CN214810843U - Colloidal silicon dioxide preparation device - Google Patents

Abstract

The utility model relates to a colloidal silica preparation facilities, including reation kettle, high temperature pump, filter and ultrafilter, reation kettle with the high temperature pump is connected, the high temperature pump with the filter is connected, the filter with the ultrafilter is connected, the ultrafilter with the reation kettle is connected; the outer wall of the reaction kettle is provided with a jacket, the jacket is used for heating the reaction kettle by circularly introducing steam when the reaction kettle is used for preparing silicon dioxide, and the jacket is used for cooling the reaction kettle by circularly introducing cooling water after the reaction of the reaction kettle is finished; the reation kettle is used for with the material via the high temperature pump is carried to the filter, the filter is carried to after filtering the material the ultrafilter, the ultrafilter carries to after concentrating the material after filtering reation kettle. The utility model discloses can realize silica granule under the high temperature and grow the while and filter the while concentration, still can avoid subsequent concentrated step simultaneously.

Description

Colloidal silicon dioxide preparation device

Technical Field

The utility model relates to a nano-particle preparation technical field especially relates to a colloidal silica preparation facilities.

Background

Colloidal silica, also called silica sol, is a dispersion of silica fine particles dispersed in water, and is widely used in catalysts, paints, precision casting, and the like, and in recent years, is widely used in the fields of Chemical Mechanical Polishing (CMP) and the like. Recently, with the continuous development of semiconductor technology, the continuous reduction of technology nodes, the continuous increase of the number of interconnection layers and the application of new materials and new processes, higher quality requirements are provided for colloidal silica abrasives, but the cost requirements are lower and lower.

The ion exchange method is a common method for preparing colloidal silicon dioxide, and the process generally comprises the steps of preparing silicic acid by ion exchange of dilute water glass, carrying out dehydration condensation nucleation on the silicic acid in a reaction kettle at a certain temperature and under certain conditions to grow into silicon dioxide particles, and concentrating the finally formed dilute silicon dioxide particles to obtain a finished product with a proper concentration (the general concentration is more than 30%). The evaporation speed of the reaction kettle is limited, the preparation period of the silicon dioxide particles is generally longer, the production efficiency is low, and a longer time of concentration step is needed after the preparation is finished to meet the requirement of the required concentration. The long preparation time not only brings difficulty to the quality control of the material, but also consumes too much energy such as required steam and the like, has high cost and is not economical and cost-effective.

SUMMERY OF THE UTILITY MODEL

The utility model aims to solve the technical problem that a colloidal silica preparation facilities is provided, can realize that silica granule grows while filtering the while concentration under the high temperature, still can avoid subsequent concentrated step simultaneously.

The utility model provides a technical scheme that its technical problem adopted is: providing a colloidal silica preparation device, which comprises a reaction kettle, a high-temperature pump, a filter and an ultrafilter, wherein the reaction kettle is connected with the high-temperature pump, the high-temperature pump is connected with the filter, the filter is connected with the ultrafilter, and the ultrafilter is connected with the reaction kettle;

the outer wall of the reaction kettle is provided with a jacket, the jacket is used for heating the reaction kettle by circularly introducing steam when the reaction kettle is used for preparing silicon dioxide, and the jacket is also used for cooling the reaction kettle by circularly introducing cooling water after the reaction of the reaction kettle is finished;

the reation kettle is used for with the material via the high temperature pump is carried to the filter, the filter is carried to after filtering the material the ultrafilter, the ultrafilter carries to after concentrating the material after filtering reation kettle.

The jacket is provided with a steam inlet for circularly introducing steam and a steam condensate outlet for circularly discharging the steam, and the jacket is also provided with a cooling water inlet for circularly introducing cooling water and a cooling water outlet for circularly discharging the cooling water.

The top of the reaction kettle is provided with a feed inlet, a feed back port and an exhaust port, and the reaction kettle is connected with the ultrafilter through the feed back port; the bottom of the reaction kettle is provided with a discharge port and a feeding port, and the reaction kettle is connected with the high-temperature pump through the feeding port.

A stirrer is arranged in the reaction kettle.

The reaction kettle is an enamel reaction kettle or a stainless steel reaction kettle.

The filter is provided with a sewage draining outlet.

The filter is a belt filter.

The ultrafilter is provided with a concentrated solution feed back outlet and a permeate discharge port, and is connected with the reaction kettle through the concentrated solution feed back outlet.

The ultrafilter comprises a membrane shell and an ultrafiltration membrane component, wherein the ultrafiltration membrane component is a hollow fiber type membrane or a tubular type membrane.

The reaction kettle, the high-temperature pump, the filter and the ultrafilter are integrated into a whole.

Advantageous effects

Since the technical scheme is used, compared with the prior art, the utility model, have following advantage and positive effect: the utility model integrates the reaction kettle, the high temperature pump, the filter and the ultrafilter, can realize the concentration of the silicon dioxide particles while growing at high temperature, can shorten the preparation period of the particles, can effectively remove the large particle number in the silicon dioxide particles, can avoid the subsequent concentration step, has simple process, greatly improves the preparation efficiency and the quality stability, and greatly reduces the steam energy consumption and the cost; the utility model discloses equipment simple and practical, small investment, with low costs and be fit for extensive volume production.

Drawings

Fig. 1 is a schematic structural view of a colloidal silica preparation apparatus according to an embodiment of the present invention.

The figure is as follows: 1. a reaction kettle; 2. a high temperature pump; 3. a filter; 4. an ultrafilter; 5. a feed inlet; 6. a feed back port; 7. an exhaust port; 8. a discharge port; 9. a feed port; 10. a steam inlet; 11. a steam condensate outlet; 12. a cooling water inlet; 13. a cooling water outlet; 14. a stirrer; 15. a sewage draining outlet; 16. a concentrated solution feed back outlet; 17. a permeate discharge port.

Detailed Description

The present invention will be further described with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the teachings of the present invention, and these equivalents also fall within the scope of the appended claims.

The embodiment of the utility model relates to a colloidal silica preparation facilities, as shown in figure 1, including reation kettle 1, high temperature pump 2, filter 3 and ultrafilter 4, reation kettle 1 with high temperature pump 2 passes through the tube coupling, high temperature pump 2 with filter 3 passes through the tube coupling, filter 3 with ultrafilter 4 passes through the tube coupling, ultrafilter 4 with reation kettle 1 passes through the tube coupling; the outer wall of the reaction kettle 1 is provided with a jacket, the jacket is used for heating the reaction kettle 1 by circularly introducing steam when the reaction kettle 1 is used for preparing silicon dioxide, and the jacket is also used for cooling the reaction kettle 1 by circularly introducing cooling water after the reaction of the reaction kettle 1 is finished; the reaction kettle 1 is used for conveying materials to the filter 3 through the high-temperature pump 2, the filter 3 filters the materials and then conveys the filtered materials to the ultrafilter 4, and the ultrafilter 4 concentrates the filtered materials and then conveys the concentrated materials to the reaction kettle 1.

Further, the first jacket is provided with a steam inlet 10 for circularly introducing steam and a steam condensate outlet 11 for circularly discharging steam, and the second jacket is provided with a cooling water inlet 12 for circularly introducing cooling water and a cooling water outlet 13 for circularly discharging cooling water.

Further, a feed inlet 5, a feed back port 6 and an exhaust port 7 are formed in the top of the reaction kettle 1, and the reaction kettle 1 is connected with the ultrafilter 4 through the feed back port 6; a discharge port 8 and a feeding port 9 are formed in the bottom of the reaction kettle 1, and the reaction kettle 1 is connected with the high-temperature pump 2 through the feeding port 9; a stirrer 14 is arranged in the reaction kettle 1; the reaction kettle 1 is an enamel reaction kettle or a stainless steel reaction kettle, and the working temperature range in the reaction kettle 1 is from room temperature to 100 ℃.

Further, the high-temperature pump 2 is a pump resistant to 100 ℃.

Further, the filter 3 is provided with a drain outlet 15; the filter 3 is a band filter.

Further, the ultrafilter 4 is provided with a concentrated solution return outlet 16 and a permeate discharge outlet 17, and the ultrafilter 4 is connected with the reaction kettle 1 through the concentrated solution return outlet 16; the ultrafilter 4 comprises a membrane shell resistant to 100 ℃ and an ultrafiltration membrane component, wherein the ultrafiltration membrane component is a hollow fiber type membrane or a tubular type membrane.

It is worth mentioning that reaction kettle 1, high temperature pump 2, filter 3 and ultrafilter 4 in this embodiment are integrated as an organic whole, and this design can realize silica granule under the high temperature and grow simultaneously filter the while and concentrate, can shorten granule preparation cycle, can effectively get rid of the big particle number (the particle number of being more than or equal to 0.56 micron) in the silica granule again, still can avoid subsequent concentrated step simultaneously, simple process, preparation efficiency and quality stability improve greatly, but steam energy consumption and cost greatly reduced.

The working process of the colloidal silica preparation apparatus of the present embodiment is as follows:

firstly, a certain amount of silicon dioxide crystal seeds are added into a reaction kettle 1 through a feeding hole 5 and are uniformly stirred through a stirrer 14, then steam is introduced from a steam inlet 10 on a jacket to heat the materials in the reaction kettle 1, and steam condensation hot water is discharged from a steam condensation water outlet 11. When the temperature of materials in a reaction kettle 1 is 100 ℃, silicic acid is added from a feeding port 5 at a certain feeding speed, the silicic acid is deposited and condensed on silicon dioxide crystal seed particles to enable the crystal seeds to grow up, when the volume of the materials in the reaction kettle 1 is high liquid level, the materials in the reaction kettle 1 are conveyed to a high-temperature pump 2 through a feeding port 9, then conveyed to a filter 3 through a high-temperature pump 2, filtered by the filter 3 and conveyed to an ultrafilter 4, the materials are concentrated in the ultrafilter 4, water is discharged from a permeate liquid discharge port 17 as permeate liquid, and the silicon dioxide concentrated liquid is conveyed to a return port 6 through a concentrated liquid return outlet 16 and is further concentrated after being mixed with the materials in the reaction kettle 1. The silicon dioxide particles are repeatedly circulated in the whole preparation system, and the material volume in the reaction kettle 1 is kept constant under a high liquid level by controlling the matching relation of the silicic acid feeding speed at the feeding port 5, the drainage speed at the permeate liquid discharge port 17 and the water vapor discharge speed at the exhaust port 7, so that the silicon dioxide particles grow, filter and concentrate in the whole system until the required particle size and concentration requirements are met. After the preparation reaction is finished, the steam input is closed, cooling water is introduced from the cooling water inlet 12 to cool the materials in the reaction kettle 1, and the cooling water is discharged from the cooling water outlet 13 through the jacket. After the temperature reduction is finished, materials in the reaction kettle 1 are conveyed to the appointed storage tank from the discharge hole 8.

Therefore, the utility model discloses with reation kettle, high temperature pump, filter and ultrafilter integration, can realize that silica granule grows while filtering the limit and concentrates under the high temperature, can shorten granule preparation cycle, can effectively get rid of the large granule number in the silica granule again, still can avoid subsequent concentrated step simultaneously.

Claims (10)

1. The colloidal silica preparation device is characterized by comprising a reaction kettle (1), a high-temperature pump (2), a filter (3) and an ultrafilter (4), wherein the reaction kettle (1) is connected with the high-temperature pump (2), the high-temperature pump (2) is connected with the filter (3), the filter (3) is connected with the ultrafilter (4), and the ultrafilter (4) is connected with the reaction kettle (1);

the outer wall of the reaction kettle (1) is provided with a jacket, the jacket is used for heating the reaction kettle (1) by circularly introducing steam when the reaction kettle (1) is used for preparing silicon dioxide, and the jacket is also used for cooling the reaction kettle (1) by circularly introducing cooling water after the reaction of the reaction kettle (1) is finished;

the reaction kettle (1) is used for conveying materials to the filter (3) through the high-temperature pump (2), the filter (3) filters the materials and then conveys the materials to the ultrafilter (4), and the ultrafilter (4) concentrates the filtered materials and then conveys the concentrated materials to the reaction kettle (1).

2. The colloidal silica production apparatus as set forth in claim 1, wherein said jacket is provided with a steam inlet (10) for circulating the introduced steam and a steam condensate outlet (11) for circulating the discharged steam, and said jacket is further provided with a cooling water inlet (12) for circulating the introduced cooling water and a cooling water outlet (13) for circulating the discharged cooling water.

3. The colloidal silica preparation device according to claim 1, wherein the top of the reaction kettle (1) is provided with a feed inlet (5), a feed back port (6) and an exhaust port (7), and the reaction kettle (1) is connected with the ultrafilter (4) through the feed back port (6); the bottom of the reaction kettle (1) is provided with a discharge port (8) and a feeding port (9), and the reaction kettle (1) is connected with the high-temperature pump (2) through the feeding port (9).

4. The colloidal silica production apparatus according to claim 1, wherein a stirrer (14) is provided inside the reaction vessel (1).

5. The colloidal silica production apparatus according to claim 1, wherein the reaction vessel (1) is an enamel reaction vessel or a stainless steel reaction vessel.

6. Colloidal silica preparation plant according to claim 1, characterized in that said filter (3) is provided with a drain (15).

7. Colloidal silica production plant according to claim 1, characterized in that said filter (3) is a belt filter.

8. Colloidal silica production plant according to claim 1, characterized in that said ultrafilter (4) is provided with a concentrate return outlet (16) and a permeate discharge (17), said ultrafilter (4) being connected to said reaction vessel (1) through said concentrate return outlet (16).

9. The colloidal silica production apparatus according to claim 1, wherein the ultrafilter (4) comprises a membrane housing and an ultrafiltration membrane module, and the ultrafiltration membrane module is a hollow fiber type membrane or a tubular type membrane.

10. The colloidal silica production apparatus according to claim 1, wherein the reaction vessel (1), the high-temperature pump (2), the filter (3) and the ultrafilter (4) are integrated.

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