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Comprehensive utilization method of hydrargillite-produced 4A zeolite waste residue

A technology of gibbsite and zeolite, which is applied in the direction of crystalline aluminosilicate zeolite, A-type crystalline aluminosilicate zeolite, chemical instruments and methods, etc., can solve the problems of comprehensive utilization that have not been seen, and achieve low equipment requirements and high reaction efficiency. The effect of mild conditions and sufficient sources

Inactive Publication Date: 2011-08-31
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no research on the comprehensive utilization of gibbsite-made 4A zeolite waste residue

Method used

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  • Comprehensive utilization method of hydrargillite-produced 4A zeolite waste residue
  • Comprehensive utilization method of hydrargillite-produced 4A zeolite waste residue
  • Comprehensive utilization method of hydrargillite-produced 4A zeolite waste residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) acid leaching reaction

[0033] In the there-necked flask, add the gibbsite waste slag that is ground to 80 objects (the mass percentage of its main chemical composition is: Fe 2 o 3 14.30%, SiO 2 24.94%; Al 2 o 330 g of 38.25%) and 90 mL of 36% hydrochloric acid at a temperature of 90° C., fully stirred and reacted for 4 h, filtered to obtain 89.9 ml of filtrate, and then washed the filter residue with 70.1 ml of deionized water to obtain 70.1 ml of washing liquid. The wet filter residue was dried to remove water to obtain 7.40 g on a dry basis.

[0034] (2) Synthesis of polyaluminum ferric chloride from the filtrate

[0035] Put 160 mL of the mixed solution of acid leaching filtrate and lotion obtained in step (1) into a three-necked flask, stir and raise the temperature to 65°C, add 48 mL of 4 mol / L sodium hydroxide solution, adjust the pH to 2.0, and react for 4 hours; After filtering, the filtrate was evaporated to dryness to obtain a solid product, polya...

Embodiment 2

[0049] Embodiment 2: (recycling of embodiment 1 synthesis 4A mother liquor)

[0050] (1) acid leaching reaction

[0051] Same as Example 1(1)

[0052] (2) Polymerization reaction to produce polyaluminum ferric chloride

[0053] Same as Example 1(2)

[0054] (3) Wet slag plus alkali roasting activates iron removal

[0055] Same as Example 1(3)

[0056] (4) Hydrothermal synthesis of 4A zeolite

[0057] The mother liquor after synthesizing 4A zeolite decomplexation is 194mL altogether, wherein alkali content is 6.745g by NaOH, Si is by SiO 2 Calculated as 1.025g (equivalent to 2.084g of sodium silicate), Al is expressed as Al 2 o 3 Calculated as 0.5126g (equivalent to 0.8242g of sodium aluminate). This mother liquor needs to add 6mL deionized water, 14.42g alkali fusion roasting activator that crosses 80 mesh sieves, 1.255g sodium hydroxide and 9.176g sodium aluminate, can make reaction solution synthesize 4A with (4) in embodiment 1 The system is the same. First add 6m...

Embodiment 3

[0064] (1) acid leaching reaction

[0065] Same as Example 1(1)

[0066] (2) Polymerization reaction to produce polyaluminum ferric chloride

[0067] Same as Example 1(2)

[0068] (3) Wet slag plus alkali roasting activates iron removal

[0069] Take 7.40 g of the wet slag obtained in step (1) and dry it to remove water, pass through 80 meshes, add 14.38 g of sodium carbonate and 0.22 g of sodium chloride, mix well, and burn at 800 ° C for 2 hours to obtain alkali fusion 17.5g of the activated substance was calcined.

[0070] (4) Hydrothermal synthesis of 4A zeolite

[0071] First, dissolve 10g of sodium aluminate and 7g of sodium hydroxide in 100mL of deionized water, mix the two solutions after they are completely dissolved, then take the mixed solution and place it in a three-necked flask with a constant temperature water bath at 40°C, and quickly add 17.5 g passed through an 80-mesh sieve and 7.8 mL of triethanolamine and alkali fusion roasting activated product, stir...

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Abstract

The invention provides a comprehensive utilization method of hydrargillite-produced 4A zeolite waste residue. The method comprises the steps of: separating the ferrosilicoaluminum component in the hydrargillite-produced 4A zeolite waste residue by means of acid leaching and filtering, wherein the obtained mixed liquor of filter liquor and filter residue washing liquor is used for preparing a polymeric aluminum ferric chloride water purifying agent; and removing iron from the wet slag obtained by washing the filter residue by means of alkali fusing, roasting and activating, and synthesizing the 4A zeolite by a hydrothermal method by means of adjusting and assembling. Triethanolamine is taken as a complexing agent of the microelement iron in the liquor during synthesizing the 4A zeolite, so that the produce of an iron precipitate is overcome, and the whiteness of a 4A zeolite product is guaranteed; sodium sulfide is reacted with a triethanolamine iron complex in the zeolite-synthesized mother liquor to reduce the triethanolamine and obtain an iron sulfide precipitate; and removing the mother liquor of the iron sulfide precipitate to realize the cycle utilization. The synthesis method of the 4A zeolite adopts a sealed cycle technology, thereby being stable in operation, and free of the generation of new waste liquor and new waste slag.

Description

technical field [0001] The invention relates to using gibbsite to prepare 4A zeolite waste residue as raw material, using hydrochloric acid acid leaching to separate aluminum iron from silicon, and the filtrate is used to produce composite coagulant polyaluminum ferric chloride, the water purifier is mainly used for domestic water and non-domestic water purification treatment; the filter residue is used to produce 4A zeolite for detergent builders. Background technique [0002] Gibbsite is a hydroxide mineral of aluminum, often accompanied by common minerals such as hematite, aluminum hematite, goethite, aluminum goethite, quartz, and kaolin. The main chemical composition of gibbsite is Al 2 o 3 , Fe 2 o 3 , SiO 2 、H 2 O, whose mass content is Al 2 o 3 22.12%~30.30%, Fe 2 o 3 9.43%~45.84%, SiO 2 7.44%~14.04%, H 2 O3.79%~16.50%; In addition, there is a small amount of TiO 2 , MnO 2 、K 2 O, Na 2 O, CaO, MgO and other components. Gibbsite has a wide range of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/14C02F1/52C11D3/12C11D9/18
Inventor 曹吉林赵园张广林刘恩海李琳刘秀伍
Owner HEBEI UNIV OF TECH
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