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X zeolite preparation

A zeolite and nanotechnology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., to achieve the effect of reducing waste residue and mother liquor and improving the environment

Inactive Publication Date: 2004-10-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as the present inventors know, there has been no report on using silicon-aluminum wet residue and / or mother liquor from catalyst plants with complex composition and composition as a raw material for preparing low-silicon-aluminum ratio X zeolite without any pretreatment

Method used

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preparation example Construction

[0013] The preparation method of the low silicon-aluminum ratio X zeolite provided by the present invention comprises:

[0014] (1) According to the chemical composition of the waste residue and / or mother liquor, add sodium hydroxide and potassium hydroxide mixed alkali and water glass and / or aluminum source into the catalyst plant waste residue and / or mother liquor according to the required feeding ratio, and mix well , so that the total molar composition of the resulting reaction mixture conforms to (4.0-6.0)Na 2 O:(1.0~2.5)K 2 O:Al 2 o 3 :(1.0~3.0)SiO 2 :(50~250)H 2 The ratio of O; among them, Al in waste residue and mother liquor 2 o 3 Accounting for the total Al of mixed material 2 o 3 0-50% by weight of the amount; SiO in waste residue and mother liquor 2 % of total SiO in mixed materials 2 15-100% by weight of the total alkali amount; the alkali in the waste residue and the mother liquor accounts for 0-45% of the total alkali amount;

[0015] (2) aging the mi...

Embodiment 1

[0027] In the 880g waste residue (taken from the comprehensive workshop of Changling Catalyst Factory, Na 2 O=1.83%, SiO 2 =76%, Al 2 o 3 = 32.4%, RE 2 o 3 = 28%, SO 4 ＝ = 1.14%, Fe = 0.046%, Cl - =0.3%, solid content=15.7%), add 310 milliliters of mother liquor (Na 2 O=47 g / L, SiO 2 =99 grams per liter), 710ml liquid caustic soda (NaOH, taken from Changling Catalyst Factory, Na 2 O=298 grams per liter), and 224 grams of KOH (chemically pure reagent, purity 82%, Beijing chemical plant), stir, after the solid alkali dissolves substantially, add 580 milliliters of low alkalinity sodium metaaluminate solutions (Na 2 O=147 g / L, Al 2 o 3 =90 g / L), stirred evenly, put into a stainless steel reactor and aged at 40°C for two days, crystallized at 70°C for 16 hours, filtered, washed, and dried. The unit cell constant of the resulting product is 2.501 nanometers, and the chemical composition of the product is Na 2 O=13%, K 2 O=12%, SiO 2 =41%, Al 2 o 3 = 33%, RE 2 o 3...

Embodiment 2

[0032] In 860g waste residue (same as above, Na 2 O=6.7%, SiO 2 =66.9%, Al 2 o 3 = 18.6%, RE 2 o 3 =0.47%, Fe 2 o 3 = 0.25%, SO 4 ＝ =5.2%, Cl - =0.30%, solid content 18.3%), add 300 milliliters of mother liquors (same as above, Na 2 O=40 g / L, SiO 2 =87 grams per liter), 650ml liquid caustic soda (same as above, Na 2 (O=297 g / liter), 220 gram KOH (same as above), 10 grams of X zeolite product gained in Example 1, stir, and add 730 milliliters of low alkalinity sodium metaaluminate (same as above, Na 2 O=152 g / L, Al 2 o 3 = 100 g / L), stirred evenly, put into a stainless steel reactor and aged at 30°C for three days, crystallized at 60°C for 24 hours, filtered, washed, and dried. The resulting product unit cell constant is 2.501 nanometers, and the chemical composition of the product is Na 2 O=14%, K 2 O=11%, SiO 2 =41%, Al 2 o 3 = 34%, RE 2 o 3 =0.15%, Fe 2 o 3 =0.1%, benzene adsorption capacity 170mg / g, whiteness 83%, specific surface area 590m 2 / g, the...

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Abstract

A process for preparing X-type zeolite with low Si / Al ration and the crystal cell constant greater than or equal to 2.5 nano includes such steps as adding the mixture of sodium hydroxide and potassium hydroxide and water glass and / or aluminium source to the dregs and / or mother liquid of catalyst factor, mixing to make that the components have such mole ratios as Na2O (4-6), K2O (1-2.5), Al2O3, SiO2 (1-3) and H2O (50-250), ageing at 20-50 deg.C for 1-4 days, and hydrothermal crystallizing at 50-90 deg.C for 10-40 hr.

Description

technical field [0001] The invention relates to a preparation method of X-type zeolite, in particular to a method for synthesizing low-silicon-aluminum ratio X-type zeolite by using catalyst plant waste residue and / or mother liquor as part of raw materials. Background technique [0002] X-type zeolite can be used as adsorbent and detergent builder, and is one of the most used zeolites. The earliest published preparation method is to use water glass and sodium aluminate hydrothermal method to synthesize, that is, to mix water glass and sodium aluminate into a gel and then hydrothermally crystallize at about 100 ° C, as described in USP2882244; The crystallization directing agent used. The composition of X zeolite is 0.9±0.2M 2 / n O·Al 2 o 3 2.5±0.5SiO2 2 ·xH 2 O (wherein M represents alkali metal or alkaline earth, n is the valence number of the metal, and x takes any number up to 8, depending on the nature of the metal M and the degree of crystal hydration). [0003] T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/22
Inventor 杨小明罗京娥
Owner CHINA PETROLEUM & CHEM CORP