SU1018706A1 - Method of producing alumosilicate adsorbent - Google Patents

Abstract

METHOD FOR OBTAINING ALYUMOSILICATE ADSORBENT - in-spinning mixing of Baiv silicate solution. with chemical reagent, forming a spherical hydrogel from the resulting mixture In oil, syneresis, actnevaish: aluminum sulphate solution, washing, drying and calcining, so that with the aim of increasing thermocouple steel an adsorbent during multi-cycle operation, a solution of sulfuric acid is used as a chemical reagent, syneresis is carried out at, and the activation of a solution of sulfuric acid aluminum is carried out at pH 3, 0-4.5.

Description

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ha The invention relates to the use of mineral adsorbents, in particular, synthetic alumina silicate adsorbents, and can be used in the production of adsorbents in Bianou oil refineries and chemical industries widely used in the processes of continuous adsorption purification and separation of petroleum products and complex organic mixtures in motion. adsorbent layer from aromatic, sulfurous, nitrogenous and resinous compounds and other impurities. There is a known method of producing aluminosilicate by adding to water alkali metal silicate solution. first mismatch of alumina A 62 (the amount of which should be enough to react with 30-90 wt.% alkali metal silicate, aged (synergizing) the resulting aluminosilicate gel for 2-180 minutes and adding a second source sodium macinate aluminate or aluminum sulphate, the alumina obtained from these two sources being 8-50% by weight of the aluminosilicate. The resulting hydrogel is separated, washed, dried, pro; potassium C 1 However, the resulting aluminosilicate is not suitable for adsorptive purification of the products due to its fine-pore structure. The method of preparation of aluminum silicate and the formation of a spherical adsorbent is closest to the invention in terms of its technical nature and results. Hydrogel in Oil, snreeze 42–55 ° C for 9–12 h at pH 8.5–9.2, activated with a solution of sulfur-containing aluminum with concentration OOD, 13ODZ (pH 2.5), washing, drying at. 100-170 ° C and calcining at 650-75 ° G in a vapor-air environment 10 hours С 3. A disadvantage of the known method is that during high-cycle thermal and thermocouple processing, the adsorption activity of the sorbent is significantly reduced,. The aim of the invention is to increase the thermocouple stability of the adsorbent during high-cycle operation. The goal is achieved in that according to the method, which consists in mixing sodium silicate and sulfuric K.0 SLOT solutions, forming a spherical hydrogel with subsequent blue-resis stages at 28-38 ° C, activated with a solution of aluminum sulfate with a pH 3-4.5, washing, drying and calcining in a vapor-air medium, paciBop sulfuric acid is used as a source reagent, the synerysis is carried out at 28-38 0, and activation with aluminum sulphate is carried out at pH 3, 0-4.5. The use of a solution of sulfuric acid in the form of a hydrogel makes it possible to obtain a silica gel matrix, which in the process of syneresis forms wide-porous structures with a large specific pore volume and a large specific surface. Conducting a syneresis stage under the indicated mode allows obtaining an optimal adsorbent structure: specific pore volume 0.75-1.0 cm / g, specific surface area 36 0-510. Carrying out the process of syneresis at 28 ° C leads to the formation of a fine-pore structure and. decrease in thermocouple stability, as a result of which the adsorption activity (ensuring the ability) of the adsorbent decreases, and at a syneresis temperature of more than 38 ° C, the total mass and specific surface area of the adsorbent decrease, which leads to a sharp decrease in the productivity of the process with a moving layer of adsorbent on the processed raw material. The occurrence of hydrodynamic complications in the stages of liquid-phase processing of a solution of a raw material with a moving adsorbent. Activation of the hydrogel under the indicated regime with aluminum sulfate with a pJ of 3-4.5 provides the content of alumina in the adsorbent 2.5-5.0 wt.%, Which is necessary to obtain an adsorbent with good strength, regenerative. characteristic thermostable: nostasis and bleaching ability. Activation at lower pH levels does not ensure the introduction of a given amount of alumina into the adsorbent, when the upper limits of pH are activated, it is not advisable to activate the pH, since the content of aluminum in the adsorbent does not increase. The technology of the method lies in the image of the ...}.,:. Solutions of sodium silicate and sulfuric acid are mixed, and the known methods are used to form a hydrogel in a hydrocarbon medium, which is then deposited in predetermined modes and conditions of syneresis, activation, washing, drying and calcining. Example, Mix 400 l of an Iy solution of sodium silicate with 200 l of Zn of a solution of sulfuric acid I1 made the formation of hydrogel balls in a hydrocarbon medium (oil), which are subjected to syneresis at pH 8.0-8.5 for 12 hours, activation 0, 13 N, a solution of aluminum sulfate with a pH of 4. Then the heated hydrogel is washed from sodium ions, dried at 11 ° and calcined in medium (30% steam) at, PRI me R 2. Mix 4OO l 2, silicate solution rub with 20O l Zn. sulfuric acid solution and the implementation of the formation of hydrogel spherical balls in a hydrogen-hydrogen medium. Hydrogel beads are subjected to syneresis at 28 ° C, pH 8–8.5 for 12 h, activation 0.13 n. With a solution of sulfuric acid alumina with jW 4.0, Over: the hydrogel is then washed, dried and calcined as in Example 1. EXAMPLE 3. 400 L of 2N sodium silicate solution with 2OO l. pacTBdpa of sulfuric acid and the hydrogel beads are formed at an angle. a hydrohydrogenous medium, a hydrogel is subjected to seikerviu at an EFR of 8.5 within 12 h, an activation of 0.13. - a solution of sulfate e lumini with p 3,0, then the resulting gddrogel is washed, dried, and calcined, as in. example; 1. v-v. ; . : PRI me R 4. Hang 400 l 2 n. sodium silicate solution with 20O l. Zn a solution of sulfuric humus and osusheoev; nfopff formation of hydrogel globules in a hydrocarbon medium. Sharshna hydrogel is subjected to synergy at 33 ° C, pH 88,: 5 for 2 h; activation of ODL., i with aluminum sulphate solution with pH 4 Then the hydrogel was washed, P1X was dissolved as, v; example 13. li p im 5 (tmeshivug 400 l 2iH. solution of sodium silicate with 2OO l. of acid solution and carry out the formation of balls of hydrogel in the hydrocarbon medium. The hydrogel balls are subjected to syneresis at 33 ° C, pH 88, 5 for 12 h, the activation of 0.13 N. gshyumini sulfate solution with a pH of 4.5. Then the hydrogel is washed, dried and calcined, as in example 1. EXAMPLE 6 4OO l of 2N sodium silicate solution and 2OO l are mixed Known sulfuric acid solution and carried out the formation of hydrogel balls into a hydrocarbon medium. The hydrogel beads are subjected to a synergy at 35 ° C, pH 88, 5 for 2 h, activated with 0.13 N. aluminum sulphate solution with pH 3.0. Then the hydrogel is washed, dried and calcined, as in the example. sodium silicate and 2OO liter of HCl solution, sulfuric acid, and hydrogel beads are formed in a water-borne medium. Hydrogel beads are subjected to syneresis at pH 8-8.5 for 2 hours, activated with 3N aluminum sulphate solution pH 4.0 Then wash the hydrogel, dry and saline, as in Example 1. Example 8. Mix 4OO l. sodium silicate solution and 200 l | 3n. solution of sulfuric acid and exercise; l) t forming hydrogel balls into yiv. Lehydrogen environment. Hydrogel balls are subjected to syneresis at 37 ° C, pH 88.5 for 12 hours, activation of U, 13 n. With aluminum sulphate solution with pH 4.0. Then the hydrogel is washed, dried and calcined, as in Example 1, Table shows indicators of the initial adsorbents, assessed by the proposed method and by e-. known, and after mech-cyclic operation in the stages of the stages of adsorption-lesorb.-drying-regeneration (when the equilibrium mode of the process is established).

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Claims (1)

METHOD FOR PRODUCING ALUMINOSILICATE ADSORBENT, including mixing a solution of sodium silicate with a chemical reagent, forming a spherical hydrogel from the resulting mixture in oil, syneresis, activating a solution of aluminum sulfate, washing, drying and calcining, characterized in that, in order to increase the thermocouple stability of the adsorbent during multi-cycle operation, a solution of sulfuric acid is used as a chemical reagent, syneresis is carried out at 28-38 ° С, and activation of aluminum sulfate solutions is carried out at a pH of 3.0-4.5. "