. Magnetic separation removes iron, so that the iron content in fly ash and boron mud is reduced to below 0.8wt%, and the filter cake is obtained by filtration. The ash filter cake was acid-dissolved with industrial hydrochloric acid with a concentration of 37wt%. The molar ratio of HCl in the hydrochloric acid to the alumina in the fly ash was 4.5:1; the reaction temperature was 200°C, the reaction time was 1 hour, and the reaction pressure was 2.1MPa , the reaction product is filtered and washed by a plate basket filter press to obtain an aluminum chloride leac...

Embodiment 2

[0033] The present embodiment provides a preparation method of low-sodium and low-iron composite pseudoboehmite and co-production of ammonium chloride, comprising the following steps:

[0034] a) with step a) of embodiment 1;

[0035] b) with step b) of embodiment 1, obtain refined aluminum chloride solution;

[0036] c) Compounding: Add TiCl to the refined aluminum chloride solution under vigorous stirring 4 and mixed evenly to obtain a mixed solution, TiCl 4 The amount added is TiO 2 0.5% by weight of the final pseudo-boehmite product;

[0037] d) Neutralization: control the temperature of the purified aluminum chloride solution to be 10 to 90° C., add 20% ammonium carbonate solution to the mixed solution under strong stirring to a pH of 6.0 to obtain colloidal precipitation; the added concentration is 1% polyvinyl alcohol solution, adding a volume of 5% of the chloride solution volume, aging at 45°C for 4 hours;

[0038] e) Drying: After aging, the composite pseudo-boe...

Embodiment 3

[0041] The present embodiment provides a preparation method of low-sodium and low-iron composite pseudoboehmite and co-production of ammonium chloride, comprising the following steps:

[0042] a) with step a) of embodiment 1;

[0043] b) with step b) of embodiment 1, obtain refined aluminum chloride solution;

[0044] c) Compounding: Add TiCl to the refined aluminum chloride solution under vigorous stirring 4 and mixed evenly to obtain a mixed solution, TiCl 4 The amount added is TiO 2 10% by weight of the final pseudo-boehmite product;

[0045] d) Neutralization: control the temperature of the refined aluminum chloride solution to be 10-90°C, add saturated ammonium bicarbonate solution to the mixed solution under strong stirring to a pH value of 5.4 to obtain colloidal precipitation; add 10% Polyethylene glycol solution, added in a volume of 2% of the chloride solution volume, aged at 30°C for 8 hours;

[0046] e) Drying: After aging, the composite pseudo-boehmite is obt...

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Abstract

The invention relates to a preparation method of low-sodium low-iron composite pseudo-boehmite and co-produced ammonium chloride, a composite pseudo-boehmite product is obtained by the steps of leaching, purifying and removing iron, adding TiCl4 for compounding, neutralizing, drying, crystallizing and the like, and an ammonium chloride product is co-produced. The specific surface area of the composite pseudo-boehmite is higher than 350 m < 2 > / g, the pore volume is larger than 1.2 ml / g, the content of Fe2O3 is not higher than 0.01 wt%, the content of Na2O is not higher than 0.02 wt%, and the content of iron and the content of sodium in the product are both low and are far lower than the standard that the content of Fe2O3 is 0.03-0.05 wt% and the content of Na2O is 0.1-0.3 wt% of the composite pseudo-boehmite in the current market. Compared with the prior art, the raw material cost is low, and the technological process is simple; the washing process is simplified, and the washing water amount is small; a titanium source is introduced in a pseudo-boehmite forming process by utilizing an acidic system, and titanium oxide compounded pseudo-boehmite is directly obtained and is suitable for being used as a hydrogenation catalyst carrier.

Description

technical field [0001] The invention relates to a method for preparing pseudo-boehmite, in particular to a preparation method for low-sodium and low-iron composite pseudo-boehmite and co-production of ammonium chloride. Background technique [0002] Pseudoboehmite (γ-AlOOH·nH 2 O, n=0.08~0.62) is also called colloidal boehmite or pseudoboehmite. Its crystal phase structure is similar to that of boehmite, but the crystallization is incomplete. Pseudo-boehmite has the characteristics of large pore volume, high specific surface area and good peptization performance, and can be widely used in petrochemical industry as catalyst carrier, catalyst, ceramic base material, etc. [0003] At present, the production methods of pseudo-boehmite can be roughly divided into two categories, namely the organic aluminum alkoxide method and the acid-base neutralization method. The organic aluminum alkoxide method uses metal aluminum, hydrogen and ethylene as raw materials, first synthesizes t...

Claims

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Application Information

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IPC IPC(8): C01F7/02C01F7/22C01F7/30C01C1/16C01G23/053B01J21/06B01J32/00
CPCC01F7/02C01F7/22C01F7/30C01C1/164C01G23/053C01G23/0536B01J21/063C01P2006/12C01P2006/14C01P2004/82C01P2006/80Y02P20/52
Inventor 魏存弟许优张培萍徐少南程妍
Owner JILIN UNIV