CN104445222B - A kind of big particle diameter and the preparation method of the acidic silicasol that is evenly distributed - Google Patents
A kind of big particle diameter and the preparation method of the acidic silicasol that is evenly distributed Download PDFInfo
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- CN104445222B CN104445222B CN201410704647.2A CN201410704647A CN104445222B CN 104445222 B CN104445222 B CN 104445222B CN 201410704647 A CN201410704647 A CN 201410704647A CN 104445222 B CN104445222 B CN 104445222B
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Abstract
The invention discloses a kind of big particle diameter and the preparation method of the acidic silicasol that is evenly distributed, with technical grade Ludox (SiO2Content 30%) and 80 325 mesh simple substance silica flours as raw material, the mixed ammonium/alkali solutions mixed liquor of ammonia (such as alkali metal hydroxide or the organic base etc. with) is catalyst, uses constant speed charging method to prepare big particle diameter and the acidic silicasol being evenly distributed.Prepared Ludox particle diameter is big, be evenly distributed, viscosity is big, metal oxide content is low.
Description
Technical field
The invention belongs to big particle diameter silica gel preparation field, particularly to a kind of big particle diameter and the acidic silicasol that is evenly distributed
Preparation method.
Background technology
Big particle diameter, the micelle of high-concentration silicon sol have huge specific surface area (the many meso-hole structures in surface) and superpower suction
Attached ability and stronger stability and adhesive property, be widely used in various fields.Such as: by molten for big particle diameter silicon
Glue is as polishing agent for mono-crystalline silicon, the most effective, and polishing velocity is fast.Acidic silicasol can be divided into according to solution ph scope
With alkaline silica sol two kinds.Alkaline silica sol is a kind of stabilising system, and relative alkaline silica sol, acidic silicasol is in metastable shape
State, can gradually occur the gel trend of the acidic silicasol of gelation, especially high concentration to become apparent from placement process,
Become the major influence factors of its application of restriction.Owing to big particle diameter acidic silicasol has good selectivity and reactivity,
The chemically mechanical polishing for electron trade, quasiconductor, hard disk, compound crystal or precision optics can be widely used in.
The Ludox particle diameter of industrial synthesis is generally 10～20nm, and concentration is 30%, it is difficult to meet some special industry to colloid grain
Footpath and the requirement of concentration, and the acidic silicasol of high concentration be in metastable state, can occur in placement process gelling make
With,.How to synthesize particle diameter bigger, concentration is higher, and the more preferable acidic silicasol of stability is to meet commercial Application demand, it has also become
One focus of Ludox research at present.
At present, the conventional preparation technology of industrial manufacture acidic silicasol has following three kinds:
One is to be prepared by ion exchange after waterglass dilutes, the acidic silicasol stability that this method prepares
Difference.If patent US2244325 is with waterglass as raw material, the resting period of prepared acidic silicasol be only several hours and its
Big concentration is 15%, improves storage and cost of transportation；Patent US3867304 is with waterglass as raw material, by repeatedly cation
With the stability that anion exchange is greatly improved gained acidic silicasol, but this method consumes a large amount of water and energy, production cost
Higher.
Another kind of method is to be reacted under the effect of catalyst by silica flour and water to prepare.Such as patent
CN200710119578.9 uses silica flour and water reaction to prepare acidic silicasol, has the feature of high stability and high concentration, but
The particle scale of silicon sol solution prepared by this method is little, it is difficult to meet the requirement to granularity in reality application, such as quasiconductor
Chip polishes special colloidal sol etc..
Also have a kind of with waterglass as raw material, use ion exchange to prepare active silicic acid, by dripping in seed solution
The method adding active silicic acid prepares big particle diameter, single dispersing Ludox, carries out the side of modified with organic acids at silica particles
Method.Prepare active silicic acid as the employing of patent CN102432027A first passes through ion exchange, add it to the waterglass of boiling
In be prepared as even-grained alkaline silica sol, use organic acid to carry out surface modification, make acidity finally by ion exchange
Ludox, the method being concentrated into desired concn.
Other method, as patent TW234579B discloses a kind of pH containing methanol Silica abrasive at 1-6
Liquid, can be used for the polishing of silicon chip；Patent JP6199515 and JP63123807 are by joining silicon dioxide by small amounts aluminum
In colloidal sol, then obtain relatively stable acid silicon dioxide sol through ion-exchange treatment.Said method, due to method itself
Restriction or the impact of raw material, often make that the acidic silicasol existence and stability prepared is poor, particle scale is little, metal ion content
The shortcomings such as height.
Summary of the invention
It is an object of the invention to as overcoming above-mentioned the deficiencies in the prior art, it is provided that a kind of big particle diameter and the acid silicon that is evenly distributed
The preparation method of colloidal sol, can be greatly reduced metal oxide content simultaneously and improve Ludox viscosity, increasing its holding time.
For achieving the above object, the present invention uses following technical proposals:
A kind of big particle diameter and the preparation method of the acidic silicasol that is evenly distributed, comprise the steps:
1) taking the technical grade Ludox that mass concentration is 10%-15%, stir under 300-350r/min, oil bath is heated to
After temperature is 75 DEG C-80 DEG C, adds simple substance silica flour, obtain pretreatment silicon sol solution I；
2) pretreatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropping, continue anti-
Answer 6～8 hours, centrifugation, obtain big particle diameter Ludox I；
3) taking above-mentioned big particle diameter Ludox I, being diluted to mass concentration is 10%-15%, stirs under 300-350r/min
Mixing, oil bath is heated to after temperature is 75 DEG C-80 DEG C, adding simple substance silica flour, obtaining pretreatment silicon sol solution II；
4) pretreatment silicon sol solution II is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropping, continue
React 6～8 hours, centrifugation, obtain big particle diameter Ludox II；
5) big particle diameter Ludox II is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, to obtain final product
Big particle diameter and the acidic silicasol that is evenly distributed；
Wherein, step 1) in, described technical grade Ludox is 70-80:1 with the mass ratio of simple substance silica flour；
Step 2) in, described pretreatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:70-90；
Step 3) in, described big particle diameter silica gel I is 70-80:1 with the mass ratio of simple substance silica flour；
Step 4) in, described pretreatment silicon sol solution II is 80:70-90 with the mass ratio of mixed ammonium/alkali solutions.
The concentration of above-mentioned technical grade Ludox is in the range of 10 15%, it is ensured that in unit volume, silicon dioxide granule is anti-
Should be active moderate, make grain growth speed surely hold in a specific interval, it is ensured that to generate the uniformity of granule.If silicon dioxide is dense
Degree content is too low, owing to the quantity of silicon dioxide granule is the most rare in unit volume, collides and react between particle
The chance occurred is substantially reduced, and the growth rate affecting silica dioxide granule affects the uniformity of its granule；On the other hand, dioxy
SiClx levels is too high, then in course of reaction, the silica concentration of system quickly reaches higher numerical value, system viscosity
Become big earlier, the growth rate of silicon dioxide granule and the stability of Ludox will be affected, the quality of the silica flour added together
It is limited, thus limits the further growth of silicon dioxide granule.
Further, step 1) in, the mesh number of described silica flour is 80-325 mesh, and purity reaches more than 99.9%.By adding
High-purity simple substance silica flour, and amberlite Ester exchange subsequently, eliminate metal cation impurity significantly, it is ensured that
The high-purity of Ludox and stability.
Further, step 2) in, what described mixed ammonium/alkali solutions was ammonia with alkali metal hydroxide or organic base is mixed
Close liquid.
Further, step 2) in, the particle diameter of described big particle diameter Ludox I is 20-30nm.
Preferably, described ammonia is 4～8:1 with the mol ratio of alkali metal hydroxide or organic base.
Ludox prepared by above-mentioned either method, its particle diameter is 50-60nm.
Present invention also offers the preparation method of the acidic silicasol that a kind of particle diameter is 20-30nm, comprise the steps:
1) taking in the technical grade Ludox that concentration is 10%-15%, stir under 300-350r/min, oil bath is heated to temperature
After degree is 75 DEG C-80 DEG C, adds simple substance silica flour, obtain pretreatment silicon sol solution；
2) pretreatment silicon sol solution is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropping, continue anti-
Answer 6～8 hours, centrifugation, obtain big particle diameter silica gel；
3) big particle diameter Ludox is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, obtain grain
Footpath is the acidic silicasol of 20-30nm；
Described silica flour, technical grade Ludox, the mass ratio of mixed ammonium/alkali solutions are 1:80:70-90.
Acidic silicasol prepared by the present invention adds in the solution after medicated beer ferments, and impure ion can be made to generate solidifying
Polymers and be removed so that product is limpid bright.Can also be used for the clarifier of rice wine, soy sauce, fruit juice etc., do not affect product
Color.And silicon is for human non-toxic's evil.When acidic silicasol is on gelled lead acid battery, raw after mixing with sulphuric acid
The colloidal silica become is the ideal not flowing electrolyte of gelled lead acid battery.The leakage that it changes traditional lead acid batteries is sour, dirty
Dye environment, and heavy acid adding, add water and the shortcoming such as maintenance, make extend the service life of accumulator, low-temperature startup performance is good, resistance to
Shake, once irrigates, safe and reliable.Acidic silicasol is applied in static flocking technology, is because acidic silicasol at its fiber
Surface forms silanol group, and makes fiber have hydrophilic, makes flocking hair charging property be improved, and it is the fine hair of electrostatic spinning
The main component of inorganic agent, plays peptizaiton.
Due to the fact that and take above technical scheme, it has the advantage that
1. use mixed ammonium/alkali solutions (alkali metal hydroxide, organic base etc. and the mixed liquor of ammonia) constant speed charging method effective
Control glue nucleus growth, reproducible
2. having synthesized big particle diameter and the acidic silicasol solution being evenly distributed, the present invention prepares 20-30nm, 50-60nm
Acidic silicasol solution etc. even particle size distribution.Overcome that Ludox particle diameter prepared by prior art is pockety asks
Topic.
3. raw material made by present invention silica flour, reduces cost, overcomes existing Ludox preparation method to use waterglass to be raw material,
Cause the problem that complex steps, water consumption are big, cost is high..
4. the acidic silicasol stability that prepared by the present invention is high, and room temperature can be stored more than six months and occur without coagulation and gel
Phenomenon.
5. the acidic silicasol that prepared by the present invention can be used for preparing the floss of clarifier, gelled lead acid battery, electrostatic spinning
Hair inorganic agent.
Accompanying drawing explanation
The acidic silicasol SEM figure of Fig. 1 20-30nm
The acidic silicasol SEM figure of Fig. 2 50-60nm
Detailed description of the invention
Mode by the following examples further illustrates the present invention, but the most therefore limits the present invention to described reality
Execute among example scope.The experimental technique of unreceipted actual conditions in the following example, conventionally selects with condition
Select.
Embodiment 1:
The size of the silicon dioxide involved by embodiments below all uses scanning electron microscope (SEM) to measure,
In Ludox, SiO2 content uses gravimetric detemination, and Ludox viscosity uses constant detection of capillary tube viscosity, metal-oxide
Content uses inductive coupling plasma emission spectrograph to measure, and pH value uses acidometer to measure.The stability of acidic silicasol
Measure according to following method: with salt acid for adjusting pH to 2.5, after stirring, add 0.375g isopropanol, continue stirring, take
State Ludox 6.0g, shake up, put in 60 DEG C of baking ovens, record gel time 163h.
With technical grade Ludox (SiO2Content 30%) and 80 325 mesh simple substance silica flours as raw material, mixed ammonium/alkali solutions (example
Mixed liquor such as alkali metal hydroxide or organic base etc. with ammonia) be catalyst, use constant speed charging method prepare big particle diameter and
The acidic silicasol being evenly distributed.Comprise the following steps that,
1. particle diameter is the preparation of acidic silicasol of 50-60nm, comprises the steps:
1) taking the technical grade Ludox that mass concentration is 12%, stir under 320r/min, it is 80 that oil bath is heated to temperature
After DEG C, add simple substance silica flour, obtain pretreatment silica gel solution I；
2) pretreatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 40mL/h, after dropping, continue reaction 7
Hour, centrifugation, obtain big particle diameter silica gel I；
3) taking above-mentioned big particle diameter silica gel I, being diluted to mass concentration is 12%, stirs under 320r/min, and oil bath is heated
After being 80 DEG C to temperature, add simple substance silica flour, obtain pretreatment silica gel solution II；
4) pretreatment silica gel solution II is added mixed ammonium/alkali solutions with the speed of 40mL/h, after dropping, continue reaction 6
～8 hours, centrifugation, obtain big particle diameter silica gel II；
5) big particle diameter silica gel II is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, obtain greatly
Particle diameter and the acidic silicasol that is evenly distributed (particle diameter is 50-60nm and is evenly distributed)；
Step 1) in, described technical grade Ludox is 80:1 with the mass ratio of simple substance silica flour；
Step 2) in, described pretreatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:80；
Step 3) in, described big particle diameter silica gel I is 80:1 with the mass ratio of simple substance silica flour；
Step 4) in, described pretreatment silicon sol solution II is 80:80 with the mass ratio of mixed ammonium/alkali solutions.
2. particle diameter is the preparation of acidic silicasol of 20-30nm, comprises the steps:
1) taking the technical grade Ludox that concentration is 12%, stir under 320r/min, oil bath is heated to after temperature is 80 DEG C,
Add simple substance silica flour, obtain pretreatment silica gel solution；
2) pretreatment silica gel solution is added mixed ammonium/alkali solutions with the speed of 40mL/h, after dropping, continue reaction 7 little
Time, centrifugation, obtain big particle diameter silica gel；
3) above-mentioned big particle diameter silica gel is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, to obtain final product
Big particle diameter and the acidic silicasol that is evenly distributed (particle diameter is 20-30nm and is evenly distributed)；
Described silica flour, technical grade Ludox, the mass ratio of mixed ammonium/alkali solutions are 1:80:80.
Gained acidic silicasol index is as shown in table 1:
Table 1 acidic silicasol
| Acidic silicasol particle diameter | 20-30nm | 50-60nm |
| SiO2Mass fraction | 40% | 42% |
| Viscosity (20 DEG C) | 5.0mPa.S | 6.5mPa.S |
| Metal oxide content | ＜ 0.13% | ＜ 0.11% |
Embodiment 2
1. particle diameter is the preparation of acidic silicasol of 50-60nm, comprises the steps:
1) taking the technical grade Ludox that mass concentration is 10%, stir under 300r/min, it is 75 that oil bath is heated to temperature
After DEG C, add simple substance silica flour, obtain pretreatment silica gel solution I；Described heating curve is: 0-15min is heated to 60 DEG C, constant temperature
10min, continuing to be heated to temperature is 75 DEG C；
2) pretreatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 20mL/h, after dropping, continue reaction 6
Hour, centrifugation, obtain big particle diameter silica gel I；
3) taking above-mentioned big particle diameter silica gel I, being diluted to mass concentration is 10%, stirs under 300r/min, and oil bath is heated
After being 75 DEG C to temperature, add simple substance silica flour, obtain pretreatment silica gel solution II；
4) pretreatment silica gel solution II is added mixed ammonium/alkali solutions with the speed of 20mL/h, after dropping, continue reaction 6
Hour, centrifugation, obtain big particle diameter silica gel II；
5) big particle diameter silica gel II is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, obtain greatly
Particle diameter and the acidic silicasol that is evenly distributed (particle diameter is 50-60nm and is evenly distributed)；
Step 1) in, described technical grade Ludox is 70:1 with the mass ratio of simple substance silica flour；
Step 2) in, described pretreatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:70；
Step 3) in, described big particle diameter silica gel I is 70:1 with the mass ratio of simple substance silica flour；
Step 4) in, described pretreatment silicon sol solution II is 80:70 with the mass ratio of mixed ammonium/alkali solutions.
2. particle diameter is the preparation of acidic silicasol of 20-30nm, comprises the steps:
1) taking in the technical grade Ludox that concentration is 10%, stir under 300r/min, oil bath heat gradient is warming up to 75
After DEG C, add simple substance silica flour, obtain pretreatment silica gel solution；Described heating curve is: 0-15min is heated to 60 DEG C, constant temperature
10min, continuing to be heated to temperature is 75 DEG C；
2) pretreatment silica gel solution is added mixed ammonium/alkali solutions with the speed of 20mL/h, after dropping, continue reaction 6 little
Time, centrifugation, obtain big particle diameter silica gel；
3) above-mentioned big particle diameter silica gel is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, to obtain final product
Big particle diameter and the acidic silicasol that is evenly distributed (particle diameter is 20-30nm and is evenly distributed)；
Described silica flour, technical grade Ludox, the mass ratio of mixed ammonium/alkali solutions are 1:80:70.
Gained acidic silicasol index is as shown in table 2:
Table 2 acidic silicasol
| Acidic silicasol particle diameter | 20-30nm | 50-60nm |
| SiO2Mass fraction | 40.5% | 42.3% |
| Viscosity (20 DEG C) | 5.1mPa.S | 6.7mPa.S |
| Metal oxide content | ＜ 0.12% | ＜ 0.10% |
Embodiment 3
1. particle diameter is the preparation of acidic silicasol of 50-60nm, comprises the steps:
1) taking the technical grade Ludox that mass concentration is 15%, stir under 350r/min, it is 80 that oil bath is heated to temperature
After DEG C, add simple substance silica flour, obtain pretreatment silica gel solution I；Described heating curve is: 0-10min is heated to 50 DEG C, constant temperature
10min, continuing to be heated to temperature is 80 DEG C；
2) pretreatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 60mL/h, after dropping, continue reaction 8
Hour, centrifugation, obtain big particle diameter silica gel I；
3) taking above-mentioned big particle diameter silica gel I, being diluted to mass concentration is 15%, stirs under 350r/min, and oil bath is heated
After being 80 DEG C to temperature, add simple substance silica flour, obtain pretreatment silica gel solution II；
4) pretreatment silica gel solution II is added mixed ammonium/alkali solutions with the speed of 60mL/h, after dropping, continue reaction 8
Hour, centrifugation, obtain big particle diameter silica gel II；
5) big particle diameter silica gel II is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, obtain greatly
Particle diameter and the acidic silicasol that is evenly distributed (particle diameter is 50-60nm and is evenly distributed)；
Step 1) in, described technical grade Ludox is 80:1 with the mass ratio of simple substance silica flour；
Step 2) in, described pretreatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:90；
Step 3) in, described big particle diameter silica gel I is 80:1 with the mass ratio of simple substance silica flour；
Step 4) in, described pretreatment silicon sol solution II is 80:90 with the mass ratio of mixed ammonium/alkali solutions.
2. particle diameter is the preparation of acidic silicasol of 20-30nm, comprises the steps:
1) taking in the technical grade Ludox that concentration is 15%, stir 10min under 350r/min, oil bath heat gradient heats up
After 80 DEG C, add simple substance silica flour, obtain pretreatment silica gel solution；Described heating curve is: 0-10min is heated to 50 DEG C, permanent
Temperature 10min, continuing to be heated to temperature is 80 DEG C；
2) pretreatment silica gel solution is added mixed ammonium/alkali solutions with the speed of 60mL/h, after dropping, continue reaction 8 little
Time, centrifugation, obtain big particle diameter silica gel；
3) above-mentioned big particle diameter silica gel is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, to obtain final product
Big particle diameter and the acidic silicasol that is evenly distributed (particle diameter is 20-30nm and is evenly distributed)；
Described silica flour, technical grade Ludox, the mass ratio of mixed ammonium/alkali solutions are 1:80:90.
Gained acidic silicasol index is as shown in table 3:
Table 3 acidic silicasol
| Acidic silicasol particle diameter | 20-30nm | 50-60nm |
| SiO2Mass fraction | 41.0% | 43.1% |
| Viscosity (20 DEG C) | 5.2mPa.S | 6.75mPa.S |
| Metal oxide content | ＜ 0.12% | ＜ 0.10% |
Although the detailed description of the invention of the present invention is described by the above-mentioned accompanying drawing that combines, but not the present invention is protected model
The restriction enclosed, one of ordinary skill in the art should be understood that on the basis of technical scheme, and those skilled in the art are not
Need to pay various amendments or deformation that creative work can make still within protection scope of the present invention.
Claims (9)
1. big particle diameter and a preparation method for the acidic silicasol that is evenly distributed, is characterized in that, comprise the steps:
1) taking the technical grade Ludox that mass concentration is 10%-15%, stir under 300-350r/min, oil bath is heated to temperature
After being 75 DEG C-80 DEG C, add simple substance silica flour, obtain pretreatment silicon sol solution I；
2) pretreatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropping, continue reaction 6～
8 hours, centrifugation, obtain big particle diameter Ludox I；
3) taking above-mentioned big particle diameter Ludox I, being diluted to mass concentration is 10%-15%, stirs under 300-350r/min, oil
Bath is heated to after temperature is 75 DEG C-80 DEG C, adding simple substance silica flour, obtaining pretreatment silicon sol solution II；
4) pretreatment silicon sol solution II is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropping, continue reaction
6～8 hours, centrifugation, obtain big particle diameter Ludox II；
5) big particle diameter Ludox II is swapped reaction, evaporation and concentration by sodium form 732 cation exchange resin, obtain grain greatly
Footpath and the acidic silicasol that is evenly distributed；
Step 1) in, described technical grade Ludox is 70-80:1 with the mass ratio of simple substance silica flour；
Step 2) in, described pretreatment silica gel solution I is 80:70-90 with the mass ratio of mixed ammonium/alkali solutions；
Step 3) in, described big particle diameter silica gel I is 70-80:1 with the mass ratio of simple substance silica flour；
Step 4) in, described pretreatment silicon sol solution II is 80:70-90 with the mass ratio of mixed ammonium/alkali solutions.
2. preparation method as claimed in claim 1, is characterized in that, step 1) in, the mesh number of described silica flour is 80-325 mesh, pure
Degree reaches more than 99.9%.
3. preparation method as claimed in claim 1, is characterized in that, step 2) in, described mixed ammonium/alkali solutions is ammonia and alkali
Metal hydroxides or the mixed liquor of organic base.
4. preparation method as claimed in claim 3, is characterized in that, described ammonia and alkali metal hydroxide or organic base
Mol ratio is 4～8:1.
5. preparation method as claimed in claim 1, is characterized in that, step 2) in, the particle diameter of described big particle diameter Ludox I is
20-30nm。
Ludox prepared by either method the most according to claims 1 to 5, it is characterised in that the particle diameter of described Ludox
For 50-60nm.
7. the Ludox described in claim 6 is applied in preparing wine clarificant.
8. the Ludox described in claim 6 is applied in preparing gelled lead acid battery.
9. the Ludox described in claim 6 is applied in the fine hair inorganic agent prepare electrostatic spinning.
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| US10604411B2 (en) * | 2015-07-31 | 2020-03-31 | Fujimi Incorporated | Method for producing silica sol |
| CN105293504B (en) * | 2015-11-10 | 2018-02-13 | 山东银丰纳米新材料有限公司 | A kind of method that organo-mineral complexing catalysis prepares monodispersed large grain-size Ludox |
| CN106395836B (en) * | 2016-08-26 | 2018-08-28 | 强新正品（苏州）环保材料科技有限公司 | A kind of high stable Ludox and preparation method thereof |
| CN109319795B (en) * | 2018-10-18 | 2020-07-31 | 江西星火狮达科技有限公司 | Method for producing silica sol by recovering and purifying silicon powder from organic silicon slag |
| CN118022701B (en) * | 2024-04-11 | 2024-07-05 | 齐鲁工业大学(山东省科学院) | Small-pore silica gel clarifying agent and preparation method and application thereof |
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