CN116459784A - Novel macroporous silica gel reaming manufacturing method based on cyclic utilization of reaming agent - Google Patents
Novel macroporous silica gel reaming manufacturing method based on cyclic utilization of reaming agent Download PDFInfo
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- CN116459784A CN116459784A CN202310437526.5A CN202310437526A CN116459784A CN 116459784 A CN116459784 A CN 116459784A CN 202310437526 A CN202310437526 A CN 202310437526A CN 116459784 A CN116459784 A CN 116459784A
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
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Abstract
The invention provides a novel reaming manufacturing method of macroporous silica gel based on cyclic utilization of a reaming agent, and belongs to the technical field of production and preparation of massive silica gel. The invention is based on reaction materials prepared by using dilute sulfuric acid with the concentration of 20-25% and sodium silicate with the concentration of 25-30% and the sodium silicate modulus of 3.2-3.4 at 15-20 ℃, and is prepared by aging, reaming, rubber cutting, water washing, secondary reaming by using ammonia water, then rubber dragging, multistage drying, obtaining silica gel with the moisture less than or equal to 5%, and finally screening, separating and automatic packaging. The method is specially used for the low-temperature gel preparation process, and the prepared macroporous silica gel has stable pore volume and pore diameter and high purity of silica; the invention solves the problems of low automation level, high labor intensity, poor working environment, difficult scale production or low production efficiency and the like in the macroporous silica gel production process in the prior art; the invention has low production cost, is economical and environment-friendly, is easy to realize large-scale industrialized production, and has good popularization significance.
Description
The application is a divisional application of patent application named 'a novel reaming manufacturing method of macroporous silica gel', the application date of the original application is 2020, 12 months and 08 days, and the application number is 202011442499.3.
Technical Field
The invention belongs to the technical field of production and preparation of massive silica gel, and particularly relates to a novel reaming manufacturing method of macroporous silica gel based on cyclic utilization of a reaming agent.
Background
Silica gel alias: silicic acid gel is a high-activity adsorption material, and belongs to amorphous substances. Silica gel is mainly composed of silicon dioxide, has stable chemical property and is not burnt.
The existing macroporous silica gel production process has the characteristics of low automation level, high labor intensity, poor working environment, difficult scale or low production efficiency, higher production cost, lower pore volume of the product, low controllability of product performance index, larger unexpected technological change influence and the like. And the environmental protection treatment cost of the production line is high, and the scale benefit is difficult to realize. The production reaming of macroporous silica gel adopts steam or high-temperature hot water reaming or salt leaching reaming, and the product has the defects of low yield of main products, large crushing, more powder, low product strength, low catalytic activity and the like. And the organic silicon and the organic pore-expanding agent are adopted as raw materials to produce the macroporous silica gel, so that the production cost of the product is high, the process control is complex, and the like.
The glue making temperature is an important factor affecting the silica gel product, but the existing reaming technology is generally aimed at the glue making process above 30 ℃, and no efficient reaming scheme specially aimed at the low-temperature glue making process of 15-20 ℃ exists at present.
Disclosure of Invention
One of the technical problems to be solved by the invention is as follows: the existing macroporous silica gel production flow in the prior art has the characteristics of low automation level, high labor intensity, poor working environment, difficult scale or low production efficiency, higher production cost, low pore volume of the product, low controllability of product performance index, larger influence of unexpected process change and the like. And the environmental protection treatment cost of the production line is high, and the scale benefit is difficult to realize. The production reaming of macroporous silica gel adopts steam or high-temperature hot water reaming or salt leaching reaming, and the product has the defects of low yield of main products, large crushing, more powder, low product strength, low catalytic activity and the like. And the organic silicon and the organic pore-expanding agent are adopted as raw materials to produce the macroporous silica gel, so that the production cost of the product is high, the process control is complex, and the like.
In order to solve the technical problem, the invention provides a novel reaming manufacturing method of macroporous silica gel, the manufacturing method comprises the steps of ageing reaction materials obtained by preparing gel at a low temperature in an ageing tank for the first time to obtain ageing materials, carrying out rubber cutting and crushing on the ageing materials by adopting low-crushing equipment to obtain rubber cutting materials, washing sodium sulfate, sulfuric acid and metal ion impurities generated in the gel preparation reaction process by adopting spray condensate countercurrent water washing in a serial water washing tank, carrying out serial washing by taking the next water washing tank as an initial water washing tank after serial washing in the initial water washing tank, then preparing a reaming agent with certain concentration and temperature by adopting a rubber fishing backwater for secondary reaming, and conveying the obtained product to a multilayer mesh belt steam drying equipment by adopting an automatic rubber fishing machine after reaming is finished to obtain low-moisture massive silica gel for screening separation, thus obtaining macroporous massive silica gel with different granularity.
The second technical problem to be solved by the invention is as follows: the glue making temperature is an important factor affecting the silica gel product, but the existing reaming technology is generally aimed at the glue making process above 30 ℃, and no efficient reaming scheme specially aimed at the low-temperature glue making process of 15-20 ℃ exists at present.
In order to solve the technical problem, the invention provides a novel reaming manufacturing method of macroporous silica gel based on cyclic utilization of a reaming agent, which comprises the steps of firstly using dilute sulfuric acid with concentration of 20-25% and sodium silicate with concentration of 25-30% and sodium silicate modulus of 3.2-3.4 at 15-20 ℃ to prepare a reaction material at low temperature, and then using the method, and strictly setting preparation parameters at the same time, so that the pore volume and pore diameter of the macroporous silica gel prepared by the low-temperature reaming process are stable, and the purity of silicon dioxide is high.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a novel macroporous silica gel reaming manufacturing method based on cyclic utilization of a reaming agent, which comprises the following steps:
(1) And (3) glue preparation at low temperature: preparing a reaction material by using dilute sulfuric acid with the concentration of 20-25% and sodium silicate with the concentration of 25-30% and the sodium silicate modulus of 3.2-3.4 at the temperature of 15-20 ℃; (2) aging reaming: aging the reaction material obtained by the reaction for 30-40 hours to perform primary reaming; (3) tapping; (4) countercurrent water washing: circulating gradient serial washing is adopted, the number of serial washing tanks is 6-9, and the temperature of hot water is 50-60 ℃; (5) secondary reaming of a reaming agent: performing secondary reaming by using ammonia water or ammonium bicarbonate or ammonium carbonate with mass concentration of 0.1-0.3% and temperature of 65-75 ℃ as a reaming agent for 6-10 h; (6) fishing out the glue; (7) drying: adopting a multi-layer mesh belt steam drying device, wherein the temperature of a first layer of mesh belt is set to be 100-140 ℃, the temperature of a second layer of mesh belt is set to be 140-160 ℃, and the temperature of a third layer of mesh belt is set to be 100-160 ℃ to obtain silica gel with the moisture less than or equal to 5%; (8) screening, separating and automatically packaging; the novel reaming manufacturing method of the macroporous silica gel is specially used for a low-temperature gel manufacturing process, and the prepared macroporous silica gel has stable pore volume and pore diameter and high purity of silica.
Preferably, the raw material pumps of the dilute sulfuric acid and the sodium silicate are automatically started, the temperature of the dilute sulfuric acid and the sodium silicate is controlled at 20 ℃, so that stable low-temperature gel preparation reaction is realized, the concentration of the dilute sulfuric acid is 18%, and the concentration of the sodium silicate is 26%.
Preferably, the low-temperature glue making reaction material enters a track type or chain type ageing tank, the ageing tank is automatically driven by a motor, the rotating speed frequency of the motor is controlled, the low-temperature glue making reaction material is automatically received, and the ageing material is obtained after the ageing time of the reaction material in the ageing tank is 36 hours.
Preferably, the aged material adopts low-crushing equipment to cut rubber through controlling the rotating speed of a motor in a variable frequency manner to obtain rubber cutting materials, the rubber cutting water is from spraying hot water, and the damaged equipment adopts a saw-tooth type or double-roller type rotating wheel.
Preferably, the countercurrent water washing hot water is from hot water obtained by spraying the drying tail gas, and the temperature of the hot water is 55 ℃.
Preferably, ammonia water with the mass concentration of 0.15% and the temperature of 70 ℃ is adopted for secondary reaming, the reaming time is 6 hours, and the reaming agent is recycled.
Preferably, the glue dragging machine is provided with a filter screen, glue dragging and binding the filter screen is used for dragging the hot water containing the pore-expanding agent through plate and frame filtration.
Preferably, the steam pressure of the drying equipment is 0.55-0.65 MPa, and the steam condensate is recycled.
Preferably, the drying tail gas generated by the drying equipment adopts a multi-layer tower plate type high-efficiency spray tower to recycle condensed water, and the high-efficiency spray tower is provided with circulating spray to improve waste heat recycling efficiency, recycle hot water and a pore-enlarging agent, and achieve high-efficiency dust removal.
Preferably, the screening device used for screening and separating is a linear vibrating screen.
Preferably, the automatic packaging equipment of the silica gel comprises automatic weighing, automatic bag sewing and automatic stacking.
Compared with the prior art, the invention has the beneficial effects that:
1. the automatic production line has simple process flow and is easy to industrially popularize.
2. And (3) recycling the pore-expanding agent, and stably expanding the pores step by step.
3. The product quality is controllable, the waste heat is comprehensively utilized, and the production cost is low.
4. The screening equipment used for screening and separating is a linear vibrating screen, has the characteristics of small damage and small abrasion, and obtains products with uniform granularity and high granularity qualification rate through multistage screening.
5. Is specially used for low-temperature glue making process.
The macroporous massive silica gel produced by the invention has the characteristics of uniform product granularity, stable pore volume and aperture and high purity of silicon dioxide, is low in production cost, economical and environment-friendly, is easy to realize large-scale industrialized production, and has good popularization significance.
Drawings
FIG. 1 is a flow chart of a silica gel manufacturing process in the invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples.
In the description of the present invention, it should be understood that the terms "longitudinal," "transverse," "vertical," "horizontal," "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present invention.
Referring to fig. 1, a novel reaming manufacturing method of macroporous silica gel is disclosed, the manufacturing method uses dilute sulfuric acid and sodium silicate as raw materials to prepare rubber at low temperature to obtain a reaction material, the reaction material is aged in an ageing tank for the first reaming to obtain an ageing material, rubber cutting and crushing are carried out on the ageing material by adopting low-crushing equipment to obtain a rubber cutting material, the rubber cutting material enters a cross washing water tank to wash sodium sulfate, sulfuric acid and metal ion impurities generated in the rubber preparation reaction process by adopting spray condensate countercurrent water washing, the next water washing tank is used as the initial water washing tank to carry out cross washing after the end of the cross washing of the initial water washing tank, the silica gel in the cross washing tank is then subjected to secondary reaming by adopting a reaming agent with certain concentration and temperature prepared by adopting a rubber fishing backwater, and after the reaming is finished, the silica gel is conveyed to a multilayer mesh belt steam drying equipment by an automatic rubber fishing machine to obtain low-moisture massive silica gel, and the massive silica gel with different granularity specifications is obtained.
In order to better manufacture silica gel, the invention also comprises the steps of automatically starting the raw material pumps of the dilute sulfuric acid and the sodium silicate, wherein the temperature of the dilute sulfuric acid and the sodium silicate is controlled at 15-20 ℃ so as to realize stable low-temperature gel manufacturing reaction, the concentration of the dilute sulfuric acid is 20-25%, the concentration of the sodium silicate is 25-30%, and the modulus of the sodium silicate is 3.2-3.4. The low-temperature glue making reaction material enters a track type or chain type ageing tank, the ageing tank is automatically driven by a motor, the rotating speed and frequency of the motor are controlled, the low-temperature glue making reaction material is automatically received, and the ageing time of the reaction material in the ageing tank is 30-40 hours, so that the ageing material is obtained. The aged material adopts low-crushing equipment to cut rubber through controlling the rotating speed of a motor in a variable frequency manner to obtain rubber cutting material, the rubber cutting water is from spraying hot water, and the damaged equipment adopts a saw-tooth type or double-roller type rotating wheel. The countercurrent washing hot water is from hot water obtained by spraying the drying tail gas, the countercurrent washing tanks are subjected to circulating gradient serial washing, the number of the serial washing tanks is 6-9, and the temperature of the hot water is 50-60 ℃. The inorganic matter of the pore-expanding agent is ammonia water or ammonium bicarbonate or ammonium carbonate, the mass concentration is 0.1-0.3%, the temperature of the pore-expanding agent is 65-75 ℃, the pore-expanding time is 6-10 h, and the pore-expanding agent is recycled. The glue dragging machine is provided with a filter screen, glue dragging and binding are performed on glue dragging of the filter screen, hot water containing a pore-enlarging agent is obtained through plate frame filtration, and the hot water is reused for pore-enlarging. The drying equipment is continuous multilayer mesh belt steam drying equipment, the drying temperature is 100-160 ℃, the steam pressure is 0.55-0.65 MPa, and the steam condensate water is recycled. The drying tail gas produced by the drying equipment adopts a multi-layer tower plate type efficient spray tower to recycle condensed water, the efficient spray tower is provided with a linear vibrating screen for circularly spraying, so that the waste heat recycling efficiency is improved, hot water and a pore-enlarging agent are recycled, and the screening equipment for high-efficiency dust removal, screening and separation is achieved. The packaging equipment of silica gel contains automatic weighing, automatic package sewing, automatic pile up neatly.
Example 1
Preparing dilute sulfuric acid with the mass concentration of 18% at the temperature of 20 ℃ and sodium silicate with the mass concentration of 26% at the preparation temperature of 20 ℃, carrying out low-temperature glue making reaction to a chain type ageing tank, standing and ageing the reaction material in the ageing tank for 36h to carry out primary reaming, then adopting a roll type crushing device to carry out rubber cutting, adopting hot water countercurrent washing with spray condensation at the temperature of 55 ℃, adopting circulating gradient serial washing of water washing tanks, serial washing the number of the serial washing tanks for 6-9, then adopting glue fishing backwater and steam condensate water to prepare 0.15% mass concentration, and carrying out secondary reaming with ammonia water at the temperature of 70 ℃ for 6h, after reaming, conveying the materials to a multi-layer mesh belt steam drying device through an automatic glue fishing machine, setting the temperature of the first layer mesh belt to be 100-140 ℃, setting the temperature of the second layer mesh belt to be 140-160 ℃, setting the temperature of the third layer mesh belt device to be 100-160 ℃ to obtain silica gel with the moisture content of less than or equal to 5%, and finally screening, automatically packaging to obtain the macroporous silica gel with the granularity of 4-8mm, 1-6mm, 0.5-2 mm and powder.
The examples described above only represent preferred embodiments of the present invention, which are described in more detail, but the present invention is not limited to these examples, and it should be noted that it is obvious to those skilled in the art that the present invention is not limited to these examples. Any modifications thereof fall within the scope of the present invention without departing from the spirit of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (9)
1. The novel macroporous silica gel reaming manufacturing method based on recycling of reaming agents is characterized by comprising the following steps of:
(1) And (3) glue preparation at low temperature: preparing a reaction material by using dilute sulfuric acid with the concentration of 20-25% and sodium silicate with the concentration of 25-30% and the sodium silicate modulus of 3.2-3.4 at the temperature of 15-20 ℃;
(2) Aging and reaming: aging the reaction material obtained by the reaction for 30-40 hours to perform primary reaming;
(3) Rubber tapping;
(4) Countercurrent water washing: circulating gradient serial washing is adopted, the number of serial washing tanks is 6-9, and the temperature of hot water is 50-60 ℃;
(5) Secondary reaming with a pore-enlarging agent: performing secondary reaming by using ammonia water or ammonium bicarbonate or ammonium carbonate with mass concentration of 0.1-0.3% and temperature of 65-75 ℃ as a reaming agent for 6-10 h;
(6) Fishing out glue;
(7) And (3) drying: adopting a multi-layer mesh belt steam drying device, wherein the temperature of a first layer of mesh belt is set to be 100-140 ℃, the temperature of a second layer of mesh belt is set to be 140-160 ℃, and the temperature of a third layer of mesh belt is set to be 100-160 ℃ to obtain silica gel with the moisture less than or equal to 5%;
(8) Screening, separating and automatically packaging;
the novel reaming manufacturing method of the macroporous silica gel is specially used for a low-temperature gel manufacturing process, and the prepared macroporous silica gel has stable pore volume and pore diameter and high purity of silica.
2. The method for producing a novel pore-enlarging silica gel according to claim 1, wherein the temperature condition in the step (1) is 20 ℃, the concentration of dilute sulfuric acid is 18%, and the concentration of sodium silicate is 26%.
3. The method for manufacturing a new type of macroporous silica gel according to claim 2, wherein the aging time in the step (2) is 36h.
4. The method for manufacturing the novel reaming of the macroporous silica gel according to claim 3, wherein the specific process of the step (3) is as follows: and (3) cutting rubber materials from the aged materials in the step (2) by adopting low-crushing equipment and controlling the rotating speed of a motor through frequency conversion, wherein the rubber cutting water is from spraying hot water, and the damaged equipment adopts a saw-tooth type or double-roller type rotating wheel.
5. The method for manufacturing the novel large pore silica gel reamer of claim 4, wherein the temperature of the hot water in the step (4) is 55 ℃, and the hot water is obtained by spraying the drying tail gas.
6. The method for manufacturing the novel reaming of the macroporous silica gel according to claim 5, wherein ammonia water with the mass concentration of 0.15% and the temperature of 70 ℃ is used in the step (5), the reaming time is 6 hours, and the reaming agent is recycled.
7. The method for manufacturing the novel reaming of the macroporous silica gel according to claim 6, wherein the glue scooping machine used in the step (6) is provided with a filter screen, the glue scooping agent which is used for scooping the binding agent and penetrating the filter screen is filtered through a plate frame to obtain hot water containing the reaming agent for reaming.
8. The method for manufacturing the novel reaming of the macroporous silica gel according to claim 7, wherein the steam pressure of the drying equipment in the step (7) is 0.55-0.65 MPa, and the steam condensate is recycled; the drying tail gas generated by the drying equipment adopts a multi-layer tower plate type high-efficiency spray tower to recycle condensed water, and the high-efficiency spray tower is provided with circulating spray to improve waste heat recovery efficiency, recycle hot water and a pore-enlarging agent, and achieve high-efficiency dust removal.
9. The method for manufacturing the novel large-pore silica gel reaming according to claim 8, wherein the screening device used in the step (8) is a linear vibrating screen, and the automatic packaging device comprises automatic weighing, automatic bag sewing and automatic stacking.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310437526.5A CN116459784A (en) | 2020-12-08 | 2020-12-08 | Novel macroporous silica gel reaming manufacturing method based on cyclic utilization of reaming agent |
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| CN202011442499.3A CN112717874A (en) | 2020-12-08 | 2020-12-08 | Novel reaming manufacturing method of macroporous silica gel |
| CN202310437526.5A CN116459784A (en) | 2020-12-08 | 2020-12-08 | Novel macroporous silica gel reaming manufacturing method based on cyclic utilization of reaming agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3501269A (en) * | 1967-04-20 | 1970-03-17 | Grace W R & Co | Process for preparing silica gel |
| CN1186254C (en) * | 2001-01-11 | 2005-01-26 | 青岛美高集团有限公司 | macroreticular silica gel and its preparing process |
| 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 |
| CN104229810A (en) * | 2013-06-20 | 2014-12-24 | 青岛康威龙日用品有限公司 | Preparation method of coarse-pore blocky silica gel |
| CN105776227A (en) * | 2014-12-13 | 2016-07-20 | 王欣欣 | Production technology of ultra-large-pore adsorptive silica gels |
| CN109292784B (en) * | 2018-10-25 | 2021-10-01 | 青岛美高集团有限公司 | Preparation method of silica gel and silica gel obtained by preparation method |
| CN209735560U (en) * | 2019-03-13 | 2019-12-06 | 青岛创客机械设备制造有限公司 | Full-automatic glue making device |
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