CN100337912C - Process for mfg. water resisting type large pore spherical silica gel - Google Patents
Process for mfg. water resisting type large pore spherical silica gel Download PDFInfo
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- CN100337912C CN100337912C CNB2005101046111A CN200510104611A CN100337912C CN 100337912 C CN100337912 C CN 100337912C CN B2005101046111 A CNB2005101046111 A CN B2005101046111A CN 200510104611 A CN200510104611 A CN 200510104611A CN 100337912 C CN100337912 C CN 100337912C
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Abstract
The present invention discloses a manufacturing method for waterproof macroporous spherical silica gel, which is characterized in that after sodium silicate reacts with diluted sulfuric acids to generate spherical gel, the spherical gel is treated by the following processes: ageing, steaming, drying, ignition, acid soaking, aqueous wash and drying. The effect of carrying out drying and ignition first and then acid soaking and aqueous wash lies in that when ignition is carried out, a great amount of sulfate in the pore structure of the spherical gel is in a melting expansion state, thereby relatively enlarging pore volume and pore diameter; in the process of acid soaking after ignition, sulfate in silica gel is dissolved, and therefore, the pore size distribution of the generated silica gel is relatively homogeneous and concentrated, and the skeleton structure of the generated silica gel is fixed to accurately control the pore size distribution range of the silica gel; consequently, the pore structure does not change in the post-treatment process; as the inner structure of the silica gel is partially sintered in the ignition process, the pore size distribution is made to be stable, and the non-explosion rate of the silica gel in water is increased.
Description
Technical field
The present invention relates to a kind of manufacture method of silica gel, specifically a kind of manufacture method of large pore spherical silica gel.
Background technology
In existing silica gel product, a kind of large pore spherical silica gel is arranged, and its manufacture method is that prepared in reaction in conversion unit goes out the gel grain by sodium silicate solution and dilution heat of sulfuric acid, this gel grain is handled through aging → acid bubble → washing → drying process again, makes the large pore spherical silica gel product.Also have another kind of manufacture method, the gel grain is handled through acid bubble → washing → aging → quadratic acid bubble → drying process, makes the large pore spherical silica gel product.
The common feature of above-mentioned technology is to carry out earlier carrying out drying again after acid bubble, the washing.This process sequence finds to exist some deficiency through actual survey, carry out earlier in the art breading drying processing after acid bubble, the washing, to cause it when reaming is carried out in the oven dry processing, make its some aperture sintering, cause its silica gel pore volume less relatively, can cause the skeleton structure instability, the silica gel pore size distribution is inhomogeneous, specific surface is less, when making support of the catalyst, is unfavorable for reacting requirement.
In addition, in the prior art, the reaming aftertreatment technology adopts steam treatment and soaks the salt processing, and this method technology is loaded down with trivial details, and the cycle is long, and productivity is low, cost height, reaming DeGrain.
How overcoming above-mentioned deficiency, then is the design problem that the present invention faced.
Summary of the invention
The invention provides a kind of manufacture method of water resisting type large pore spherical silica gel, it can solve macroporous silica gel skeleton structure instability, and pore size distribution is inhomogeneous, meets problems such as water bursts.
In order to reach the purpose that solves the problems of the technologies described above, technical scheme of the present invention is, a kind of manufacture method of water resisting type large pore spherical silica gel, after it is characterized in that water glass and dilute sulphuric acid prepared in reaction gel ball, undertaken by following process sequence: aging → decatize → oven dry → calcination → acid bubble → washing → oven dry, the mean pore size 35-40nm of described large pore spherical silica gel.
In the present invention, also have following technical characterictic: described twice oven dry treatment process: bake out temperature is 120-200 ℃, and drying time is 10-50 hour; Calcination technology is: calcination temperature is 500-900 ℃, and calcination time is 20-120 minute.
In the present invention, also have following technical characterictic: described acid bubble treatment process: carry out the acid bubble with 1-4% sulfuric acid, hydrochloric acid or nitric acid and handle, the sour bubble time is 2-8 hour.
In the present invention, also has following technical characterictic: handled 2-8 hour for burin-in process technology: 25-30 ℃; Decatize treatment process: vapor pressure: 0.05-0.6MPa, the logical 2-20 hour vapour time; Washing process:, be washed till pH value at 5-7.5 with 30-90 ℃ of washing.
In the present invention, also have following technical characterictic: the macroporous silica gel of described method manufacturing has following performance index: mean pore size 35-40nm, pore volume 1.30-1.35ml/g, specific surface 130-154m
2/ g.
The invention has the beneficial effects as follows, 1. dry earlier, calcination, after carry out acid bubble, water washing effect is, during calcination, the a large amount of vitriol melting expansion that exists in its pore structure, can make pore volume, the aperture all enlarges relatively, sour again bubble is with the vitriol stripping in the silica gel after the calcination, can make the silica gel pore size distribution of generation more even like this, concentrate, and its skeleton structure is fixed, and can control the silica gel pore size distribution range exactly, it is no longer changed at the aftertreatment technology central hole structure, the calcination treating processes has the effect of partially sintering to the silica gel internal structure, can play the effect of stablizing pore size distribution and can improve its chance water not burst rate.2. carrying out the advantage that decatize is handled under the 0.05-0.6MPa pressure is: this technology generations has been replaced traditional inorganic salt chambering process and high temperature poach chambering process, the sodium sulfate that retains with the glue process carries out reaming by decatize, has stable reaming effect, and shortened the production cycle, reduce cost, improved production efficiency.3. improve the not fried rate performance index of chance water, met the not fried rate of water 〉=98% after tested.
Embodiment
Embodiment 1:
The manufacturing approach craft process of large pore spherical silica gel of the present invention is as follows:
1. water glass and dilute sulphuric acid prepared in reaction gel ball;
2. burin-in process technology: handled 2 hours for 25 ℃;
3. decatize treatment process: vapor pressure: 0.1MPa, logical 8 hours vapour time;
4. oven dry treatment process: bake out temperature is 120 ℃, and the time is 10 hours;
5. the calcination treatment process is: calcination temperature is 500 ℃, and calcination time is 100min;
6. treatment process is steeped in acid: carry out the acid bubble with 1-4% sulfuric acid and handle, the sour bubble time is 2 hours;
7. washing treatment process:, be washed till pH value at 5-7.5 with 55 ℃ of washings;
8. oven dry treatment process: bake out temperature is 120 ℃, and the time is 10 hours.
Embodiment 2:
The manufacturing approach craft process of large pore spherical silica gel of the present invention is as follows:
1. water glass and dilute sulphuric acid prepared in reaction gel ball;
2. burin-in process technology: handled 8 hours for 30 ℃;
3. decatize treatment process: vapor pressure: 0.3MPa, logical 6 hours vapour time;
4. oven dry treatment process: bake out temperature is 200 ℃, and the time is 40 hours;
5. the calcination treatment process is: calcination temperature is 600 ℃, and calcination time is 80min;
6. treatment process is steeped in acid: carry out the acid bubble with 1-4% sulfuric acid and handle, the sour bubble time is 8 hours;
7. washing treatment process:, be washed till pH value at 5-7.5 with 40-45 ℃ of washing;
8. oven dry treatment process: bake out temperature is 200 ℃, and the time is 50 hours.
Embodiment 3:
The manufacturing approach craft process of large pore spherical silica gel of the present invention is as follows:
1. water glass and dilute sulphuric acid prepared in reaction gel ball;
2. burin-in process technology: handled 5 hours for 27 ℃;
3. decatize treatment process: vapor pressure: 0.4MPa, logical 8 hours vapour time;
4. oven dry treatment process: bake out temperature is 150 ℃, and the time is 30 hours;
5. the calcination treatment process is: calcination temperature is 700 ℃, and calcination time is 80min;
6. treatment process is steeped in acid: carry out the acid bubble with 1-4% sulfuric acid and handle, the sour bubble time is 5 hours;
7. washing treatment process:, be washed till pH value at 5-7.5 with 45-50 ℃ of washing;
8. oven dry treatment process: bake out temperature is 150 ℃, and the time is 30 hours.
Embodiment 4:
The manufacturing approach craft process of large pore spherical silica gel of the present invention is as follows:
1. water glass and dilute sulphuric acid prepared in reaction gel ball;
2. burin-in process technology: handled 6 hours for 26 ℃;
3. decatize treatment process: vapor pressure: 0.5MPa, logical 6 hours vapour time;
4. oven dry treatment process: bake out temperature is 160 ℃, and the time is 36 hours;
5. the calcination treatment process is: calcination temperature is 750 ℃, and calcination time is 60min;
6. treatment process is steeped in acid: carry out the acid bubble with 1-4% sulfuric acid and handle, the sour bubble time is 6 hours;
7. washing treatment process:, be washed till pH value at 5-7.5 with 55-60 ℃ of washing;
8. oven dry treatment process: bake out temperature is 160 ℃, and the time is 36 hours.
Embodiment 5:
The manufacturing approach craft process of large pore spherical silica gel of the present invention is as follows:
1. water glass and dilute sulphuric acid prepared in reaction gel ball;
2. burin-in process technology: handled 8 hours for 28 ℃;
3. decatize treatment process: vapor pressure: 0.6MPa, logical 8 hours vapour time;
4. oven dry treatment process: bake out temperature is 170 ℃, and the time is 30 hours;
5. the calcination treatment process is: calcination temperature is 850 ℃, and calcination time is 50min;
6. treatment process is steeped in acid: carry out the acid bubble with 1-4% sulfuric acid and handle, the sour bubble time is 5 hours;
7. washing treatment process:, be washed till pH value at 5-7.5 with 50-55 ℃ of washing;
8. oven dry treatment process: bake out temperature is 170 ℃, and the time is 30 hours.
Embodiment 6:
The manufacturing approach craft process of large pore spherical silica gel of the present invention is as follows:
1. water glass and dilute sulphuric acid prepared in reaction gel ball;
2. burin-in process technology: handled 2 hours for 25 ℃;
3. decatize treatment process: vapor pressure: 0.06MPa, logical 2 hours vapour time;
4. oven dry treatment process: bake out temperature is 120 ℃, and the time is 10 hours;
5. the calcination treatment process is: calcination temperature is 500 ℃, and calcination time is 20min;
6. treatment process is steeped in acid: carry out the acid bubble with 1-4% sulfuric acid and handle, the sour bubble time is 2 hours;
7. washing treatment process:, be washed till pH value at 5-7.5 with 55-60 ℃ of washing;
8. oven dry treatment process: bake out temperature is 120 ℃, and the time is 10 hours.
Embodiment 7:
The manufacturing approach craft process of large pore spherical silica gel of the present invention is as follows:
1. water glass and dilute sulphuric acid prepared in reaction gel ball;
2. burin-in process technology: handled 8 hours for 30 ℃;
3. decatize treatment process: vapor pressure: 0.6MPa, logical 20 hours vapour time;
4. oven dry treatment process: bake out temperature is 200 ℃, and the time is 50 hours;
5. the calcination treatment process is: calcination temperature is 900 ℃, and calcination time is 120min;
6. treatment process is steeped in acid: carry out the acid bubble with 1-4% sulfuric acid and handle, the sour bubble time is 8 hours;
7. washing treatment process:, be washed till pH value at 5-7.5 with 35-40 ℃ of washing;
8. oven dry treatment process: bake out temperature is 200 ℃, and the time is 50 hours.
In the above-described embodiments, the large pore spherical silica gel of manufacturing has following performance index: mean pore size 35-40nm, pore volume 1.30-1.35ml/g, specific surface 130-154m
2/ g meets the not fried rate of water 〉=98%.
The physical and chemical performance table of water-fast macroporous silica gel embodiment
| 10 | 35.8 | 151 | 1.35 |
Annotate: the physical and chemical performance testing tool in the table 2 is specific surface area, the pore analysis instrument of the SA3100 type of U.S. Beckman company product.
Certainly, the present invention is not limited to above-mentioned giving an example, and under main intention design of the present invention, the present invention also has the embodiment of some variations, also should belong to protection scope of the present invention.
Claims (5)
1. the manufacture method of a water resisting type large pore spherical silica gel, after it is characterized in that water glass and dilute sulphuric acid prepared in reaction gel ball, undertaken by following process sequence: aging → decatize → oven dry → calcination → acid bubble → washing → oven dry, the mean pore size 35-40nm of described large pore spherical silica gel.
2. method according to claim 1, it is characterized in that described twice oven dry treatment process: bake out temperature is 120-200 ℃, and drying time is 10-50 hour; Calcination technology is: calcination temperature is 500-900 ℃, and calcination time is 20-120 minute.
3. method according to claim 1 and 2, it is characterized in that described acid bubble treatment process: carry out the acid bubble with 1-4% sulfuric acid, hydrochloric acid or nitric acid and handle, the sour bubble time is 2-8 hour.
4. method according to claim 3 is characterized in that described burin-in process technology: handled 2-8 hour for 25-30 ℃; Decatize treatment process: vapor pressure: 0.05-0.6MPa, the logical 2-20 hour vapour time; Washing process:, be washed till pH value at 5-7.5 with 30-90 ℃ of washing.
5. method according to claim 4 is characterized in that the macroporous silica gel of described method manufacturing has following performance index: mean pore size 35-40nm, pore volume 1.30-1.35ml/g, specific surface 130-154m
2/ g.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101046111A CN100337912C (en) | 2005-12-23 | 2005-12-23 | Process for mfg. water resisting type large pore spherical silica gel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101046111A CN100337912C (en) | 2005-12-23 | 2005-12-23 | Process for mfg. water resisting type large pore spherical silica gel |
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| CN100337912C true CN100337912C (en) | 2007-09-19 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221705A (en) * | 1997-12-30 | 1999-07-07 | 化学工业部天津化工研究院 | Prodn. method of spherical silica gel |
| 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 |
| CN1522958A (en) * | 2003-02-21 | 2004-08-25 | 青岛海洋化工有限公司 | Process for manufacturing macroreticular spherical silica gel |
-
2005
- 2005-12-23 CN CNB2005101046111A patent/CN100337912C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221705A (en) * | 1997-12-30 | 1999-07-07 | 化学工业部天津化工研究院 | Prodn. method of spherical silica gel |
| 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 |
| CN1522958A (en) * | 2003-02-21 | 2004-08-25 | 青岛海洋化工有限公司 | Process for manufacturing macroreticular spherical silica gel |
Non-Patent Citations (1)
| Title |
|---|
| 大孔径硅胶的制备研究 张松涛，上海化工，第5期 1994 * |
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