CN104860322B - A kind of preparation method of low sodium ions content high-purity silicasol - Google Patents
A kind of preparation method of low sodium ions content high-purity silicasol Download PDFInfo
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Abstract
The present invention is a kind of preparation method of low sodium ions content high-purity silicasol, and this method includes：Using industrial metasilicate and sulfuric acid as raw material, 3~6wt% sodium silicate aqueous solution and 20~30wt% aqueous sulfuric acid are configured to；Sodium silicate aqueous solution is added into retort, under 80 150 revs/min of speed of agitator, 30 40 DEG C are warming up to, it is 1~2 to add aqueous sulfuric acid to pH, is warming up to 60~80 DEG C and is incubated 3~4 hours；Plus deionized water be washed to washing water conductivity to below 20 μ s/cm then；Filter cake after washing is transferred to peptization tank, plus 8~10wt% of deionized water adjustment silica concentration, under 80~100 revs/min of low whipping speed, stirring 20~30 minutes, it is 9~10 to add chemical pure ammoniacal liquor adjustment slurry pH, it is warming up to 120~150 DEG C and is incubated the Ludox obtained for 34 hours, be filtrated to get the silicon sol solution of clarification；Concentrating silica made from finally being concentrated to 40~41wt% of concentration, sodium ions content is less than 0.01%.
Description
Technical field
The present invention relates to the preparation method of Ludox, more specifically to a kind of low sodium ions content high-purity silicasol
Preparation method.
Background technology
Ludox is the colloidal solution that is dispersed in water of colloidal particles of silica, is amorphous Si O2Particle is in water
The stable dispersion system of formation.As a kind of important inorganic macromolecule material, Ludox is widely used to chemical industry, accurate casting
Make, weave, papermaking, coating, food, electronics, the field such as ore dressing.
Because common Ludox sodium ions content is too high, the industries, and high-purity silicasol master such as industry casting are only used for
The industries such as polished semiconductor, the preparation of catalyst carrier, kinescope adhesive, glass fibre are applied to, therefore, exploitation is a kind of
Simple, the with low cost high-purity silicasol method of technique, the upgrading of industries for Ludox is particularly important.
The Ludox industrial process of current comparative maturity mainly includes the step water of (1) ion-exchange (2) elemental silicon one
Solution, other techniques are mostly still in the laboratory research stage.The technique of two kinds of production methods is summarized as follows：
(1) ion-exchange reactions
First by waterglass distilled water diluting, by certain flow rate by cationic ion-exchange resin layer, make Na in waterglass+
With the H on cationic ion-exchange resin+Ion exchange is carried out, and is taken a sample to check at any time.Now, the Na in waterglass+It has been be removed that, H+With the SiO in waterglass3 2-Ion combination flows out into active polysilicon acid solution thin liquid.Ion-exchange reactions formula is
2RSiO3H+Na2O·nSiO2→2RSiO3Na+(nSiO2+H2O)
Male post Ludox
The poly- silicon pH value of solution generated after ion exchange is 2-3, need to add a small amount of stabilizer such as Na0H solution.And it is rapid
Stirring makes colloidal sol quickly reach pH=8.5-10.5, and ie in solution is in the region of stable state.
(2) elemental silicon dissolution method
Elemental silicon dissolution method is a kind of new technology for preparing Ludox of rising in recent years, newly upper Ludox domestic at present
The method is used mesh more.Preparing reason is：Elemental silicon reacts under the catalytic action of alkali with water, generates silicate hydrate, silicate hydrate
Gradually it polymerize in water, is voluntarily dehydrated by monomer and aggregates into diploid, triplet or even polyploid gradually, become silicate hydrate
The aqueous solution, be exactly Ludox.
Elemental silicon dissolution process prepares the flow of Ludox as shown in figure 1, with deionized water as dissolving medium, by pure silicon
Powder is added thereto, plus the appropriate base catalyst of people, is then heated whole dissolver, can be obtained after reaction Ludox into
Product.
In order to which the Ludox patent CN1155514A for preparing high-purity discloses " high-purity, high concentration, high single-size
The manufacture method of the large granular silicon dioxide gel of distribution " this method, using ion exchange twice, and adds sulfuric acid, oxalic acid and removes
It is miscellaneous.Ammonium ion exchange is eventually passed, the stable Ludox of ammonification is prepared, although high-purity silicon can be prepared using this method molten
Glue, but technological process is long, and ion exchange is repeated, and cost is high, and patent CN1064878A discloses " high-purity superfine silica sol
Preparation method " invention by tertiary amine and epoxyalkane reaction generation organic base, in the basic conditions, hydrolyzing tetraethoxy orthosilane,
Form Ludox.It is mainly using this method and prepares the effective high-purity silicasol of electronigraph.Patent EP0504467A1 is disclosed
" a kind of preparation method of high-purity silicasol " its using sodium metasilicate be that raw material by following steps prepares high-purity silicasol：
1) dilute silicate solution cationic ion-exchange resin exchanges and obtains acidic silicic acid；
2) acid, sulfuric acid, nitric acid, oxalic acid ageing are strengthened；
3) again through zwitterion resins exchange, further deionization；
4) take part potassium, soda stable as bottom liquid；
5) heating of bottom liquid and add active silicic acid in the case where alkali is stable, make granular grows, and at the boil evaporation water yield and
The active silicic acid amount of addition is equal；
6) the stable metal ion introduced of alkali is removed through cation and anion exchange again；
7) stir lower ammonification and realize that Ludox is made in stabilisation.
In order to obtain the Ludox of high-purity in above-mentioned several patents document, generally require by ion exchange several times,
Resin needs regeneration repeatedly, wastes substantial amounts of human and material resources, causes environmental pollution.
The content of the invention：
For the deficiency of the production high-purity silicasol method of current Ludox, reduction pollution, reduction production cost, Wo Menfa
Understand a kind of working system of the high-purity silicasol of low sodium ions content, using this method, raw material is easy to get, technique is simple, it is easy to work
Industry.
The present invention uses industrial metasilicate for raw material, low using gel-peptization method prepares narrowly distributing, sodium ions content
High-purity silicasol.
In order to solve the above technical problems, the invention provides a kind of preparation method of low sodium ions content high-purity silicasol,
This method comprises the following steps：
1) dispensing：The industrial metasilicate that modulus is 3.3~3.4 is added water and is configured to 3~6wt% sodium silicate aqueous solution,
Industrial sulphuric acid, which adds water, is configured to 20~30wt% aqueous sulfuric acid；
2) prepared by gel：By step 1) prepare sodium silicate aqueous solution add retort, be kept stirring for speed 80~150
Rev/min, 30~40 DEG C are warming up to, step 1 is added using 200~300ml/min speed) aqueous sulfuric acid prepared is to pH as 1
~2, it is warming up to 60~80 DEG C of insulations and obtains gel in 3~4 hours；
3) wash：By step 2) gel for preparing adds the deionized water of suction filtration tank, power-up conductance in 2~5 μ s/cm
Washed, be washed to washing water conductivity untill below 50 μ s/cm；
4) peptization：By step 3) the obtained filter cake of washing is transferred to peptization tank, plus deionized water adjustment silica concentration is extremely
Stirred 20~30 minutes under 8-10wt%, 80~100 revs/min of low whipping speed, the chemical pure ammoniacal liquor adjustment slurry pH to 9 of addition~
10, it is warming up to 120~150 DEG C and is incubated 3~4 hours；
5) filter：By step 4) obtained product, it is removed by filtration the Ludox that the gel not reacted clarified molten
Liquid；
6) concentrate：By step 5) made from silicon sol solution be concentrated into 40~41wt% of concentration, sodium ions content is less than
0.01wt%.
The inventive method compared with prior art, with simple to operate, it is easy to industrialized feature, and uses the present invention
Method, which prepares Ludox, has the advantages that sodium ions content is low, Ludox concentration is high.
Brief description of the drawings
Fig. 1 is the flow chart that elemental silicon dissolution process prepares Ludox.
Embodiment：
In order that the inventive method easily facilitates understanding, with reference to embodiment to technical side of the present invention
Case is described further, but the present invention is not limited only to this.
Embodiment 1.
1st, dispensing：3wt% 1000 grams of sodium silicate aqueous solution is prepared, the aqueous solution with Sulphuric acid 30wt% is some standby；
2nd, prepared by gel：By 1000 grams of addition retort of sodium silicate aqueous solution of preparation, 80 revs/min of speed is kept stirring for,
40 DEG C are warming up to, the aqueous sulfuric acid prepared is added to pH as 1~2 using 300ml/min charging rate, 80 DEG C of guarantors are warming up to
Temperature 3 hours；
3rd, wash：Above-mentioned gel is added into suction filtration tank, is washed with deionized water that (deionized water electrical conductivity is maintained at 2
~5 μ s/cm)；Washing water conductivity is washed to below 20 μ s/cm；
4th, peptization：Filter cake after washing is transferred to peptization tank, plus deionized water adjustment silica concentration 8%, in stirring
Stirred 30 minutes under 80 revs/min of speed, it is 9~10 to add chemical pure ammoniacal liquor and adjust slurry to pH, is warming up to 120 DEG C and insulation 4
Hour；
5th, filter：By step 4) obtained product, it is removed by filtration the Ludox that the gel not reacted clarified molten
Liquid.
6 concentrations：Obtained silicon sol solution is concentrated into 40wt%, sodium ions content 0.0087wt%.
Embodiment 2.
1st, dispensing：4wt% 1000 grams of sodium silicate aqueous solution is prepared, the aqueous solution with Sulphuric acid 30wt% is some standby；
2nd, prepared by gel：By 1000 grams of addition retort of sodium silicate aqueous solution of preparation, 90 revs/min of speed is kept stirring for,
40 DEG C are warming up to, the aqueous sulfuric acid prepared is added to pH as 1~2 using 300ml/min charging rate, 70 DEG C of guarantors are warming up to
Temperature 3 hours.
3rd, wash：Above-mentioned gel is added into suction filtration tank, is washed with deionized water that (deionized water electrical conductivity is maintained at 2
~5 μ s/cm)；Washing water conductivity is washed to below 20 μ s/cm.
4th, peptization：Filter cake after washing is transferred to peptization tank, plus deionized water adjustment silica concentration 8wt%, stirred
Mix and stirred 20 minutes under 80 revs/min of speed, add chemical pure ammoniacal liquor adjustment slurry to pH9~10. and be warming up to 130 DEG C and insulation 4
Hour forms Ludox；
5th, filter：By obtained Ludox, the silicon sol solution that the gel not reacted is clarified is removed by filtration；
6 concentrations：By obtained concentrating silica to concentration 40.5wt%, sodium ions content 0.009wt%.
Embodiment 3.
1st, dispensing：5wt% 1000 grams of sodium silicate aqueous solution is prepared, the aqueous solution with Sulphuric acid 30wt% is some standby；
2nd, prepared by gel：By the 5wt% of preparation 1000 grams of addition retort of sodium silicate aqueous solution, speed is kept stirring for
100 revs/min, 30 DEG C are warming up to, the aqueous sulfuric acid prepared is added to pH as 1~2 using 200ml/min speed, is warming up to
70 DEG C are incubated 3 hours；
3rd, wash：Above-mentioned gel is added into suction filtration tank, is washed with deionized water that (deionized water electrical conductivity is maintained at 2
~5 μ s/cm), washing water conductivity is washed to below 20 μ s/cm；
4th, peptization：Filter cake after washing is transferred to peptization tank, plus deionized water adjustment silica concentration 9wt%, stirred
Mix and stirred 20 minutes under 90 revs/min of speed, add chemical pure ammoniacal liquor adjustment slurry to pH9~10. and be warming up to 150 DEG C and insulation 3
Hour forms Ludox；
5th, filter：By obtained Ludox, the silicon sol solution that the gel not reacted is clarified is removed by filtration；
6 concentrations：By obtained concentrating silica to concentration 40.2wt%, sodium ions content 0.006wt%.
Embodiment 4.
1st, dispensing：6wt% 1000 grams of sodium silicate aqueous solution is prepared, the aqueous solution with Sulphuric acid 20wt% is some standby；
2nd, prepared by gel：By the 6wt% of preparation 1000 grams of addition retort of sodium silicate aqueous solution, speed is kept stirring for
150 revs/min, 30 DEG C are warming up to, the aqueous sulfuric acid prepared is added to pH as 1~2 using 200ml/min speed, is warming up to
60 DEG C are incubated 3 hours.
3rd, wash：Above-mentioned gel is added into suction filtration tank, is washed with deionized water that (deionized water electrical conductivity is maintained at 2
~5 μ s/cm).Washing water conductivity is washed to below 50 μ s/cm.
4th, peptization：Filter cake after washing is transferred to peptization tank, plus deionized water adjustment silica concentration 9wt%, stirred
Mix and stirred 30 minutes under 100 revs/min of speed, it is 9~10 to add chemical pure ammoniacal liquor and adjust slurry to pH, is warming up to 150 DEG C and protects
Temperature 4 hours.
5th, filter：By obtained Ludox, the silicon sol solution that the gel not reacted is clarified is removed by filtration.
6 concentrations：By obtained concentrating silica to concentration 40wt%, sodium ions content 0.005wt%.
Claims (1)
1. a kind of preparation method of low sodium ions content high-purity silicasol, it is characterised in that comprise the following steps：
1) prepared by gel：3 ~ 6wt% sodium silicate aqueous solution is added into retort, 80 ~ 150 revs/min of speed is kept stirring for, heated up
To 30 ~ 40 DEG C, the aqueous sulfuric acid using 200 ~ 300ml/min 20 ~ 30wt% of speed addition is warming up to 60 ~ 80 to pH as 1 ~ 2
DEG C insulation obtains gel in 3 ~ 4 hours；
2) wash：By step 1）The gel prepared adds suction filtration tank, power-up conductance and carried out in 2 ~ 5 μ s/cm deionized water
Washing, is washed to washing water conductivity untill below 50 μ s/cm；
3) peptization：By step 2）Wash obtained filter cake and be transferred to peptization tank, plus deionized water adjusts silica concentration to 8-
Stirred 20 ~ 30 minutes under 10wt%, 80 ~ 100 revs/min of low whipping speed, add chemical pure ammoniacal liquor adjustment slurry pH to 9 ~ 10, rise
Temperature is to 120 ~ 150 DEG C and is incubated 3 ~ 4 hours；
4) filter：By step 3）Obtained product, is removed by filtration the silicon sol solution that the gel not reacted is clarified；
5) concentrate：By step 4) made from concentrating silica to concentration be 40 ~ 41wt%, sodium ions content be less than 0.01wt%.
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Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Applicant after: CHINA NATIONAL OFFSHORE OIL Corp. Applicant after: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Applicant after: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Applicant before: CHINA NATIONAL OFFSHORE OIL Corp. Applicant before: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Applicant before: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. |
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Effective date of registration: 20161017 Address after: No. three road 300131 Tianjin city Hongqiao District dingzigu No. 85 Applicant after: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Applicant after: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Applicant before: CHINA NATIONAL OFFSHORE OIL Corp. Applicant before: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Applicant before: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. |
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