CN104445222A - Preparation method of acidic silica sol with large particle size and uniform distribution - Google Patents
Preparation method of acidic silica sol with large particle size and uniform distribution Download PDFInfo
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- CN104445222A CN104445222A CN201410704647.2A CN201410704647A CN104445222A CN 104445222 A CN104445222 A CN 104445222A CN 201410704647 A CN201410704647 A CN 201410704647A CN 104445222 A CN104445222 A CN 104445222A
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Abstract
The invention discloses a preparation method of acidic silica sol with large particle size and uniform distribution. Industrial grade silica sol with 30% of SiO2 content and 80-325-mesh monatomic silicon powder are taken as raw materials, mixed aqueous alkali such as a mixed solution of alkali metal hydroxide or organic base and the like with ammonia water is taken as a catalyst, and the acidic silica sol with large particle size and uniform distribution is prepared with a constant-speed feeding method. The prepared acidic silica sol has large particle size, high viscosity and low oxide content and is uniformly distributed.
Description
Technical field
The invention belongs to Large stone silica gel preparation field, particularly a kind of Large stone and the preparation method of the acidic silicasol that is evenly distributed.
Background technology
The micelle of Large stone, high-concentration silicon sol has huge specific surface area (surperficial many meso-hole structures) and superpower adsorptive power and stronger stability and adhesive property, is widely used in various fields.Such as: using Large stone silicon sol as polishing agent for mono-crystalline silicon, not only effective, and polishing velocity is fast.Acidic silicasol and alkaline silica sol two kinds can be divided into according to solution ph scope.Alkaline silica sol is a kind of stabilising system, relative alkaline silica sol, acidic silicasol is in metastable state, gradually pectisation can occur in put procedure, especially the gel trend of the acidic silicasol of high density is more obvious, becomes the major influence factors of its application of restriction.Because Large stone acidic silicasol has good selectivity and reactive behavior, the chemically machinery polished for electron trade, semi-conductor, hard disk, compound crystal or precision optics can be widely used in.The silicon sol particle diameter of industrial synthesis is generally 10 ~ 20nm, and concentration is 30%, is difficult to meet the requirement of some special industry to colloidal particle size and concentration, and the acidic silicasol of high density be in metastable state, can pectisation be there is in put procedure.How to synthesize particle diameter larger, concentration is higher, and the better acidic silicasol of stability, to meet industrial application demand, has become a focus of current silicon sol research.
At present, the conventional preparation technology of industrial manufacture acidic silicasol has following three kinds:
One is prepared by ion exchange method after water glass dilution, the acidic silicasol poor stability that this method is obtained.If patent US2244325 is raw material with water glass, the shelf-time of obtained acidic silicasol is only several hours and its peak concentration is 15%, improves storage and transportation cost; Patent US3867304 take water glass as raw material, greatly can improve the stability of gained acidic silicasol by repeatedly positively charged ion and anionresin, but the large water gaging of this method consumption and energy, production cost is higher.
Another kind method under the effect of catalyzer, reacts obtained by silica flour and water.As patent CN200710119578.9 adopts silica flour and the obtained acidic silicasol of water reaction, there is the feature of high stability and high density, but the particle scale of silicon sol solution prepared by this method is little, be difficult to meet the requirement to granularity in practical application, as the special colloidal sol of semi-conductor chip polishing etc.
Also having a kind of is raw material with water glass, adopts ion exchange method to prepare active silicic acid, prepares Large stone, single dispersing silicon sol, carry out the method for modified with organic acids at silica particles by the method dripping active silicic acid in seed solution.First active silicic acid is prepared by ion exchange method as patent CN102432027A adopts, joined in the water glass of boiling and be prepared into even-grained alkaline silica sol, adopt organic acid to carry out surface modification, make acidic silicasol finally by ion-exchange, be concentrated into the method for desired concn.
Other method, as patent TW234579B discloses a kind of pH containing methyl alcohol at the Silica abrasive liquid of 1-6, can be used for the polishing of silicon substrate; Patent JP6199515 and JP63123807, by joining in silicon dioxide gel by small amounts aluminium, obtains comparatively stable acid silicon dioxide sol through ion exchange treatment then.Aforesaid method, due to the restriction of method itself or the impact of raw material, often makes the shortcomings such as the acidic silicasol existence and stability that obtains is poor, particle scale is little, metal ion content is high.
Summary of the invention
The object of the invention is for overcoming above-mentioned the deficiencies in the prior art, providing a kind of Large stone and the preparation method of the acidic silicasol that is evenly distributed, significantly can reduce metal oxide content simultaneously and improve silicon sol viscosity, increasing its shelf time.
For achieving the above object, the present invention adopts following technical proposals:
Large stone and a preparation method for the acidic silicasol that is evenly distributed, comprise the steps:
1) get the technical grade silicon sol that mass concentration is 10%-15%, stir under 300-350r/min, it is, after 75 DEG C-80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silicon sol solution I;
2) pre-treatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropwising, continue reaction 6 ~ 8 hours, centrifugation, obtains Large stone silicon sol I;
3) get above-mentioned Large stone silicon sol I, being diluted to mass concentration is 10%-15%, stirs under 300-350r/min, and it is, after 75 DEG C-80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silicon sol solution II;
4) pre-treatment silicon sol solution II is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropwising, continue reaction 6 ~ 8 hours, centrifugation, obtains Large stone silicon sol II;
5) Large stone silicon sol II is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed;
Wherein, step 1) in, the mass ratio of described technical grade silicon sol and simple substance silica flour is 70-80:1;
Step 2) in, described pre-treatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:70-90;
Step 3) in, described Large stone silica gel I is 70-80:1 with the mass ratio of simple substance silica flour;
Step 4) in, described pre-treatment silicon sol solution II is 80:70-90 with the mass ratio of mixed ammonium/alkali solutions.
The concentration of above-mentioned technical grade silicon sol is in 10-15% scope, and in guarantor unit's volume, the reactive behavior of silicon dioxide granule is moderate, makes grain growth speed surely be held between a given zone, ensures the homogeneity generating particle.If silica concentration content is too low, because the quantity of silicon dioxide granule in unit volume is comparatively rare, collide between particle and the chance occurred that reacts reduces greatly, the rate of growth affecting silica dioxide granule affects the homogeneity of its particle; On the other hand, silica concentration too high levels, then in reaction process, the silica concentration of system reaches higher numerical value very soon, system viscosity becomes large earlier, by the stability of the rate of growth and silicon sol that affect silicon dioxide granule, the quality of the silica flour added together will be restricted, thus limit the further growth of silicon dioxide granule.
Further, step 1) in, the order number of described silica flour is 80-325 order, and purity reaches more than 99.9%.By adding high purity simple substance silica flour, and amberlite Ester exchange subsequently, eliminate metallic cation impurity significantly, ensure that high purity and the stability of silicon sol.
Further, step 2) in, described mixed ammonium/alkali solutions is the mixed solution of ammoniacal liquor and alkali metal hydroxide or organic bases.
Further, step 2) in, the particle diameter of described Large stone silicon sol I is 20-30nm.
Preferably, the mol ratio of described ammoniacal liquor and alkali metal hydroxide or organic bases is 4 ~ 8:1.
Silicon sol prepared by above-mentioned either method, its particle diameter is 50-60nm.
Present invention also offers the preparation method that a kind of particle diameter is the acidic silicasol of 20-30nm, comprise the steps:
1) getting concentration is in the technical grade silicon sol of 10%-15%, stirs under 300-350r/min, and it is, after 75 DEG C-80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silicon sol solution;
2) pre-treatment silicon sol solution is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropwising, continue reaction 6 ~ 8 hours, centrifugation, obtains Large stone silica gel;
3) Large stone silicon sol is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain the acidic silicasol that particle diameter is 20-30nm;
The mass ratio of described silica flour, technical grade silicon sol, mixed ammonium/alkali solutions is 1:80:70-90.
Acidic silicasol prepared by the present invention add beer ferment after solution in, impure ion can be made to generate condensation product and be removed, make product limpid bright.Also can be used for the finings of rice wine, soy sauce, fruit juice etc., do not affect the color of product.And silicon is for human non-toxic's evil.When acidic silicasol is on gelled lead acid battery, the colloidal silica generated after mixing with sulfuric acid is the ideal not flowing electrolyte of gelled lead acid battery.It changes leakage acid, the contaminate environment of traditional lead acid batteries, and heavy acid adding, adds water and the shortcoming such as maintenance, and the work-ing life of store battery is extended, and low-temperature startup performance is good, shatter-proof, once pours into, safe and reliable.Acidic silicasol is applied in static flocking technology, be because acidic silicasol forms silanol group at its fiber surface, and make fiber have wetting ability, flocking hair charging property is improved, it is the main component of the fine hair treatment agent of static flocking, plays dissemination.
The present invention is owing to taking above technical scheme, and it has the following advantages:
1. adopt the mixed ammonium/alkali solutions mixed solution of ammoniacal liquor (alkali metal hydroxide, the organic bases etc. with) constant speed charging method effectively to control glue nucleus growth, reproducible
2. synthesized Large stone and the acidic silicasol solution be evenly distributed, the present invention prepares the acidic silicasol solution of the even particle size distribution such as 20-30nm, 50-60nm.Overcome the problem that silicon sol size distribution prepared by prior art is uneven.
3. raw material made by the present invention's silica flour, reduces costs, and overcomes existing silicon sol preparation method and adopts water glass to be raw material, cause the problem that complex steps, water consumption are large, cost is high.。
4. the acidic silicasol stability prepared of the present invention is high, and normal temperature can be stored and not occur coagulation and gelatin phenomenon in more than six months.
5. the acidic silicasol that prepared by the present invention can be used for the fine hair treatment agent preparing finings, gelled lead acid battery, static flocking.
Accompanying drawing explanation
The acidic silicasol SEM of Figure 120-30nm schemes
The acidic silicasol SEM of Figure 25 0-60nm schemes
Embodiment
Mode by the following examples further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally selects with condition.
Embodiment 1:
The size of the silicon-dioxide involved by following embodiment all adopts scanning electronic microscope (SEM) to measure, in silicon sol, SiO2 content adopts gravimetric determination, silicon sol viscosity adopts constant detection of capillary tube viscosity, metal oxide content adopts inductive coupling plasma emission spectrograph to measure, and pH value adopts acidometer to measure.The stability of acidic silicasol measures according to following method: with salt acid for adjusting pH to 2.5, after stirring, add 0.375g Virahol, continues to stir, gets above-mentioned silicon sol 6.0g, shake up, put into 60 DEG C of baking ovens, record gel time 163h.
With technical grade silicon sol (SiO
2content 30%) and 80-325 order simple substance silica flours as raw material, the mixed ammonium/alkali solutions mixed solution of ammoniacal liquor (such as alkali metal hydroxide or the organic bases etc. with) is catalyzer, adopts constant speed charging legal system for Large stone and the acidic silicasol be evenly distributed.Concrete steps are as follows,
1. particle diameter is the preparation of the acidic silicasol of 50-60nm, comprises the steps:
1) get the technical grade silicon sol that mass concentration is 12%, stir under 320r/min, it is, after 80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silica gel solution I;
2) pre-treatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 40mL/h, after dropwising, continue reaction 7 hours, centrifugation, obtains Large stone silica gel I;
3) get above-mentioned Large stone silica gel I, being diluted to mass concentration is 12%, stirs under 320r/min, and it is, after 80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silica gel solution II;
4) pre-treatment silica gel solution II is added mixed ammonium/alkali solutions with the speed of 40mL/h, after dropwising, continue reaction 6 ~ 8 hours, centrifugation, obtains Large stone silica gel II;
5) Large stone silica gel II is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed (particle diameter is 50-60nm and is evenly distributed);
Step 1) in, the mass ratio of described technical grade silicon sol and simple substance silica flour is 80:1;
Step 2) in, described pre-treatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:80;
Step 3) in, described Large stone silica gel I is 80:1 with the mass ratio of simple substance silica flour;
Step 4) in, described pre-treatment silicon sol solution II is 80:80 with the mass ratio of mixed ammonium/alkali solutions.
2. particle diameter is the preparation of the acidic silicasol of 20-30nm, comprises the steps:
1) get the technical grade silicon sol that concentration is 12%, stir under 320r/min, it is, after 80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silica gel solution;
2) pre-treatment silica gel solution is added mixed ammonium/alkali solutions with the speed of 40mL/h, after dropwising, continue reaction 7 hours, centrifugation, obtains Large stone silica gel;
3) above-mentioned Large stone silica gel is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed (particle diameter is 20-30nm and is evenly distributed);
The mass ratio of described silica flour, technical grade silicon sol, mixed ammonium/alkali solutions is 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 |
| SiO 2Massfraction | 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 the acidic silicasol of 50-60nm, comprises the steps:
1) get the technical grade silicon sol that mass concentration is 10%, stir under 300r/min, it is, after 75 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silica gel solution I; Described heating curve is: 0-15min is heated to 60 DEG C, constant temperature 10min, and continuing to be heated to temperature is 75 DEG C;
2) pre-treatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 20mL/h, after dropwising, continue reaction 6 hours, centrifugation, obtains Large stone silica gel I;
3) get above-mentioned Large stone silica gel I, being diluted to mass concentration is 10%, stirs under 300r/min, and it is, after 75 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silica gel solution II;
4) pre-treatment silica gel solution II is added mixed ammonium/alkali solutions with the speed of 20mL/h, after dropwising, continue reaction 6 hours, centrifugation, obtains Large stone silica gel II;
5) Large stone silica gel II is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed (particle diameter is 50-60nm and is evenly distributed);
Step 1) in, the mass ratio of described technical grade silicon sol and simple substance silica flour is 70:1;
Step 2) in, described pre-treatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:70;
Step 3) in, described Large stone silica gel I is 70:1 with the mass ratio of simple substance silica flour;
Step 4) in, described pre-treatment silicon sol solution II is 80:70 with the mass ratio of mixed ammonium/alkali solutions.
2. particle diameter is the preparation of the acidic silicasol of 20-30nm, comprises the steps:
1) getting concentration is in the technical grade silicon sol of 10%, stirs, after oil bath heat gradient is warming up to 75 DEG C, add simple substance silica flour, obtain pre-treatment silica gel solution under 300r/min; Described heating curve is: 0-15min is heated to 60 DEG C, constant temperature 10min, and continuing to be heated to temperature is 75 DEG C;
2) pre-treatment silica gel solution is added mixed ammonium/alkali solutions with the speed of 20mL/h, after dropwising, continue reaction 6 hours, centrifugation, obtains Large stone silica gel;
3) above-mentioned Large stone silica gel is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed (particle diameter is 20-30nm and is evenly distributed);
The mass ratio of described silica flour, technical grade silicon sol, mixed ammonium/alkali solutions is 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 |
| SiO 2Massfraction | 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 the acidic silicasol of 50-60nm, comprises the steps:
1) get the technical grade silicon sol that mass concentration is 15%, stir under 350r/min, it is, after 80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silica gel solution I; Described heating curve is: 0-10min is heated to 50 DEG C, constant temperature 10min, and continuing to be heated to temperature is 80 DEG C;
2) pre-treatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 60mL/h, after dropwising, continue reaction 8 hours, centrifugation, obtains Large stone silica gel I;
3) get above-mentioned Large stone silica gel I, being diluted to mass concentration is 15%, stirs under 350r/min, and it is, after 80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silica gel solution II;
4) pre-treatment silica gel solution II is added mixed ammonium/alkali solutions with the speed of 60mL/h, after dropwising, continue reaction 8 hours, centrifugation, obtains Large stone silica gel II;
5) Large stone silica gel II is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed (particle diameter is 50-60nm and is evenly distributed);
Step 1) in, the mass ratio of described technical grade silicon sol and simple substance silica flour is 80:1;
Step 2) in, described pre-treatment silica gel solution I with the mass ratio of mixed ammonium/alkali solutions is: 80:90;
Step 3) in, described Large stone silica gel I is 80:1 with the mass ratio of simple substance silica flour;
Step 4) in, described pre-treatment silicon sol solution II is 80:90 with the mass ratio of mixed ammonium/alkali solutions.
2. particle diameter is the preparation of the acidic silicasol of 20-30nm, comprises the steps:
1) getting concentration is in the technical grade silicon sol of 15%, stirs 10min, after oil bath heat gradient is warming up to 80 DEG C, add simple substance silica flour, obtain pre-treatment silica gel solution under 350r/min; Described heating curve is: 0-10min is heated to 50 DEG C, constant temperature 10min, and continuing to be heated to temperature is 80 DEG C;
2) pre-treatment silica gel solution is added mixed ammonium/alkali solutions with the speed of 60mL/h, after dropwising, continue reaction 8 hours, centrifugation, obtains Large stone silica gel;
3) above-mentioned Large stone silica gel is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed (particle diameter is 20-30nm and is evenly distributed);
The mass ratio of described silica flour, technical grade silicon sol, mixed ammonium/alkali solutions is 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 |
| SiO 2Massfraction | 41.0％ | 43.1％ |
| Viscosity (20 DEG C) | 5.2mPa.S | 6.75mPa.S |
| Metal oxide content | ＜0.12％ | ＜0.10％ |
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (9)
1. Large stone and a preparation method for the acidic silicasol that is evenly distributed, is characterized in that, comprise the steps:
1) get the technical grade silicon sol that mass concentration is 10%-15%, stir under 300-350r/min, it is, after 75 DEG C-80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silicon sol solution I;
2) pre-treatment silica gel solution I is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropwising, continue reaction 6 ~ 8 hours, centrifugation, obtains Large stone silicon sol I;
3) get above-mentioned Large stone silicon sol I, being diluted to mass concentration is 10%-15%, stirs under 300-350r/min, and it is, after 75 DEG C-80 DEG C, add simple substance silica flour that oil bath is heated to temperature, obtains pre-treatment silicon sol solution II;
4) pre-treatment silicon sol solution II is added mixed ammonium/alkali solutions with the speed of 20-60mL/h, after dropwising, continue reaction 6 ~ 8 hours, centrifugation, obtains Large stone silicon sol II;
5) Large stone silicon sol II is carried out permutoid reaction, evaporation concentration by sodium form 732 Zeo-karb, obtain Large stone and the acidic silicasol that is evenly distributed;
Step 1) in, the mass ratio of described technical grade silicon sol and simple substance silica flour is 70-80:1;
Step 2) in, described pre-treatment silica gel solution I is 80:70-90 with the mass ratio of mixed ammonium/alkali solutions;
Step 3) in, described Large stone silica gel I is 70-80:1 with the mass ratio of simple substance silica flour;
Step 4) in, described pre-treatment 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 order number of described silica flour is 80-325 order, and purity 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 the mixed solution of ammoniacal liquor and alkali metal hydroxide or organic bases.
4. preparation method as claimed in claim 3, it is characterized in that, the mol ratio of described ammoniacal liquor and alkali metal hydroxide or organic bases is 4 ~ 8:1.
5. preparation method as claimed in claim 1, is characterized in that, step 2) in, the particle diameter of described Large stone silicon sol I is 20-30nm.
6. silicon sol prepared by either method according to claims 1 to 5, is characterized in that, the particle diameter of described silicon sol is 50-60nm.
7. silicon sol according to claim 6 is applied preparing in wine clarificant.
8. silicon sol according to claim 6 is applied preparing in gelled lead acid battery.
9. silicon sol according to claim 6 is applied in the fine hair treatment agent preparing static flocking.
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| CN109319795A (en) * | 2018-10-18 | 2019-02-12 | 江西星火狮达科技有限公司 | The method of recycling purification silicon powder production silica solution from organosilicon slag |
| 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 |
| CN118022701A (en) * | 2024-04-11 | 2024-05-14 | 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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