CN106006651B - Acidic silicasol and preparation method thereof - Google Patents
Acidic silicasol and preparation method thereof Download PDFInfo
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- CN106006651B CN106006651B CN201610324627.1A CN201610324627A CN106006651B CN 106006651 B CN106006651 B CN 106006651B CN 201610324627 A CN201610324627 A CN 201610324627A CN 106006651 B CN106006651 B CN 106006651B
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- exchange column
- silicic acid
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The present invention provides a kind of acidic silicasol acidic silicasol, viscosity<2cp, pH value are 2~3；The content of silica is 35%~40% in Ludox, and the average grain diameter of silica is 20~50nm；Na in Ludox+<500ppm.The present invention also provides the preparation methods of above-mentioned acidic silicasol.Acidic silicasol concentration produced by the present invention is high, viscosity is low, has higher stability at room temperature.
Description
Technical field
The present invention relates to a kind of high concentrations, low viscous, high stable acidic silicasol and preparation method thereof.
Background technology
Ludox is the colloidal solution that silicon dioxide microparticle is dispersed in water, also known as colloidal silicon dioxide, because having
The advantages that particle is uniform, nontoxic and pollution-free, large specific surface area, reactivity are high, adsorption capacity and adhesive property are strong and use extensively
In all conglomeraties such as building coating, hot investment casting, refractory ceramic material, catalyst carrier, papermaking, weaving, food.
The preparation method of Ludox is numerous, has two class of dispersoid and coagel for principle, there is ion for technique
Exchange process, elemental silicon dissolution method, peptisation, electroosmose process, direct acidization etc., ion exchange methods are because simple for process, former
Expect research and production of low cost and that be widely used in Ludox, and the achievable Ludox of adjustment of ion-exchange process is dense
The adjusting of the performances such as degree, viscosity, grain size, impurity content and stability.
Ludox because pH value difference is divided into alkalinity and acid two classes, deposit by the wherein high stability of alkaline silica sol, room temperature
The storage phase is generally 2 years or more, but metal ion in alkaline silica sol（Usually sodium ion）Content is higher, this makes it be thrown in chemistry
The application of the industries such as light, catalysis is restricted.Metal ion content is relatively low in acidic silicasol, can effectively avoid polishing device
Pollution and the problems such as catalyst poisoning, but its stability is relatively low, storage at room temperature time are generally 3~6 months or even shorter,
This makes the viscosity of acidic silicasol that can be gradually increased in placement process, to influence the storage, transport and reality of Ludox
It applies on border.In addition, this low problem of acidic silicasol stability can limit the raising of its concentration, to ensure acidic silicasol again
Stability, concentration are usually 10%~30%, currently, preparing high concentration, low viscous and high stability acidic silicasol as grinding
The hot spot studied carefully.
Invention content
The purpose of the present invention is to provide a kind of acidic silicasol and preparation method thereof, acidic silicasol concentration obtained
Height, viscosity are low, have higher stability at room temperature.
To achieve the above object, the present invention provides a kind of acidic silicasol, viscosity<2cp, pH value are 2~3；Ludox
The content of middle silica is 35%~40%, and the average grain diameter of silica is 20~50nm；Na in Ludox+<500ppm。
The present invention also provides the preparation methods of above-mentioned acidic silicasol, include the following steps：
1）It is successively handed over by highly acidic cation exchange column and strong alkalinity anion after waterglass is diluted with deionized water
Change column；
2）PH value of solution is adjusted to 7.0 or more with lye again, active silicic acid solution is made；
3）It takes the above-mentioned active silicic acid solution of certain volume in reaction vessel, heats certain time, crystal seed is made；
4）Concentration method is heated using permanent liquid level, active silicic acid solution is persistently added dropwise in above-mentioned crystal seed, it is molten that alkalinity silicon is made
Glue；
5）By above-mentioned alkaline silica sol by highly acidic cation exchange column, acidic silicasol is made.
Preferably, step 1）In waterglass used be sodium silicate, the modulus of sodium silicate is 3.2~3.4.
Preferably, based on mass fraction, step 1）A concentration of the 3%~6% of silica after middle waterglass dilution.
Preferably, step 1）Water glass solution is handed over by highly acidic cation exchange column, strong alkalinity anion after middle dilution
The flow velocity for changing column is 2~4BV/h（BV is resin bed volume）.
Preferably, step 2）The pH value of middle active silicic acid solution is 7~8；Step 2）In lye used be sodium hydroxide, ammonia
Water or amine, a concentration of the 4%~10% of lye.
Preferably, step 3）The time of middle heating is 6~12h.
Preferably, step 4）The middle volume that active silicic acid solution is added dropwise is 10~15 times of crystal seed volume；Step 4）Middle perseverance
Liquid level heating concentration temperature be 90~100 DEG C, the time be 1~3d, carried out under certain vacuum degree, vacuum degree control-
0.01Mpa~-0.05Mpa.
Preferably, step 5）The flow velocity that neutral and alkali Ludox passes through highly acidic cation exchange column is 2~4BV/h.
Preferably, institute's spent ion exchange resin is in the highly acidic cation exchange column and strong alkalinity anion exchange column
The loading of polystyrene gel type resin, resin is that highly acidic cation exchange column or strong alkalinity anion exchange column volume
60%~80%；Institute's spent ion exchange resin is 732 strong acidic ion resins in highly acidic cation exchange column；Strong basicity the moon from
Institute's spent ion exchange resin is 717 strongly basic anionic resins in sub- exchange column.
The present invention is using waterglass as raw material, using Production of Silica Sol by Ion-Exchange；By control water glass solution concentration,
The pH value of ion exchange flow velocity and solution obtains stable active silicic acid solution；The method concentrated again using permanent liquid level heating,
Active silicic acid solution is continuously added into certain volume mother liquor, by controlling mother liquor amount, additive amount, reaction time, reaction temperature
Etc. parameters prepare alkaline silica sol, then acidic silicasol is prepared by cation exchange resin, the adjustment of response parameter is adjustable
The indexs such as concentration, viscosity, pH, grain size and the stability of Ludox.
The performance of acidic silicasol and active silicic acid solution concentration, ion exchange flow velocity, lye addition, reaction temperature,
The multiple factors such as reaction time are related, and the present invention is by rationally controlling parameters, silica in gained acidic silicasol
Concentration is up to 40%, the viscosity of acidic silicasol<2cp, and the high stability of acidic silicasol, room temperature can place 6~24
Month.
The quality of waterglass has certain influence to the performance of Ludox, preferably selects clear, impurity content few and mould
Number（That is the molar ratio of silica and sodium oxide molybdena）Higher waterglass, modulus are preferably 3.2~3.4.
The concentration of water glass solution preferably controls in 3%~6% range after dilution, and no more than 6%, otherwise waterglass is molten
Liquid easy gel when passing through cation exchange column, so as to cause the hardened of ion exchange resin, not easy cleaning and regeneration；Concentration
Not preferably less than 3%, otherwise follow-up permanent liquid level heating concentration process need to evaporate a large amount of water, energy consumption increases, efficiency reduces.
Water glass solution is preferably controlled by the flow velocity of ion exchange column in 2~4BV/h, and flow velocity is too fast can be so that in the middle part of solution
Segregant not yet exchanges i.e. by ion exchange column, causes exchange to be not thorough, goes out liquid pH and increase；On the one hand flow velocity is excessively slow to be made
Exchange efficiency reduces, and on the other hand so that solution residence time in exchange column is longer, is also easy to produce gelatin phenomenon.
Water glass solution is 3.5~5.0, easily gel by the pH value after ion exchange column, need to carry out stabilization processes,
Solution ph is adjusted to 7.0 or more by the present invention with lye, and lye used can be sodium hydroxide, ammonium hydroxide or amine etc., preferably hydrogen
Sodium oxide molybdena.The boiling point of ammonium hydroxide and amine is usually relatively low, readily volatilized in permanent liquid level heats concentration process, causes the change of bottom liquid pH
Change, easy gel in preparation process.Lye（Sodium hydroxide）Concentration is preferably 4%~10%, if concentration is too low, be added lye amount compared with
Greatly, active silicic acid solution can be diluted；If excessive concentration, easily cause topical gel in adjustment process.
The stability of acidic silicasol is related with sodium ions content, and sodium ions content is lower, and Ludox stability is higher.It is living
Property silicate solution pH adjust quite important, the viscosity, pH value and sodium ions content of alkaline silica sol can be influenced, and then influence
The stability of acidic silicasol.The pH value of active silicic acid solution preferably controls in 7.0~8.0 ranges, if pH is higher than 8.0, adds
It is more to enter lye amount, sodium ion introducing is more, and the sodium ions content that gained alkaline silica sol is exchanged into acidic silicasol is also higher,
The easy gel of room temperature.If pH is less than 7.0, the stability of active silicic acid solution is poor, not yet concentration i.e. gel.The adjusting of pH with
The concentration of active silicic acid solution also has certain relationship, when active silicic acid solution concentration is relatively low（3.0%~4.0%）, active silicic acid
The pH of solution is preferably adjusted to 7.0~7.5；When active silicic acid solution concentration is higher（4.0%~6.0%）, active silicic acid solution
PH is preferably adjusted to 7.5~8.0.
The purpose for preparing crystal seed is that active silicic acid is made to be grown to small particle-size silica, more conducively permanent liquid level heating in next step
The growth of particle in concentration process, heating time are preferably 6~12h.
To obtain high-concentration silicon sol, it is 10~15 times of crystal seed volume that the volume of addition active silicic acid solution, which should control,
Addition manner is added for constant current；High temperature is conducive to the growth of silica dioxide granule, and fluid temperature control is 90~100 in the present invention
℃；Vacuum degree appropriate is conducive to the evaporation of moisture, but vacuum degree is unsuitable excessively high, and otherwise the temperature of solution is difficult to rise, this hair
Bright middle vacuum degree control is -0.01~-0.05Mpa, is adjusted with vacuum regulator；Reaction time（That is active silicic acid solution
The addition time）The growth that can influence silica dioxide granule, to obtain the Ludox product of greater particle size, reaction time of the invention
Control is 1~3d, if the reaction time is too short, Ludox grain size is smaller, and stability is poor, if the reaction time is long, produces effect
Rate reduces.
The flow velocity that alkaline silica sol passes through cation exchange column is preferably 2~4BV/h, and flow velocity is unsuitable too fast, otherwise Ludox
Middle sodium ion removal is not thorough, and can influence the stability of acidic silicasol.
Specific implementation mode
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more
Add and clearly demonstrate technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
The present invention provides a kind of preparation method of acidic silicasol, includes the following steps：
1）It is successively handed over by highly acidic cation exchange column and strong alkalinity anion after waterglass is diluted with deionized water
Change column；
2）PH value of solution is adjusted to 7.0 or more with lye again, active silicic acid solution is made；
3）It takes the above-mentioned active silicic acid solution of certain volume in reaction vessel, heats certain time, crystal seed is made；
4）Concentration method is heated using permanent liquid level, active silicic acid solution is persistently added dropwise in above-mentioned crystal seed, it is molten that alkalinity silicon is made
Glue；
5）By above-mentioned alkaline silica sol by highly acidic cation exchange column, acidic silicasol is made.
Step 1）In waterglass used be sodium silicate, the modulus of sodium silicate is 3.2~3.4.
Based on mass fraction, step 1）A concentration of the 3%~6% of silica after middle waterglass dilution.
Step 1）Water glass solution passes through highly acidic cation exchange column, the stream of strong alkalinity anion exchange column after middle dilution
Speed is 2~4BV/h（BV is resin bed volume）.
Step 2）The pH value of middle active silicic acid solution is 7~8；Step 2）In lye used be sodium hydroxide, ammonium hydroxide or amine,
A concentration of the 4%~10% of lye.
Step 3）The time of middle heating is 6~12h.
Step 4）The middle volume that active silicic acid solution is added dropwise is 10~15 times of crystal seed volume；Step 4）Middle perseverance liquid level heating
The temperature of concentration be 90~100 DEG C, the time be 1~3d, carried out under certain vacuum degree, vacuum degree control -0.01Mpa~-
0.05Mpa。
Step 5）The flow velocity that neutral and alkali Ludox passes through highly acidic cation exchange column is 2~4BV/h.
Institute's spent ion exchange resin is styrene in the highly acidic cation exchange column and strong alkalinity anion exchange column
Be gel type resin, the loading of resin is highly acidic cation exchange column or strong alkalinity anion exchange column volume 60%~
80%；Institute's spent ion exchange resin is 732 strong acidic ion resins in highly acidic cation exchange column；Strong alkalinity anion is handed over
It is 717 strongly basic anionic resins to change institute's spent ion exchange resin in column.
Acidic silicasol prepared by the present invention, viscosity<2cp, pH value are 2~3；The content of silica is in Ludox
35%~40%, the average grain diameter of silica is 20~50nm；Na in Ludox+<500ppm。
The more specific embodiment of the present invention is as follows：
Embodiment 1
13kg waterglass is diluted to 104kg with deionized water（I.e. silica percentage composition is 3.5%）, with 800ml/
The flow velocity of min is respectively by cation and anion-exchange column that size is φ 170mm*1700mm, with 8%NaOH by its pH tune
To 7.0, active silicic acid solution is obtained.It takes 6kg active silicic acids solution to be heated to reflux 6h for 95 DEG C in 10L round-bottomed flasks, prepares crystal seed.
It changes reflux into vacuum distillation apparatus, vacuum degree is adjusted to by -0.02Mpa by pressure reducing valve, weighs 90kg active silicic acids
Solution is continuously added into the flow velocity of 31ml/min in crystal seed with constant flow pump, by adjusting heating amount to adjust evaporation capacity, thus
Maintain the constant of liquid level.After charging, reflux 6h is reheated, to ensure that the active silicic acid of addition is all grown to silica
Particle, the alkaline silica sol thus prepared are exchanged with the flow velocity of 60ml/min by the cation that size is φ 80mm*800mm again
The pH of column, gained acidic silicasol is 2.47, viscosity 1.2cp, solid content 40.2%, wherein Na+Content is 210ppm, surely
Periodically about 2 years.
Embodiment 2
13kg waterglass is diluted to 81kg with deionized water（I.e. silica percentage composition is 4.5%）, with 600ml/
Its pH is adjusted to 7.5 with 8%NaOH, obtains active silicic acid solution by the flow velocity of min by cation and anion-exchange column.Take 6kg
Active silicic acid solution is heated to reflux 6h for 95 DEG C in 10L round-bottomed flasks, prepares crystal seed.65kg active silicic acid solution is weighed, with perseverance
Stream pump is continuously added into the flow velocity of 23ml/min in crystal seed, and vacuum degree is adjusted to -0.02Mpa, adjusts heating amount, maintaining liquid
Face is constant.After charging, it is heated to reflux 6h, gained alkaline silica sol is exchanged with the flow velocity of 60ml/min by cation
The pH of column, gained acidic silicasol is 2.65, viscosity 1.8cp, solid content 39.4%, wherein Na+Content is 360ppm, surely
Periodically about 1 year.
Embodiment 3
The pH of active silicic acid solution in 2 operating process of embodiment is adjusted to 8.0 with NaOH, remaining step is identical, gained
The pH of acidic silicasol is 2.81, viscosity 1.6cp, solid content 38.7%, Na+Content is 490ppm, and stationary phase is about 6
Month.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (1)
1. the preparation method of acidic silicasol, which is characterized in that include the following steps：
1）Successively pass through highly acidic cation exchange column and strong alkalinity anion exchange column after waterglass is diluted with deionized water；
Waterglass used is sodium silicate, and the modulus of sodium silicate is 3.2~3.4；A concentration of the 3% of silica after waterglass dilution
~6%；The flow velocity that water glass solution passes through highly acidic cation exchange column, strong alkalinity anion exchange column after dilution is 2~4BV/
h；
2）PH value of solution is adjusted to 7~8 with lye again, active silicic acid solution is made；Lye used be sodium hydroxide, ammonium hydroxide or amine,
A concentration of the 4%~10% of lye；
3）It takes the above-mentioned active silicic acid solution of certain volume in reaction vessel, heats 6~12h, crystal seed is made；
4）Concentration method is heated using permanent liquid level, active silicic acid solution is persistently added dropwise in above-mentioned crystal seed, alkaline silica sol is made；Drop
It is 10~15 times of crystal seed volume to add the volume of active silicic acid solution；The temperature of permanent liquid level heating concentration is 90~100 DEG C, the time
For 1~3d, carried out under certain vacuum degree, vacuum degree control is in -0.01Mpa~-0.05Mpa；
5）By above-mentioned alkaline silica sol by highly acidic cation exchange column, acidic silicasol is made；Alkaline silica sol passes through strong
The flow velocity of acidic cation exchange column is 2~4BV/h；
Institute's spent ion exchange resin is solidifying for polystyrene in above-mentioned highly acidic cation exchange column and strong alkalinity anion exchange column
The loading of glue-type resin, resin is that highly acidic cation exchange column or strong alkalinity anion exchange the 60%~80% of column volume；
Institute's spent ion exchange resin is 732 strong acidic ion resins in highly acidic cation exchange column；Strong alkalinity anion exchange column
Middle institute's spent ion exchange resin is 717 strongly basic anionic resins；
Acidic silicasol obtained, viscosity<2cp, pH value are 2~3；The content of silica is 35%~40% in Ludox,
The average grain diameter of silica is 20~50nm；Na in Ludox+<500ppm。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1155514A (en) * | 1996-01-25 | 1997-07-30 | 天津市化学试剂一厂 | Manufacture of high purity, high concentration and high granularity large granular silicon dioxide gel |
| CN102432027A (en) * | 2011-08-31 | 2012-05-02 | 湖北大学 | Monodisperse large-grain-diameter and high-stability acid silica sol and preparation method thereof |
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2016
- 2016-05-17 CN CN201610324627.1A patent/CN106006651B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1155514A (en) * | 1996-01-25 | 1997-07-30 | 天津市化学试剂一厂 | Manufacture of high purity, high concentration and high granularity large granular silicon dioxide gel |
| CN102432027A (en) * | 2011-08-31 | 2012-05-02 | 湖北大学 | Monodisperse large-grain-diameter and high-stability acid silica sol and preparation method thereof |
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