CN103030150A - Technological process of mesoporous silica gel - Google Patents

Technological process of mesoporous silica gel Download PDF

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Publication number
CN103030150A
CN103030150A CN201210578059XA CN201210578059A CN103030150A CN 103030150 A CN103030150 A CN 103030150A CN 201210578059X A CN201210578059X A CN 201210578059XA CN 201210578059 A CN201210578059 A CN 201210578059A CN 103030150 A CN103030150 A CN 103030150A
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silica gel
mesoporous silica
reaction tower
water washing
reaction
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CN201210578059XA
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Inventor
乔伟光
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Qingdao Zhongneng Group Co Ltd
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Qingdao Zhongneng Group Co Ltd
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Priority to CN201210578059XA priority Critical patent/CN103030150A/en
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Abstract

The invention relates to a technological process of mesoporous silica gel. Mixing, reaction and water washing are conducted through an alkali preparation pool, an acid preparation tank, a reaction tower and a water washing tank. The technological process comprises the specific steps that a sodium silicate solution with the SiO2 content of 20-30% is prepared through the alkali preparation pool on silica gel production equipment at 30-35 DEG C; a sulfuric acid solution with the content of 25-35% is prepared in the acid preparation tank at 30-35 DEG C; the sulfuric acid solution is added to the reaction tower; the prepared sodium silicate solution is added to the reaction tower; silica gel particles are formed after reaction, and aged for 15-18h in an acid solution with a PH value of 1-3, enter the water washing tank, and are subjected to water washing in 40-45 DEG C water, soaked with ammonia for 6-8h after the water washing is completed, and then subjected to filter pressing and drying in an oven; and then the mesoporous silica gel is obtained.

Description

A kind of mesoporous silica gel technical process
Technical field
The invention belongs to silica gel manufacturing technology field, be specifically related to a kind of mesoporous silica gel technical process.
Background technology
The Application Areas of silica gel is day by day extensive; see with regard to present should being used for; be mainly mesoporous silica gel at its silica gel dry and provide protection of the field of food such as tealeaves; mesoporous silica gel has all obtained good application in Application Areass such as flocculating aids, matting agent, tactile flat agent, support of the catalyst, selective adsorptions in addition, and existing Technology is also not obvious in the effect that size-grade distribution obtains at present.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, has proposed a kind of mesoporous silica gel technical process, and described mesoporous silica gel carries out the colloidal sol reaction by water glass and sulfuric acid and makes, and its reaction signal formula is:
Na 2SiO 3+H 2SO 4 Na 2SO 4+H 4SiO 4
H 4SiO 4
Figure 376099DEST_PATH_IMAGE001
SiO 2· nH 2 O
Technical scheme of the present invention is: a kind of mesoporous silica gel technical process, and to mix, react and wash by joining alkali pond, complex acid tank, reaction tower and water washing tank, the concrete technology flow process is: prepare SiO by joining the alkali pond on silica gel production equipment 2Content is the sodium silicate solution of 20-30%, temperature is 30-35 ℃, configuration content is the sulphuric acid soln of 25-35% in the complex acid tank, temperature is 30-35 ℃, sulphuric acid soln is joined in the reaction tower, again the sodium silicate solution for preparing is joined in the reaction tower, form silica gel particle after the reaction, silica gel particle is after in the acidic solution of pH value at 1-3 aging 15-18 hour, enter into water washing tank, wash in 40-45 ℃ water, washing was carried out the ammonia bubble 6-8 hour behind terminal point, then press filtration oven dry in baking oven namely gets mesoporous silica gel.
The reaction tower interior reaction temperature is 80-90 ℃.
Washing time is 35-40 hour in the water washing tank.
The temperature of press filtration baking stage baking oven is 100-150 ℃, and drying time is 48-52 hour.
The present invention has following beneficial effect:
1) need not starting material are carried out special processing.
2) production process is all carried out under condition of normal pressure, is conducive to large-scale production.
3) washing temperature is carried out at normal temperatures in the water washing process, the silica gel even particle size distribution that makes.
4) can in water washing process, carry out according to client's needs reaming and process, satisfy different clients' index request.
5) shortened the production cycle, utilization ratio of device obviously improves.
Further specify the present invention below in conjunction with embodiment.
Embodiment
Below be embodiment of the present invention:
Embodiment 1:
First 10 liter of 25% sulphuric acid soln joined experiment with in the reaction tower, again with 6 liters of SiO that prepare 2Content is that 30% sodium silicate solution is injected to experiment with in the reaction tower, temperature is 81 ℃ in the tower, after in the acidic solution of pH value at 1-3 aging 16 hours, enter into the experimental water cleaning of evaporator, in 41 ℃ water, wash, carried out the ammonia bubble after the washing to 37 hour 7 hours, then the temperature of press filtration baking stage baking oven is 100 ℃, and drying time is 48 hours experimental datas such as tables 1.
Table 1 experimental data table
Figure 899485DEST_PATH_IMAGE002
Embodiment 2:
First 10 liter of 35% sulphuric acid soln joined experiment with in the reaction tower, again with 6 liters of SiO that prepare 2Content is that 25% sodium silicate solution is injected to experiment with in the reaction tower, temperature is 85 ℃ in the tower, after in the acidic solution of pH value at 1-3 aging 17 hours, enter into the experimental water cleaning of evaporator, in 44 ℃ water, wash, carried out the ammonia bubble after the washing to 36 hour 7 hours, then the temperature of press filtration baking stage baking oven is 120 ℃, and drying time is 52 hours experimental datas such as tables 2.
Table 2 experimental data table
Figure 201210578059X100002DEST_PATH_IMAGE003
Embodiment 3:
First 10 liter of 30% sulphuric acid soln joined experiment with in the reaction tower, again with 6 liters of SiO that prepare 2Content is that 20% sodium silicate solution is injected to experiment with in the reaction tower, temperature is 89 ℃ in the tower, after in the acidic solution of pH value at 1-3 aging 15 hours, enter into the experimental water cleaning of evaporator, in 42 ℃ water, wash, carried out the ammonia bubble after the washing to 36 hour 7 hours, then the temperature of press filtration baking stage baking oven is 140 ℃, and drying time is 49 hours experimental datas such as tables 3.
Table 3 experimental data table
Figure 735854DEST_PATH_IMAGE004
Embodiment 4:
First 10 liter of 32% sulphuric acid soln joined experiment with in the reaction tower, again with 6 liters of SiO that prepare 2Content is that 30% sodium silicate solution is injected to experiment with in the reaction tower, temperature is 85 ℃ in the tower, after in the acidic solution of pH value at 1-3 aging 18 hours, enter into the experimental water cleaning of evaporator, in 44 ℃ water, wash, carried out the ammonia bubble after the washing to 39 hour 7 hours, then the temperature of press filtration baking stage baking oven is 148 ℃, and drying time is 50 hours experimental datas such as tables 4.
Table 4 experimental data table
Figure 508637DEST_PATH_IMAGE005
Embodiment 5:
First 10 liter of 30% sulphuric acid soln joined experiment with in the reaction tower, again with 6 liters of SiO that prepare 2Content is that 20% sodium silicate solution is injected to experiment with in the reaction tower, temperature is 90 ℃ in the tower, after in the acidic solution of pH value at 1-3 aging 18 hours, enter into the experimental water cleaning of evaporator, in 42 ℃ water, wash, carried out the ammonia bubble after the washing to 38 hour 7 hours, then the temperature of press filtration baking stage baking oven is 130 ℃, and drying time is 49 hours experimental datas such as tables 5.
Table 5 experimental data table
Figure 783761DEST_PATH_IMAGE006

Claims (4)

1. mesoporous silica gel technical process is characterized in that: mix, react and wash by joining alkali pond, complex acid tank, reaction tower and water washing tank, the concrete technology flow process is: prepare SiO by joining the alkali pond on silica gel production equipment 2Content is the sodium silicate solution of 20-30%, temperature is 30-35 ℃, configuration content is the sulphuric acid soln of 25-35% in the complex acid tank, temperature is 30-35 ℃, sulphuric acid soln is joined in the reaction tower, again the sodium silicate solution for preparing is joined in the reaction tower, form silica gel particle after the reaction, silica gel particle is after in the acidic solution of pH value at 1-3 aging 15-18 hour, enter into water washing tank, wash in 40-45 ℃ water, washing was carried out the ammonia bubble 6-8 hour behind terminal point, then press filtration oven dry in baking oven namely gets mesoporous silica gel.
2. mesoporous silica gel technical process according to claim 1 is characterized in that: the reaction tower interior reaction temperature is 80-90 ℃.
3. mesoporous silica gel technical process according to claim 1 and 2 is characterized in that: washing time is 35-40 hour in the water washing tank.
4. mesoporous silica gel technical process according to claim 3 is characterized in that: the temperature of press filtration baking stage baking oven is 100-150 ℃, and drying time is 48-52 hour.
CN201210578059XA 2012-12-26 2012-12-26 Technological process of mesoporous silica gel Pending CN103030150A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103539134A (en) * 2013-09-23 2014-01-29 安徽良臣硅源材料有限公司 Preparation method of drink stabilizer silica gel
CN104860322A (en) * 2015-05-07 2015-08-26 中国海洋石油总公司 Low-sodion-content high-purity silica solution preparation method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1363514A (en) * 2001-01-11 2002-08-14 青岛美晶化工有限公司 macroreticular silica gel and its preparing process
CN101327931A (en) * 2008-07-24 2008-12-24 青岛美高集团有限公司 Silica gel cleaning production method and sulfuric acid production method
CN101591022A (en) * 2009-06-29 2009-12-02 青岛中能集团有限公司 A kind of preparation process of high-purity silica gel and method
CN101591021A (en) * 2009-06-29 2009-12-02 青岛中能集团有限公司 A kind of preparation method of thick-hole block silica gel

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1363514A (en) * 2001-01-11 2002-08-14 青岛美晶化工有限公司 macroreticular silica gel and its preparing process
CN101327931A (en) * 2008-07-24 2008-12-24 青岛美高集团有限公司 Silica gel cleaning production method and sulfuric acid production method
CN101591022A (en) * 2009-06-29 2009-12-02 青岛中能集团有限公司 A kind of preparation process of high-purity silica gel and method
CN101591021A (en) * 2009-06-29 2009-12-02 青岛中能集团有限公司 A kind of preparation method of thick-hole block silica gel

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103539134A (en) * 2013-09-23 2014-01-29 安徽良臣硅源材料有限公司 Preparation method of drink stabilizer silica gel
CN104860322A (en) * 2015-05-07 2015-08-26 中国海洋石油总公司 Low-sodion-content high-purity silica solution preparation method

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Application publication date: 20130410