CN112705142A - Continuous flow silica sol synthesis device and synthesis method - Google Patents
Continuous flow silica sol synthesis device and synthesis method Download PDFInfo
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- CN112705142A CN112705142A CN202011534910.XA CN202011534910A CN112705142A CN 112705142 A CN112705142 A CN 112705142A CN 202011534910 A CN202011534910 A CN 202011534910A CN 112705142 A CN112705142 A CN 112705142A
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- pump
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- reaction kettle
- preheater
- silica sol
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
- B01J19/1881—Stationary reactors having moving elements inside resulting in a loop-type movement externally, i.e. the mixture leaving the vessel and subsequently re-entering it
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
- C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
- C01B33/1485—Stabilisation, e.g. prevention of gelling; Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a flow continuous silica sol synthesis device and a synthesis method. The running water continuous silicasol synthesis device comprises a reaction kettle, a spray pipe, an alkaline ultrafiltration water tank body, an exhaust valve, a stabilizer tank body, a silicic acid tank body, a first feeding pump, a second feeding pump, a first mixer, a second mixer, a circulating pump, a first lead-out pump, a preheater, a second lead-out pump and a static crystallization tower; the stabilizer box body is connected with the first feeding pump in series, the silicic acid box body is connected with the second feeding pump in series, the first feeding pump and the second feeding pump are connected with the first mixer in parallel, the first mixer is communicated with the reaction kettle through the second mixer, and the reaction kettle is provided with an exhaust valve. The invention can solve the technical problem of how to continuously synthesize the silica sol.
Description
Technical Field
The invention relates to a device for continuously synthesizing silica sol by using flowing water, and also relates to a method for synthesizing silica sol by using the device.
Background
The synthesis of silica sol generally needs alkaline glass water, a stabilizer and silicic acid, the prior synthesis method comprises the steps of mixing the stabilizer and the silicic acid according to a certain proportion, introducing the mixture into a reaction kettle, stirring, introducing the alkaline glass water, keeping static mixing for a period of time, and then carrying out heat exchange and heat preservation on materials in the reaction kettle through a heat exchange rubber sleeve of the reaction kettle, wherein the heat exchange and heat preservation must be kept for a period of time, so that the synthesis of the silica sol of the next batch can be finished only after the heat exchange and heat preservation of the last batch, and continuous production cannot be kept, thereby achieving efficiency.
Disclosure of Invention
The invention aims to provide a running water continuous silica sol synthesis device, which solves the technical problem of how to continuously synthesize silica sol.
Another object of the present invention is to provide a process for synthesizing silica sol by continuous flow.
The running water continuous silicasol synthesis device comprises a reaction kettle, a spray pipe, an alkaline ultrafiltration water tank body, an exhaust valve, a stabilizer tank body, a silicic acid tank body, a first feeding pump, a second feeding pump, a first mixer, a second mixer, a circulating pump, a first lead-out pump, a multi-stage preheater, a second lead-out pump, a static crystallization tower and a heat source; the stabilizer box body is connected with a first feeding pump in series, the silicic acid box body is connected with a second feeding pump in series, the first feeding pump and the second feeding pump are connected with a first mixer in parallel, the first mixer is communicated with a reaction kettle through a second mixer, an exhaust valve is arranged on the reaction kettle, and the alkaline ultrafiltration water box body is communicated with the reaction kettle through a spray pipe; the second mixer, the circulating pump and the reaction kettle jointly form material circulation, a branch is arranged between the second mixer and a pipeline of the circulating pump, the branch is communicated with the multi-stage preheater through the first export pump, preheaters in the multi-stage preheater are communicated with each other, and the multi-stage preheater is communicated with a material inlet of the static crystallization tower through the second export pump; the material outlet of the static crystallization tower is communicated with part of preheaters in the multi-stage preheater; the spray pipes are arranged at the top inside the reaction kettle, the static crystallization tower is in a multi-stage series connection design, each stage is arranged in a longitudinal mode, and the heat source is communicated with part of preheaters in the multi-stage preheaters.
And a sight glass is also arranged between the circulating pump and the reaction kettle.
The first mixer and the second mixer are plastic three-way valves.
The continuous flow silica sol synthesizing process includes the following steps:
a. respectively feeding the stabilizer and the silicic acid into a first mixer through a first feeding pump and a second feeding pump, and then introducing the stabilizer and the silicic acid into a reaction kettle through a second mixer;
b. introducing alkaline ultrafiltration water into a reaction kettle through a spray pipe and stirring;
c. starting a circulating pump to continuously and circularly mix the stabilizer, the silicic acid and the alkaline ultrafiltration water in the reaction kettle for uniform reaction to form a mixed solution;
d. leading the mixed liquid into a preheater through a first leading-out pump;
e. the heat source heats the mixed liquid initially entering a part of preheaters to meet the crystallization temperature requirement, and the mixed liquid after heat exchange is guided into the static crystallization tower through the second guide-out pump for crystallization;
f. the crystallized mixed liquid flows back to a part of the preheater to preheat the mixed liquid which just enters the preheater subsequently, and the heat source supplements heat for the preheated mixed liquid in the subsequent preheater, so that the crystallization temperature requirement of the crystallized mixed liquid entering the static crystallization tower is met;
g. and continuously and repeatedly introducing the next batch of the stabilizer, the silicic acid and the alkaline ultrafiltration water into the reaction kettle for reaction according to the mode.
The flow rate of the stabilizer is 80-90L/h.
The flow rate of the silicic acid is 3-5 square meters per hour.
The induced flow wave of the circulating pump is 25-30 square meters per hour.
The invention has the beneficial effects that: because the static crystallization tower and the preheater are additionally arranged, the mixed liquid in the reaction kettle can be introduced into the static crystallization tower to wait for crystallization without being in the reaction kettle, so that when the mixed liquid in the static crystallization tower of the previous batch is in a crystallization state, the material of the next batch can be introduced into the reaction kettle, and the materials of the upper batch and the lower batch cannot interfere with each other, thereby achieving the effect of continuous reaction synthesis by flowing water; and adopt the vertical tower column structure of static crystallization tower, the material in each tower avoids mutual interference, is favorable to the formation of crystallization like this.
Drawings
FIG. 1 is a schematic illustration of the mixing of the mixed liquor prior to introduction into the preheater and static crystallization column;
FIG. 2 is a schematic diagram of the crystallization of the mixed liquor through a preheater and a static crystallization column;
in the figure, 1, a reaction kettle, 2, a spray pipe, 3, an alkaline ultrafiltration water tank body, 4, an exhaust valve, 5, a stabilizer tank body, 6, a silicic acid tank body, 7, a first feeding pump, 8, a second feeding pump, 9, a first mixer, 10, a second mixer, 11, a circulating pump, 12, a first export pump, 13, a preheater, 14, a second export pump, 15, a static crystallization tower and 16, a heat source are arranged.
Detailed Description
Referring to fig. 1 and 2, the continuous flowing-water silica sol synthesizing apparatus in the figure includes a reaction kettle 1, a spray pipe 2, an alkaline ultrafiltration water tank 3, an exhaust valve 4, a stabilizer tank 5, a silicic acid tank 6, a first feed pump 7, a second feed pump 8, a first mixer 9, a second mixer 10, a circulating pump 11, a first lead-out pump 12, a preheater group composed of a plurality of preheaters 13, a second lead-out pump 14, a static crystallization tower 15, and a heat source 16 for supplementing heat. The reaction kettle 1 is used for mixing and stirring the three materials. The spray pipe 2 is used for guiding the alkaline ultrafiltration water in the alkaline ultrafiltration water tank body 3 into the reaction kettle 1 to increase the contact area with other two materials. The vent valve 4 is used for discharging the rest of the reaction kettle 1. The stabilizer tank 5, the first feed pump 7, the first mixer 9, and the second mixer 10 are used to introduce the stabilizer into the reaction vessel 1. The silicic acid tank 6, the second feed pump 8, the first mixer 9, and the second mixer 10 are used to introduce silicic acid into the reaction vessel 1. The circulating pump 11 is used for continuously circulating the three materials in the reaction kettle 1 so as to complete uniform mixing reaction. The first lead-out pump 12 is used to introduce the recycled mixed material into the preheater 13.
The partial preheaters 13 in the preheater group firstly directly heat the mixed liquid just entering the preheater 13 to the temperature meeting the crystallization requirement through the heat source 16, such as directly heating from 10 ℃ to 90 ℃. After crystallization, because the mixture with crystals needs heat dissipation and cooling, the mixed liquid entering the preheater 13 subsequently is preheated by using the heat dissipation, so that the crystallization requirement can be met only by using partial heat in the last preheater 13, for example, the mixed liquid entering subsequently at 10 degrees is preheated to 80 degrees by using 90-degree crystallization heat, and then the heat is supplemented to 90 degrees from 80 degrees without directly heating 10 degrees to 90 degrees by using a heat source, so that the heat of crystallization can be fully utilized, and the utilization of heat energy is reduced. The preheater 13 is used for performing heat exchange operations such as preheating and heat compensation on the mixed liquid. The second discharge pump 14 is used to introduce the mixed liquid in the preheater 13 into the static crystallization tower 15. The static crystallization tower 15 is used for static crystallization of the mixed liquid. The components are all the existing components, and the innovation of the scheme is to innovatively combine the components.
The reaction kettle 1 adopts a conventional reaction kettle 1 structure, an exhaust valve 4 is arranged on the reaction kettle 1, and a spray pipe 2 is arranged at the top of the reaction kettle; with this arrangement, the alkaline ultrafiltrate can be introduced into the reaction vessel 1.
The stabilizer box body 5 is connected with a first feeding pump 7 in series, the silicic acid box body 6 is connected with a second feeding pump 8 in series, the first feeding pump 7 and the second feeding pump 8 are connected with a first mixer 9 in parallel, and the first mixer 9 is communicated with the reaction kettle 1 through a second mixer 10; with this arrangement, the stabilizer and the silicic acid can be introduced into the reaction tank 1.
The second mixer 10, the circulating pump 11 and the reaction kettle 1 form material circulation together; thus realizing the mixing reaction of the three materials.
A branch is provided between the second mixer 10 and the pipe of the circulation pump 11, the branch is communicated with a preheater 13 through a first lead-out pump 12, and the preheater 13 is communicated with a static crystallization tower 15 through a second lead-out pump 14; the mixed liquid is thus crystallized in the static crystallization tower 15.
Above-mentioned static crystallization tower 15 becomes the multistage design of concatenating, and every grade is arranged from vertical mode, can play fine like this with whole mixed liquid mutual isolation effect, be favorable to the formation of crystallization. A sight glass is also arranged between the circulating pump 11 and the reaction kettle 1, so that the reaction condition can be observed conveniently. The first mixer 9 and the second mixer 10 are plastic three-way valves, which avoid corrosion.
The flow-continuous silica sol synthesis method comprises the following steps:
a. the stabilizer in the stabilizer box body 5 and the silicic acid in the silicic acid box body 6 are respectively fed into a first mixer 9 through a first feeding pump 7 and a second feeding pump 8, and then are introduced into the reaction kettle 1 through a second mixer 10; the flow rate of the stabilizer is 80-90L/h; the flow rate of the silicic acid is 3-5 square meters per hour;
b. leading alkaline ultrafiltration water in an alkaline ultrafiltration water tank body 3 into a reaction kettle 1 through a spray pipe 2 and stirring; the flow rate of the alkaline ultrafiltration water can be determined according to the needs;
c. starting a circulating pump 11 to continuously circulate, mix and react the stabilizer, the silicic acid and the alkaline ultrafiltration water in the reaction kettle 1 uniformly to form a mixed solution; the induced flow wave of the circulating pump 11 is 25-30 square meters per hour;
d. introducing the mixed liquid into the preheater 13 through the first discharge pump 12;
e. the heat source 16 directly heats and exchanges heat with part of the preheater 13; introducing the mixed solution after heat exchange into a static crystallization tower 15 through a second lead-out pump 14 for crystallization;
f. the crystallized mixed liquor flows back to a part of the preheater 13 to preheat the mixed liquor which just enters the preheater 13 subsequently, and the heat source 16 supplements heat to the preheated mixed liquor in the subsequent preheater 13, so that the crystallization temperature requirement of the crystallized mixed liquor entering the static crystallization tower 15 is met;
g. and continuously and repeatedly introducing the next batch of the stabilizer, the silicic acid and the alkaline ultrafiltration water into the reaction kettle for reaction according to the mode.
In order to make the purpose, technical solution and advantages of the present invention more apparent, the following detailed description of the present invention is provided with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present disclosure and are not intended to limit the present disclosure.
In the description of the present technical solution, it should be noted that the terms such as "above" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, which is only for convenience of describing the technical solution and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation and operate, and thus, should not be construed as limiting the technical solution. Furthermore, the terms "first" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. The number of each part of the scheme can be adaptively changed according to the requirement.
Although embodiments of the present technical solution have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the technical solution, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The running water serialization silica sol synthesizer is characterized in that: the device comprises a reaction kettle, a spray pipe, an alkaline ultrafiltration water tank body, an exhaust valve, a stabilizer tank body, a silicic acid tank body, a first feed pump, a second feed pump, a first mixer, a second mixer, a circulating pump, a first lead-out pump, a multi-stage preheater, a second lead-out pump, a static crystallization tower and a heat source; the stabilizer box body is connected with a first feeding pump in series, the silicic acid box body is connected with a second feeding pump in series, the first feeding pump and the second feeding pump are connected with a first mixer in parallel, the first mixer is communicated with a reaction kettle through a second mixer, an exhaust valve is arranged on the reaction kettle, and the alkaline ultrafiltration water box body is communicated with the reaction kettle through a spray pipe; the second mixer, the circulating pump and the reaction kettle jointly form material circulation, a branch is arranged between the second mixer and a pipeline of the circulating pump, the branch is communicated with the multi-stage preheater through the first export pump, preheaters in the multi-stage preheater are communicated with each other, and the multi-stage preheater is communicated with a material inlet of the static crystallization tower through the second export pump; the material outlet of the static crystallization tower is communicated with part of preheaters in the multi-stage preheater; the spray pipes are arranged at the top inside the reaction kettle, the static crystallization tower is in a multi-stage series connection design, each stage is arranged in a longitudinal mode, and the heat source is communicated with part of preheaters in the multi-stage preheaters.
2. The in-line continuous silica sol synthesizing apparatus according to claim 1, wherein: and a sight glass is also arranged between the circulating pump and the reaction kettle.
3. The in-line continuous silica sol synthesizing apparatus according to claim 1, wherein: the first mixer and the second mixer are plastic three-way valves.
4. A method for continuous flow-through silica sol synthesis using the continuous flow-through silica sol synthesis apparatus according to claim 1, characterized in that: the method comprises the following steps:
a. respectively feeding the stabilizer and the silicic acid into a first mixer through a first feeding pump and a second feeding pump, and then introducing the stabilizer and the silicic acid into a reaction kettle through a second mixer;
b. introducing alkaline ultrafiltration water into a reaction kettle through a spray pipe and stirring;
c. starting a circulating pump to continuously and circularly mix the stabilizer, the silicic acid and the alkaline ultrafiltration water in the reaction kettle for uniform reaction to form a mixed solution;
d. leading the mixed liquid into a preheater through a first leading-out pump;
e. the heat source heats the mixed liquid initially entering a part of preheaters to meet the crystallization temperature requirement, and the mixed liquid after heat exchange is guided into the static crystallization tower through the second guide-out pump for crystallization;
f. the crystallized mixed liquid flows back to a part of the preheater to preheat the mixed liquid which just enters the preheater subsequently, and the heat source supplements heat for the preheated mixed liquid in the subsequent preheater, so that the crystallization temperature requirement of the crystallized mixed liquid entering the static crystallization tower is met;
g. and continuously and repeatedly introducing the next batch of the stabilizer, the silicic acid and the alkaline ultrafiltration water into the reaction kettle for reaction according to the mode.
5. The method for synthesizing an in-line continuous silica sol according to claim 4, wherein: the flow rate of the stabilizer is 80-90L/h.
6. The method for synthesizing an in-line continuous silica sol according to claim 4, wherein: the flow rate of the silicic acid is 3-5 square meters per hour.
7. The method for synthesizing an in-line continuous silica sol according to claim 4, wherein: the induced flow wave of the circulating pump is 25-30 square meters per hour.
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| CN202011534910.XA CN112705142B (en) | 2020-12-22 | 2020-12-22 | Continuous flow silica sol synthesis device and synthesis method |
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| CN202011534910.XA CN112705142B (en) | 2020-12-22 | 2020-12-22 | Continuous flow silica sol synthesis device and synthesis method |
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| CN112705142A true CN112705142A (en) | 2021-04-27 |
| CN112705142B CN112705142B (en) | 2022-04-01 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3756958A (en) * | 1972-04-12 | 1973-09-04 | Du Pont | Process for increasing size of silica particles in aqueous silica sol |
| CN101306260A (en) * | 2007-07-12 | 2008-11-19 | 项公浩 | Multifunctional multiple-effect automatic continuous evaporative crystallization technique and crystallization device |
| US20090239288A1 (en) * | 2008-03-19 | 2009-09-24 | Gas Technology Institute | Integrated membrane separation - bioreactor for selective removal of organic products and by-products |
| CN104071761A (en) * | 2014-05-12 | 2014-10-01 | 江苏大明科技有限公司 | Continuous crystallizing and centrifuging system for producing phosphorous acid |
| CN104829153A (en) * | 2015-05-08 | 2015-08-12 | 郑祖兰 | Production system of naphthalene series industrial water reducer |
| WO2018040852A1 (en) * | 2016-08-30 | 2018-03-08 | 成都锐思环保技术股份有限公司 | System and method for treating desulfurization wastewater using flue gas waste heat |
| CN209039068U (en) * | 2018-10-16 | 2019-06-28 | 枝江市富成化工有限责任公司 | Silica solution production system |
-
2020
- 2020-12-22 CN CN202011534910.XA patent/CN112705142B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3756958A (en) * | 1972-04-12 | 1973-09-04 | Du Pont | Process for increasing size of silica particles in aqueous silica sol |
| CN101306260A (en) * | 2007-07-12 | 2008-11-19 | 项公浩 | Multifunctional multiple-effect automatic continuous evaporative crystallization technique and crystallization device |
| US20090239288A1 (en) * | 2008-03-19 | 2009-09-24 | Gas Technology Institute | Integrated membrane separation - bioreactor for selective removal of organic products and by-products |
| CN104071761A (en) * | 2014-05-12 | 2014-10-01 | 江苏大明科技有限公司 | Continuous crystallizing and centrifuging system for producing phosphorous acid |
| CN104829153A (en) * | 2015-05-08 | 2015-08-12 | 郑祖兰 | Production system of naphthalene series industrial water reducer |
| WO2018040852A1 (en) * | 2016-08-30 | 2018-03-08 | 成都锐思环保技术股份有限公司 | System and method for treating desulfurization wastewater using flue gas waste heat |
| CN209039068U (en) * | 2018-10-16 | 2019-06-28 | 枝江市富成化工有限责任公司 | Silica solution production system |
Non-Patent Citations (1)
| Title |
|---|
| 范渊卿等: "大粒径高浓度硅溶胶的制备及其应用", 《辽宁化工》 * |
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