CN103466635B - Preparation method for silicon dioxide - Google Patents

Preparation method for silicon dioxide Download PDF

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CN103466635B
CN103466635B CN201310373057.1A CN201310373057A CN103466635B CN 103466635 B CN103466635 B CN 103466635B CN 201310373057 A CN201310373057 A CN 201310373057A CN 103466635 B CN103466635 B CN 103466635B
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sodium silicate
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silica slurry
silicate solution
pressure
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CN103466635A (en
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王永庆
阙伟东
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Quechen Silicon Chemical Co Ltd
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Quechen Silicon Chemical Co Ltd
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Abstract

The invention provides a preparation method for silicon dioxide. The method comprises the following steps: allowing a sodium silicate solution and sulphuric acid to react to obtain silicon dioxide slurry; filtering the silicon dioxide slurry to obtain filtered matters; pulpifying the filtered matters to obtain silicon dioxide seriflux with the viscosity below 1000 cp; drying the silicon dioxide seriflux. The silicon dioxide prepared by the manufacturing technology of the silicon dioxide provided by the invention has suitable particle size, and high dispersity while milling with rubber; when the silicon dioxide is used as a reinforced material, the abrasion and the heat-generation of a rubber product can be obviously lowered, and the breaking strength, the elongation at break, and the tearing strength of the rubber product can be obviously strengthened.

Description

A kind of preparation method of silicon-dioxide
Technical field
The present invention relates to chemical production technical field, in particular to a kind of preparation method of silicon-dioxide.
Background technology
Hydrated SiO 2 is commonly called as white carbon black, and molecular formula is SiO 2nH 2o, mode of appearance is powdery, microballon, particulate state, and white carbon black is the widely used material of reinforcing rubber, in general, because white carbon black (ultra-fine, surface-treated exception) reinforcing effect is good no more than carbon black, therefore belongs to half reinforcement and filler material.Therefore to determine according to use occasion the percentage ratio replacing carbon black.Precipitated silica is used for the Tire & Tube that rubber item has automobile, dump truck, truck, tractor, fork truck, bike etc., industrial belt, sebific duct, liner, offset plate, grain processing shelling rubber roll, and to white carbon black be used all more or less in the various technical rubber goods such as rubber overshoes.The work-ing life that a certain amount of white carbon black can improve tire is added in conventional tyre.Test-results shows according to the study, joins 10 ~ 20 parts of white carbon blacks and just can improve cementing property and tear strength, tread life is improved if can increase, and can also strengthen the gripping power of tire road pavement simultaneously, be beneficial to safe driving.Due to the requirement of energy-saving and emission-reduction and environmental protection, increasing white carbon black is applied to rubber for tire industry.Using white carbon black as filler and natural gum and synthetical glue mixing, being applied to tire can reduce rolling resistance, improves wet and slippery performance, thus make automobile oil consumption low, reduce exhaust gas emission.
White carbon black is applied in tire can improve the wear resistance of goods, tear-resistant intensity and hardness as the weighting agent of rubber, but because the progenitor of common white carbon black is larger, hole in agglomerate and between agglomerate and aggregate is smaller, with compounding rubber bad dispersibility, the heat-dissipating of goods is high, and wear away high, tear strength is low, the tire drag made is large, and in mixing process, consume the more energy.
At present, the main production process of white carbon black mainly contains the intermediate processing in vapor phase process and liquid phase method.The former makes application limited because cost is high.Provide a kind of preparation method of white carbon black in prior art, comprise the following steps: S1, water glass removal of impurities: water glass dissolution of solid is obtained the thick liquid of raw material, then in the thick liquid of raw material, add white carbon black, after filtration, obtain qualified water glass solution; S2, white carbon black synthesize: the water glass solution obtained by step S1 mixes with the vitriol oil, obtains white carbon black crude product after reaction; S3, white carbon black are purified: carry out press filtration, washing, making beating to the white carbon black crude product that step S2 obtains, obtain white carbon black finished product after drying.But the initial size of the white carbon black obtained by aforesaid method comparatively large and and compounding rubber dispersiveness poor, make the abrasion of rubber item and heat-dissipating high, and the problem such as the tensile strength at yield of rubber product, tensile yield and tear strength be low.
Summary of the invention
For the problem of silicon-dioxide in prior art and compounding rubber bad dispersibility, the invention provides a kind of method preparing silicon-dioxide, the method comprises:
A () is reacted: sodium silicate solution and sulfuric acid are reacted, obtains silica slurry;
B () filters: filtered silica slip also obtains much filtrate;
C () pulp: carry out pulp to much filtrate, obtains viscosity at 1000cp(centipoise) following silica slurry; And
D () is dry: dried silica slurries.
Specifically, aforesaid method is implemented in the following manner:
In reactions steps, first in reactor, add the water of the first volume and the mixed solution of sodium silicate solution.Wherein, the first volume is between 30% and 60% of reactor volume, and preferred value is between 40% and 50%, by first adding a certain amount of water and sodium silicate solution in reactor, reaction medium can be provided for reaction, thus accelerate speed of reaction, carrying out smoothly advantageously in reaction; The pH value of the mixed solution of water and sodium silicate solution is between 9.0 and 11.0, and preferred value is between 9.5 and 10.5.Be set between 15rpm and 30rmp by the stir speed (S.S.) in reactor, stir speed (S.S.), between 20rpm and 25rmp, by continuous stirring, and controls between 15rpm and 30rpm by preferred value, effectively can add the speed that fast response carries out; Pass into the water vapour that pressure is greater than 0.3Mpa, make temperature control between 70 DEG C and 100 DEG C, in reactor, then add the sodium silicate solution of volume ratio between 16:1 to 17:1 and sulfuric acid simultaneously, wherein, concentration >=98% of sulfuric acid.The suitable silica dioxide granule of size can be generated by the concentration controlling sodium silicate solution and the volume ratio (between 16:1 to 17:1) of sulfuric acid, the concentration (>=98%) of sulfuric acid and sodium silicate solution; When reacted between 70 minutes and 100 minutes, pH value >=7 of mixed solution when preferred value is between 80 minutes and 90 minutes or when sulfuric acid and water glass, when preferred value is between 7 to 10, reaction terminating; After reaction terminating, in the mixed reaction solution in reactor, drip sulfuric acid to regulate pH value.Thus make the pH value of mixed reaction solution between 2.5 and 6.0, preferred value between 3.5 and 6.0, more preferably between 4.0 and 5.0.In this step, reaction can be enable to carry out completely by the mixed solution in reactor being adjusted to acidity; By temperature of reaction being controlled between 70 DEG C and 100 DEG C, not only the nucleus formation speed of silicon-dioxide is fast but also quantity is many, thus form the suitable crystal of size, in addition, temperature of reaction is controlled between 70 DEG C and 100 DEG C, also can accelerate speed of reaction.
In filtration step, use pressure filter to implement filtration step, setting pressure is between 0.3Mpa and 0.8Mpa, and preferred value is between 0.4Mpa and 0.6Mpa, the time of implementing to filter, preferred value was between 12 minutes and 17 minutes between 10 minutes and 20 minutes.Filtration step comprises washing step further, uses pressure filter to implement washing step.In washing step, setting pressure is between 0.5Mpa and 0.8Mpa, and preferred value is between 0.6Mpa and 0.8Mpa.Repeat washing step, until the washing electrical conductivity of water < 1000 μ s/cm after washing, to remove impurity Na wherein 2sO 4.After filtration and washing step, form much filtrate, content≤3.0% of vitriol in much filtrate; And the solid content of much filtrate is between 15.0% and 30.0%, preferred value is between 20.0% and 25.0%.
In slurry step, use belt conveyor to be sent in hollander by the much filtrate formed in filtration step, much filtrate, between 150rpm and 250rpm, is slurried into the paste liquid (silica slurry) of mobility by the shearing rate controlling hollander impeller.The viscosity of the silica slurry generated is between 100cp and 1000cp, and preferred value is between 400cp and 800cp, and further preferred value is between 600cp and 800cp.In this step, the viscosity by controlling silica slurry can make the silicon-dioxide dispersing property of generation good at below 1000cp.
In drying step, the silica slurry water pump obtained in above-mentioned slurry step is delivered in drying tower and carries out spraying dry, preferred pressure formula drying plant, control the inlet temperature of drying tower between 400 DEG C and 700 DEG C simultaneously, temperature out, between 80 DEG C and 150 DEG C, obtains silicon-dioxide.By controlling the inlet temperature of drying tower between 400 DEG C and 700 DEG C, temperature out can make the hole between the silica dioxide granule of generation comparatively large between 80 DEG C and 150 DEG C, and then makes the dispersing property of silicon-dioxide good.
In method of the present invention, before reactions steps, dissolving step and set-up procedure can also be comprised.In dissolving step, in static pressure kettle, place sodium silicate solid (Na 2onSiO 2) and water, and pass into water vapour, form sodium silicate solution within a certain period of time, after using pressure filter to leach throw out (impurity), obtain transparent pure water glass strong solution.In dissolving step, SiO in sodium silicate solid 2with Na 2the mass ratio of O is between 2 and 4, and preferred value is between 3.0 and 3.7.The quality of sodium silicate solid and the mass ratio of water are between 2:1 and 3:1, and preferred value is 2:1.Pass into the pressure > 0.3Mpa of water vapour.Dissolution time is between 1.5 hours and 3 hours, and preferred value is between 1.5 hours and 2.5 hours.The density of the water glass strong solution formed is between 1.01g/cm 3and 1.40g/cm 3between, preferred value is between 1.1g/cm 3and 1.3g/cm 3between.
In set-up procedure, the water glass strong solution obtained in dissolving step and water being joined adjusts in tank, thus regulate the solubility of sodium silicate solution between 1.0mol/L and 3.0mol/L, preferred value is between 1.5mol/L and 2.5mol/L, and further preferred value is between 2.0mol/L and 2.5mol/L.
The initial size size to fit of the silicon-dioxide prepared by method provided by the invention, with good dispersity during compounding rubber; And when using as supporting material, obviously can reduce abrasion and the heat-dissipating of rubber product, and the tensile strength at yield of the remarkable Reinforced Rubber product of energy, tensile yield and tear strength.
Accompanying drawing explanation
Fig. 1 is the method flow diagram preparing silicon-dioxide according to embodiments of the invention 1;
Fig. 2 is the method flow diagram preparing silicon-dioxide according to embodiments of the invention 2;
Fig. 3 is the method flow diagram preparing silicon-dioxide according to embodiments of the invention 3.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.Illustrated preferred embodiment is only for illustration of technical scheme of the present invention, and non-limiting the present invention.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, all belongs to the scope of protection of the invention.
The detailed process using production technique of the present invention to prepare easily disperse silicon-dioxide is described below by specific embodiment.And the silicon-dioxide prepared by the present invention is processed into further rubber product to compare with contrast product.
Embodiment 1: the preparation of silicon-dioxide S1
1) dissolve: as shown in S102 in Fig. 1, sodium silicate solid (Anhui Que Cheng chemistry of silicones company limited: Gu-2 types) and water are added in dissolving static pressure kettle according to the mass ratio of 2:1, pass into the water vapour that pressure is 0.4Mpa, abundant dissolving 1.5 hours, obtain transparent pure concentrated liquid water glass after leaching throw out with pressure filter, its density (20 DEG C) is 1.1g/cm 3;
Wherein in sodium silicate solid, SiO 2/ Na 2the weight ratio 3.35 of O;
2) regulate: as shown in S104 in Fig. 1, in the concentrated liquid water glass obtained by step 1), add water, to adjust wherein Na 2onSiO 2concentration obtain dilute liquid water glass to 2.20mol/l;
3) synthesize: as shown in S106 in Fig. 1, in advance in reactor (request for utilization number disclosed in the precipitation reactor of 201220391123.9 production silicon-dioxide reactor), add appropriate water and by step 2) the dilute liquid water glass (the volume summation of the water added and dilute liquid water glass accounts for 40% of reactor cumulative volume) that obtains, ensure that pH value is 10.1.Be under the condition of 20rpm in stir speed (S.S.), by by step 2) the dilute liquid water glass that obtains and mass concentration be 98.2% sulfuric acid add in synthesis reaction vessel according to the volume ratio of 16.3:1 simultaneously, pass into water vapour simultaneously, control vapor pressure is 0.4Mpa, 85min is reacted at the temperature of 75 DEG C, it is 9.2 that reaction terminates material pH value, stops adding dilute liquid water glass.Continue to drip sulfuric acid and pH value is adjusted to 4.0, obtain rare silica slurry;
Reaction equation is as follows:
Na 2O·nSiO 2+H 2SO 4→nSiO 2·H 2O+Na 2SO 4
4) filter: as shown in S108 in Fig. 1, pressure filter is used to filter rare silica slurry that step 3) obtains, first charging 13 minutes under the pressure of 0.45Mpa, then wash under the pressure of 0.65Mpa, repeated washing, until washing water specific conductivity is that 8000 μ s/cm are with removing impurity Na wherein 2sO 4, form much filtrate, the solid content in much filtrate be 22.2%, sulphate content 2.0%;
5) pulp: as shown in S110 in Fig. 1, much filtrate step 4) obtained adds in pulp tank by rotary conveyor, and the shearing rate of setting hollander impeller is 150rpm, much filtrate is broken into the liquid of the pulpous state of mobility, control viscosity is 600cp, obtains silica slurry.
6) dry: as shown in S112 in Fig. 1, silica slurry water pump step 5) obtained is delivered to drying tower pressure type drying plant and carried out spraying dry, set spray-dired temperature in drying tower is 600 DEG C simultaneously, obtains silicon-dioxide S1.
Embodiment 2: the preparation of silicon-dioxide S2
1) dissolve: as shown in S202 in Fig. 2, sodium silicate solid (Anhui Que Cheng chemistry of silicones company limited: Gu-2 types) and water are added in dissolving static pressure kettle according to the mass ratio of 2:1, pass into the water vapour that pressure is 0.4Mpa, abundant dissolving 2.0 hours, obtain transparent pure concentrated liquid water glass after leaching throw out with pressure filter, its density (20 DEG C) is 1.3g/cm 3;
Wherein in sodium silicate solid, SiO 2/ Na 2the weight ratio 3.40 of O;
2) regulate: as shown in S204 in Fig. 2, in the concentrated liquid water glass obtained by step 1), add water, to adjust wherein Na 2onSiO 2concentration obtain dilute liquid water glass to 2.35mol/l;
3) synthesize: as shown in S206 in Fig. 2, in advance in reactor (request for utilization number disclosed in the precipitation reactor of 201220391123.9 production silicon-dioxide reactor), add appropriate water and by step 2) the dilute liquid water glass (the volume summation of the water added and dilute liquid water glass accounts for 45% of reactor cumulative volume) that obtains, ensure that pH value is 10.4.Be under the condition of 25rpm in stir speed (S.S.), by by step 2) the dilute liquid water glass that obtains and mass concentration be 98.4% sulfuric acid add in synthesis reaction vessel according to the volume ratio of 16.5:1 simultaneously, pass into water vapour simultaneously, control vapor pressure is 0.4Mpa, 90min is reacted at the temperature of 85 DEG C, it is 9.6 that reaction terminates material pH value, stops adding dilute liquid water glass.Continue to drip sulfuric acid and pH value is adjusted to 4.5, obtain rare silica slurry;
Reaction equation is as follows:
Na 2O·nSiO 2+H 2SO 4→nSiO 2·H 2O+Na 2SO 4
4) filter: as shown in S208 in Fig. 2, pressure filter is used to filter rare silica slurry that step 3) obtains, first charging 15 minutes under the pressure of 0.6Mpa, then wash under the pressure of 0.7Mpa, repeated washing, until washing water specific conductivity is that 6000 μ s/cm are with removing impurity Na wherein 2sO 4, form much filtrate, the solid content in much filtrate be 23.6%, sulphate content 1.5%;
5) pulp: as shown in S210 in Fig. 2, much filtrate step 4) obtained adds in pulp tank by rotary conveyor, and the shearing rate of setting hollander impeller is 200rpm, much filtrate is broken into the liquid of the pulpous state of mobility, control viscosity is 700cp, obtains silica slurry.
6) dry: as shown in S212 in Fig. 2, silica slurry water pump step 5) obtained is delivered to drying tower pressure type drying plant and carried out spraying dry, in setting drying tower, spray-dired temperature is 500 DEG C, obtains silicon-dioxide S2.
Embodiment 3: the preparation of silicon-dioxide S3
1) dissolve: as shown in S302 in Fig. 3, sodium silicate solid (Anhui Que Cheng chemistry of silicones company limited: Gu-2 types) and water are added in dissolving static pressure kettle according to the mass ratio of 2:1, pass into the water vapour that pressure is 0.4Mpa, abundant dissolving 2.2 hours, obtain transparent pure concentrated liquid water glass after leaching throw out with pressure filter, its density (20 DEG C) is 1.2g/cm 3;
Wherein in sodium silicate solid, SiO 2/ Na 2the weight ratio 3.34 of O;
2) regulate: as shown in S304 in Fig. 3, in the concentrated liquid water glass obtained by step 1), add water, to adjust wherein Na 2onSiO 2concentration obtain dilute liquid water glass to 2.37mol/l;
3) synthesize: as shown in S306 in Fig. 3, in advance in reactor (request for utilization number disclosed in the precipitation reactor of 201220391123.9 production silicon-dioxide reactor), add appropriate water and by step 2) the dilute liquid water glass (the volume summation of the water added and dilute liquid water glass accounts for 51% of reactor cumulative volume) that obtains, ensure that pH value is 10.7.Be under the condition of 22rpm in stir speed (S.S.), by by step 2) the dilute liquid water glass that obtains and mass concentration be 98.3% sulfuric acid add in synthesis reaction vessel according to the volume ratio of 16.6:1 simultaneously, pass into water vapour simultaneously, control vapor pressure is 0.4Mpa, 90min is reacted at the temperature of 90 DEG C, it is 9.8 that reaction terminates material pH value, stops adding dilute liquid water glass.Continue to drip sulfuric acid and pH value is adjusted to 4.4, obtain rare silica slurry;
Reaction equation is as follows:
Na 2O·nSiO 2+H 2SO 4→nSiO 2·H 2O+Na 2SO 4
4) filter: as shown in S308 in Fig. 3, pressure filter is used to filter rare silica slurry that step 3) obtains, first charging 15 minutes under the pressure of 0.5Mpa, then wash under the pressure of 0.7Mpa, repeated washing, until washing water specific conductivity is that 5000 μ s/cm are with removing impurity Na wherein 2sO 4, form much filtrate, the solid content in much filtrate be 23.4%, sulphate content 1.4%;
5) pulp: as shown in S310 in Fig. 3, much filtrate step 4) obtained adds in pulp tank by rotary conveyor, and the shearing rate of setting hollander impeller is 250rpm, much filtrate is broken into the liquid of the pulpous state of mobility, control viscosity is 700cp, obtains silica slurry.
6) dry: as shown in S312 in Fig. 3, silica slurry water pump step 5) obtained is delivered to drying tower pressure type drying plant and carried out spraying dry, in setting drying tower, spray-dired temperature is 400 DEG C, obtains silicon-dioxide S3.
Carry out test chemical to three crowdes of silicon-dioxide S1, S2 and S3 prepared by above 3 embodiments respectively according to the testing method of HG/T3061-2009 " rubber ingredients precipitated hydrated silica ", test result is in table 1.By 500,000 times of electronic transmission electron microscopic observation silicon-dioxide initiating particle sizes, according to the pore volume of the testing method test silicon-dioxide of ISO15901-1:2005.
Table 1
Above 3 embodiments are prepared three crowdes of silicon-dioxide S1, S2 and S3 and be respectively 1#, 2# and 3# from the numbering that H company buys three batches of HC SIL-833MP type silicon-dioxide as a comparison product according to the method recorded in 5.2 lower mill mixing steps in HG/T2404-2008 (qualification of rubber ingredients precipitated hydrated silica butadiene-styrene rubber), use mill to be prepared into silica product (rubber item) respectively.Then, 6 batches of silica products are worn away, tensile strength at yield, heat-dissipating, tensile yield, tear strength properties test.
Testing method:
Abrasion: use Akron abrasion machine, the mensuration according to GB/T1689-1998(vulcanized rubber wear resisting property) the middle method recorded;
Tensile strength at yield: use tension testing machine, according to the method recorded in ASTM D412-1998A;
Heat-dissipating: use compression heat generation instrument, according to the method recorded in ASTM D623-1999;
Tensile yield: use tension testing machine, according to the method recorded in ASTM D412-1998A;
Tear strength: use stretching testing machine, according to the method recorded in ISO34-1-2010.Test result:
The mechanical and physical performance parameter of the different silica product of table 2
Known by data in table 2, compared with contrast product, when silicon-dioxide obtained in embodiment 1-3 and compounding rubber, its dispersed tool is significantly improved, thus makes to use silicon-dioxide provided by the invention to be applied in rubber product and have the advantages such as abrasion are low, tensile strength at yield is high, heat-dissipating is little, tensile yield is large, tear strength.It can thus be appreciated that, the dispersing property of the product silicon-dioxide using the preparation technology of easily disperse silicon-dioxide provided by the invention to make to prepare is better, can be better mixing with rubber, decrease the energy consumption in mixing process, and heat-dissipating, the abrasion of silica slurry and compounding rubber resulting product can be reduced significantly.
It is to be understood that foregoing invention content and embodiment are intended to the practical application proving technical scheme provided by the present invention, should not be construed as limiting the scope of the present invention.Those skilled in the art in spirit of the present invention and principle, when doing various amendment, equivalent replace or improve.Protection scope of the present invention is as the criterion with appended claims.

Claims (10)

1. a preparation method for silicon-dioxide, is characterized in that, comprises the following steps:
With water dissolution sodium silicate solid Na 2onSiO 2to form described sodium silicate solution, and by the concentration adjustment of described sodium silicate solution be between 2.0mol/L and 2.5mol/L;
In a kettle., sodium silicate solution and sulfuric acid are reacted, obtains silica slurry; Be specially: add in described reactor by the mixed solution of the water of the first volume and described sodium silicate solution, the pH value of described mixed solution is between 9.5 and 10.5, and described first volume is between 40% and 50% of described reactor volume; Stir speed (S.S.) is between 15rpm and 30rpm; After the mixed solution of the water of the first volume and described sodium silicate solution is added the step of described reactor, under the condition of water vapour heating that pressure is greater than 0.3MPa, add the described sodium silicate solution of volume ratio between 16:1 and 17:1 and described sulfuric acid in described reactor simultaneously, described sodium silicate solution and described sulfuric acid are reacted at the temperature between 70 DEG C and 100 DEG C, wherein, concentration >=98% of described sulfuric acid;
Duration of the reaction between 80 minutes and 90 minutes, or when the pH value of described silica slurry is between 7 and 10 reaction terminating;
After described reaction terminating, drip sulfuric acid and regulate the pH value of described silica slurry between 4.0 and 5.0;
Filter described silica slurry and obtain much filtrate;
Utilize hollander to carry out pulp to described much filtrate, the shearing rate of described hollander, between 150rpm and 250rpm, obtains the silica slurry of viscosity at below 1000cp; And
Dry described silica slurry;
Wherein, implemented the step of dry described silica slurry in pressure type drying tower by spray-dired mode, the inlet temperature of described pressure type drying tower is between 400 DEG C and 700 DEG C, and temperature out is between 80 DEG C and 150 DEG C.
2. according to the preparation method described in claim 1, it is characterized in that, described sodium silicate solution and described sulfuric acid are carried out in the step of reacting, and stir speed (S.S.) is between 20rpm and 25rpm.
3. according to the preparation method described in claim 1, it is characterized in that, the viscosity of described silica slurry is between 400cp and 800cp.
4. according to the preparation method described in claim 1, it is characterized in that, the viscosity of described silica slurry is between 600cp and 800cp.
5. according to the preparation method described in claim 1, it is characterized in that, use pressure filter to implement to filter described silica slurry and the step obtaining much filtrate.
6. preparation method according to claim 5, is characterized in that, in the step of filtering described silica slurry, the pressure of described pressure filter is between 0.4MPa and 0.6MPa; Implement the time of press filtration between 12 minutes and 17 minutes.
7. preparation method according to claim 1, is characterized in that, implements to dissolve described sodium silicate solid to form the step of described sodium silicate solution in static pressure kettle.
8. the preparation method according to claim 1 or 7, is characterized in that, described dissolved solids water glass comprises further with the operation forming sodium silicate solution:
Make mass ratio be that the sodium silicate solid of 2:1 and water fully dissolve under water vapour pressure is greater than the condition of 0.3MPa, dissolution time, between 1.5 hours and 2.5 hours, forms water glass just liquid; And in pressure filter, filter the first liquid of described water glass to form sodium silicate solution.
9. preparation method according to claim 1, is characterized in that, in described sodium silicate solid, and SiO 2with Na 2the mass ratio of O is between 3.0:1 and 3.7:1.
10. preparation method according to claim 1, is characterized in that, in adjustment tank, implement the step regulating described sodium silicate solution concentration.
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