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Silica microspheres and its preparation method

A technology of silica gel and microspheres, applied in chemical instruments and methods, silica, silica, etc., can solve the problems of inability to obtain specific surface area and pore volume of silica gel microspheres, and achieve the effect of high pore volume

Active Publication Date: 2011-09-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is the technical problem that the prior art cannot obtain microsphere silica gel with high specific surface area and pore volume, and a new microsphere silica gel is provided

Method used

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  • Silica microspheres and its preparation method

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Effect test

Embodiment 1

[0015] 15% (weight, as SiO 2 (meter) water glass and 10% (weight) of sulfuric acid are mixed by the nozzle place, adjust the pH of the mixed solution to 6.5 by adjusting the ratio of the two materials and then form in the oil column with a temperature of 50 ° C, and the hydrogel is formed from the lower end of the oil column The aqueous layer was removed. The hydrogel was washed with running water until the eluate was 1% (wt) AgNO 3 The aqueous solution showed a negative reaction, and then the hydrogel was transferred to an equal volume of 2-(sodiumsulfophenyl)ethylsiloxane aqueous solution with a weight concentration of 5%, adjusted to pH 8.0 with ammonia water, and soaked at room temperature for 3 hours. Then the temperature was raised to 90° C. and kept (ie, aged) for 24 hours. After filtering, the aged hydrogel was dried in a blast oven at 80°C for 8 hours, and then fired in a muffle furnace at 400°C for 4 hours. The specific surface area of ​​the microsphere silica gel...

Embodiment 2

[0022] 10% (weight, SiO 2 The water glass of meter) and the sulfuric acid of 15% (weight) are mixed by the nozzle place, by adjusting these two kinds of material proportions, the pH of the mixed solution is adjusted to 7.0, then it is molded in the oil column that the temperature is 80 ℃, and the hydrogel is formed from the oil The water layer at the lower end of the column is raised. The hydrogel was washed with water until the eluate was 1 wt% AgNO 3 The aqueous solution shows negative reaction, then the hydrogel is transferred to an equal volume of weight concentration of 30% 3-(sodium sulfonate) propylsiloxane aqueous solution, adjusted to pH6.0 with acetic acid and soaked at room temperature for 4 hours, then Raise the temperature to 40°C for aging for 48 hours. After filtering, the aged hydrogel was dried in a blast drying oven at 120°C for 8 hours, and then calcined in a muffle furnace at 600°C for 4 hours. The specific surface area of ​​the microsphere silica gel wa...

Embodiment 3

[0025] 15% (weight, as SiO 2 The water glass of meter) and the sulfuric acid of 20% (weight) are mixed by nozzle place, by adjusting these two kinds of material proportions, mixed solution pH is adjusted to 8.0, is then formed in the oil column that temperature is 65 ℃, and hydrogel is formed from oil The water layer at the lower end of the column is raised. The hydrogel was washed with water until the eluate was 1 wt% AgNO 3 The aqueous solution showed a negative reaction, and then the hydrogel was transferred to an equal volume of 17% 3-(sodium sulfonate-2-hydroxyl-propoxyl) propylsiloxane aqueous solution, and adjusted to pH6. 0 and soak at room temperature for 5 hours, then heat up to 60°C and age for 12 hours. After filtering, the aged hydrogel was dried in a blast oven at 90°C for 8 hours, and then fired in a muffle furnace at 450°C for 4 hours. The specific surface area of ​​the microsphere silica gel was measured to be 476 square meters per gram, and the pore volume...

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Abstract

The invention relates to silica microspheres and its preparation method, which mainly solves the problem of the unavailable silica microspheres with a high specific surface area and pore volume existing in the prior art. Silica microspheres adopted in the invention is characterized in that the specific surface is 350 to 500 square meters per gram and the pore volume is 1.3 to 1.6 cubic centimeters per gram, and the invention also provides the method for producing the silica microspheres. The method comprises the following steps: (A) mixing water glass and a sulfuric acid aqueous solution for obtaining a mixed liquor with a pH value of 6.5 to 10; (B) dropping the mixed liquor obtained from the step (A) into an oil column forming device for producing hydrogel; (C) washing, aging, drying and roasting the hydrogel for obtaining silica, wherein an aqueous solution for aging contains at least one organosilicon from 2-(sodium sulfophenyl ) ethyl siloxane, 3-(sulfonate ) propyl group siloxane and 3-(sulfonate-2-hydroxy-propanolato) for solving the problem, the present invention can be used for the industrial production of silica microspheres.

Description

technical field [0001] The invention relates to a microsphere silica gel and a preparation method thereof. Background technique [0002] Microsphere silica gel is a kind of porous substance, which is commonly used as catalyst carrier. According to the specific surface and pore volume index of microsphere silica gel, microsphere silica gel can be roughly divided into four categories. The first type, the pore volume is generally 1.0-2.0 cubic centimeters / g, and the specific surface is generally 150-300 square meters / g. This type of silica gel is usually called macroporous microsphere silica gel; the second type, the pore volume is generally 0.8- 1.2 cubic centimeters per gram, the specific surface is generally 300-500 square meters per gram, this type of silica gel is usually called coarse-porous microsphere silica gel; the third type, the pore volume is generally 0.60-0.65 cubic centimeters per gram, and the specific surface is generally 450-650 square meters / g, this type o...

Claims

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Application Information

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IPC IPC(8): C01B33/14C01B33/157C01B33/16B01J32/00
Inventor 张士福杨运信张丽斌宋朝红姚哲查晓钟秦群英
Owner CHINA PETROLEUM & CHEM CORP