CN104418330B - A kind of silica slurry and preparation method thereof - Google Patents
A kind of silica slurry and preparation method thereof Download PDFInfo
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- CN104418330B CN104418330B CN201310374813.2A CN201310374813A CN104418330B CN 104418330 B CN104418330 B CN 104418330B CN 201310374813 A CN201310374813 A CN 201310374813A CN 104418330 B CN104418330 B CN 104418330B
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Abstract
The invention provides a kind of Aerosil 200 serosity and preparation method thereof, method comprises the following steps: use sulphuric acid and sodium silicate solution to react generation silica slurry；Filter described silica slurry and obtain much filtrate；And described much filtrate pulp is obtained silica slurry, wherein, described silica slurry there was added high molecular reactive agent.By the said method of the present invention, it is possible to increase dispersibility when silica slurry and compounding rubber.The method can also significantly reduce silica slurry and the heat of compounding rubber resulting product, abrasion.Additionally, be effectively improved silica slurry and the tearing strength of compounding rubber resulting product, breaking strength, elongation at break etc. by the method.
Description
Technical field
The present invention relates to chemical production technical field, it particularly relates to a kind of silica slurry and
Its preparation method.
Background technology
Hydrated SiO 2 (silica slurry) mode of appearance is powdery, microballon, graininess, again
Claiming white carbon, the method manufacturing white carbon in prior art is mainly the sedimentation method and vapor phase method.Vapor phase method
It is that (particle diameter is little for the cotton-shaped translucent solid colloidal nanoparticle of white-amorphous under the white carbon normality produced
In 100nm), nontoxic, there is huge specific surface area, this type of method white carbon is entirely nano-silica
SiClx, product purity is up to 99%, and particle diameter is up to 10～20nm, but complicated process of preparation, price is held high
Expensive；The sedimentation method are divided into again the tradition sedimentation method and special precipitation.
The application of white carbon is quite varied, such as, can apply to agricultural chemical, dailyization
In work goods, cementing agent, anti-caking agent, papermaking filler and rubber.Due to energy-saving and emission-reduction with
The requirement of environmental protection, increasing white carbon is applied to rubber for tire industry.Silicon dioxide is made
Mixing with natural gum and rubber polymer for filler, it is applied to tire and can reduce resistance to rolling, improve wet and slippery
Performance, thus make automobile oil consumption low, reduce waste gas discharge.
White carbon is applied in tire be used in natural rubber as the filler of rubber or synthetic rubber is made
Adhesive in, it is provided that thixotropy and reinforcing.Can improve goods wearability, tear-resistant by force
Degree and hardness.Prior art provides a kind of method manufacturing white carbon, the step bag of this method
Include: dilute sodium silicate solution is joined in reactor by (a)；B sulphuric acid is joined dilute sodium silicate by ()
Solution reacts；C reacted mixed solution is stood by () so that it is aging, forms crystal seed；(d)
Mixed solution after aging is stirred；E high-temperature vapor is passed through in mixed solution and adds by ()
Heat, until solution temperature is heated to 70 DEG C～80 DEG C, adds dilute sodium silicate until solution pH value is
11.0～11.5；F high-temperature vapor is passed through in the solution in reactor and heats, when solution temperature by ()
When degree is heated to 86 DEG C～95 DEG C, stops being passed through high-temperature water vapor, and sulphuric acid is added in solution；(g)
It is 3.0～5.0 to be to have precipitate to separate out when the pH value of solution；(h) by precipitate through filter, making beating
Form finished product.But the white carbon that the sedimentation method involved in prior art manufacture and compounding rubber dispersion
Property poor, the heat of goods is high, abrasion height, bad mechanical property.
Summary of the invention
For prior art makes silica slurry and the problem of compounding rubber bad dispersibility, this
A kind of method preparing silica slurry of bright proposition, the method includes:
A () is reacted: use sulphuric acid and sodium silicate solution to react generation silica slurry；
B () filters: filtered silica slip also obtains much filtrate；
(c) pulp: described much filtrate pulp is obtained silica slurry, wherein, described silica slurry
Liquid there was added high molecular reactive agent.
In said method, it is accomplished by above-mentioned steps:
In reactions steps, in reactor, first add the water of the first volume and the mixed of sodium silicate solution
Close solution.Reactor is heated by steam, and temperature controls between 70 DEG C and 100 DEG C.If it is anti-
Answer temperature too low, the particle diameter of silicon dioxide ultimately generated can be made excessive, thus can be at follow-up dioxy
Affecting the dispersion of silicon dioxide in the mixing process of SiClx serosity and rubber, impact is final mixed further
The mechanical performance etc. of refined product, therefore should control reaction temperature between 70 DEG C and 100 DEG C.To steam
The pressure of vapour is set to 0.3Mpa；And the stir speed (S.S.) of reactor is set between 15rpm and
Between 30rmp, preferred value is between 20rpm and 25rmp.First volume is between reactor volume
30% and 60% between, preferred value is between 40% and 50%.
Then in reactor, add the sulphuric acid of the second volume and the sodium silicate solution of third volume simultaneously.
The ratio of the second volume and third volume is between 16:1 and 17:1.The sodium silicate solution used
Ph value is between 9.0 and 11.0, and preferred value is between 9.5 and 10.5；Reaction is used
Concentration >=98% of sulphuric acid.When reaction is between 70 minutes and 100 minutes, and preferred value is between 80 points
Between clock and 90 minutes or pH value >=7 of mixed solution of reaction, preferred value is between 7 and 10
Time, reaction stops.
After reaction stops, the mixed reaction solution in reactor drips sulphuric acid to regulate pH value.
So that the pH value of mixed reaction solution is between 2.5 and 6.0, preferred value between 3.5 and 6.0 it
Between, further preferably between 4.0 and 5.0.Owing to this reaction belongs to acid-base neutralization reaction, pass through
Mixed reaction solution in regulation reactor, to acid, can make reaction carry out completely.
In filtration step, use pressure filter to implement filtration step, set pressure filter pressure between 0.3Mpa
With between 0.8Mpa, preferred value is between 0.4Mpa and 0.6Mpa, and the time implementing to filter is situated between
Between 10 minutes and 20 minutes, preferred value is between 12 minutes and 17 minutes.Filtration step
Farther include washing step, use pressure filter to implement washing step.In washing step, set filter pressing
Machine pressure is between 0.5Mpa and 0.8Mpa, and preferred value is between 0.6Mpa and 0.8Mpa.
Repeat washing step to remove the impurity (sodium sulfate) in much filtrate, until the washing after Xi Di
Electrical conductivity of water ＜ 10000 μ s/cm.After filtration and washing step, form much filtrate, much filtrate
Content≤3.0% of middle sulfate；And the solid content of much filtrate is between 15.0% and 30.0%, preferably
Value is between 20.0% and 25.0%.
In slurry step, belt conveyor is used to be sent to the much filtrate formed in filtration step beat
In pulp grinder, through the high speed shear effect of beater impeller, much filtrate is slurried into the pulpous state of mobility
Liquid (silica slurry).The viscosity of silica slurry between 100cp and 1000cp,
Preferred value is between 400cp and 800cp, and further preferably value is between 600cp and 800cp.
Can be before mashing step, at least one situation in mashing step or after mashing step
Add high molecular reactive agent.Added before mashing step in the case of high molecular reactive agent, by high score
Sub-activating agent and much filtrate are simultaneously introduced in beater, are formed containing macromolecule by above-mentioned slurry step
The silica slurry of activating agent；Mashing step adds in the case of high molecular reactive agent, first makes
Implement the pulp to much filtrate with beater, be subsequently adding high molecular reactive agent, re-use beater complete
The pulp of much filtrate in pairs；Add after mashing step in the case of high molecular reactive agent, will making beating
The silica slurry formed in step and high molecular reactive agent join in agitator, stir 30 points
Clock, ultimately forms silica slurry finished product.High molecular reactive agent is cationic high-molecular activating agent,
Preference is amino alkyl acrylates copolymer, modified polyethyleneimine, propylene containing quaternary ammonium salt
Acid amide copolymer, polystyrene methyl trimethoxy ammonium salt, further preferred polystyrene methyl trimethoxy ammonium
Salt.High molecular reactive agent the ratio of quality and the gross mass of high molecular reactive agent and silica slurry
Between 3 ‰ and 10 ‰, preferred value is 8 ‰.
High molecular reactive agent is a class of surfactant, its molecule formed by two kinds of different particles,
A kind of particle has an extremely strong lipophile, another kind of then have extremely strong hydrophilic.Lived by macromolecule
In property agent molecule, affine respectively for biphase (water, oil) of different piece, makes biphase all by macromolecule
The composition of this phase regarded as by activating agent, and high molecular reactive agent molecule arranges between the two phases, makes biphase table
Face proceeds to intramolecule.Thus reduce by two alternate surface tension.Due to biphase all by high molecular reactive
A component of this phase is regarded in agent as, and biphase and surfactant molecule is all formed without interface, the most quite
Eliminate two alternate interfaces in part in this way, thus reduce surface tension and surface
Free energy.Due to surface tension and the reduction of surface free energy, improve the solubility of organic compound.
Utilize this amphipathic characteristic and the emulsification of surfactant, promote that surfactant is evenly coated at
Silica particles, stops silica dioxide granule to be reunited, reduces the particle diameter of silica dioxide granule,
Improve silica slurry dispersibility in the organic medias such as latex, thus play silica slurry
Solubilization when being blended with latex.In the step that follow-up silica slurry and latex are blended, two
The dispersion of silicon oxide is improved, thus ultimately increases the mechanical performance that glue is dry mixed made with resistance to
Abrasion ability.Amino alkyl acrylates copolymer, modified polyethyleneimine, containing inspection propylene
Acid amide copolymer, polystyrene methyl trimethoxy ammonium salt are respectively provided with above-described high score subclass activating agent
Advantage.
In the method for the present invention, it is also possible to added dissolving step and set-up procedure before reactions steps.
In dissolving step, static pressure kettle is placed sodium silicate solid (Na2O·nSiO2) and water, and be passed through
Steam, forms sodium silicate solution within a certain period of time, obtains transparent after leaching precipitate (impurity)
Pure sodium silicate concentrated solution.In dissolving step, SiO in sodium silicate solid2With Na2The matter of O
Amount ratio is between 2 and 4, and preferred value is between 3.0 and 3.7.The quality of sodium silicate solid and water
Mass ratio between 2:1 and 3:1, preferred value is 2:1.It is passed through the pressure ＞ 0.3Mpa of steam.
Dissolution time is between 1.5 hours and 3 hours, and preferred value is between 1.5 hours and 2.5 hours.
Pressure filter is used to implement the operation of impurity screening.Formed sodium silicate concentrated solution density between
1.01g/cm3And 1.40g/cm3Between, preferred value is between 1.1g/cm3And 1.3g/cm3Between.
In set-up procedure, the sodium silicate concentrated solution obtained in dissolving step and water are joined adjustment tank
In, thus regulating the solubility of sodium silicate solution between 3.0 and 3.7, preferred value is between 1.5mol/L
With between 2.5mol/L, further preferably value is between 2.0mol/L and 2.5mol/L.
Present invention also offers a kind of silica slurry, including:
The silicon dioxide of 20.0% to 25.0%；
High molecular reactive agent between 3 ‰ to 10 ‰；And
Remaining is water.
Wherein, high molecular reactive agent include amino alkyl acrylates copolymer, modified polyethyleneimine,
Acrylic acid amides copolymer containing quaternary ammonium salt or polystyrene methyl trimethoxy ammonium salt.And high molecular reactive
The preferred value of agent is 8 ‰.
By the said method of the present invention, it is possible to increase silicon dioxide is at silica slurry with rubber altogether
Dispersibility time mixed.And then, the method can also significantly reduce silica slurry and compounding rubber institute
Obtain the heat of goods, abrasion.Additionally, be effectively improved silica slurry and rubber by the method
The tearing strength of mixing resulting product, breaking strength, elongation at break etc..
Accompanying drawing explanation
Fig. 1 is the flow chart of the technique for manufacturing silicon dioxide according to some embodiments.
Detailed description of the invention
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 entered
Row clearly and completely describes, it is clear that described embodiment is only a part of embodiment of the present invention,
Rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are obtained
The every other embodiment obtained, broadly falls into the scope of protection of the invention.
As shown in S102 in Fig. 1, by sodium silicate solid (wherein, the weight ratio of SiO2 Yu Na2O
It is 3.5) it is dissolved in water in static pressure kettle, the quality of the water added and the mass ratio of sodium silicate solid
For 1:2.Course of dissolution continues 2 hours, and is passed through the pressure water steaming more than 0.3Mpa in static pressure kettle
Gas.Then the sodium silicate solution after using pressure filter to dissolve filters, and obtaining density is 1.2g/cm3
Sodium silicate concentrated solution.As shown in S104 in Fig. 1, sodium silicate concentrated solution is added and adjusts in tank, and
Add water the concentration of sodium silicate is adjusted to 2.0mol/L.
As shown in S106 in Fig. 1, the water of the first volume is molten with the mixing of the sodium silicate solution configured
Liquid adds in reactor, and wherein the first volume is between the 45% of reactor volume.Use pressure is 0.3Mpa
Steam reactor is heated, it is 90 DEG C that the temperature of reactor controls；And the stirring of reactor
Speed is 20rpm.Water controls to be 10 with the pH value of the mixed solution of sodium silicate.Then it is simultaneously introduced
Sulphuric acid (concentration >=98%) and silicic acid and the sodium silicate solution configured, wherein sulphuric acid and sodium silicate solution
Volume ratio be 16:1.React 85 minutes in a kettle. or when the pH value of mixed reaction solution is 7,
Reaction terminating.After reaction terminates, use sulphuric acid that the pH value of mixed reaction solution is modulated to 4.5.Reflection
Step obtains dilute silica slurry after terminating.
As shown in S108 in Fig. 1, use pressure filter that silica slurry is filtered.First exist
Feed under the pressure of 0.5Mpa 15 minutes, then wash 45 minutes under the pressure of 0.7Mpa, control
Washings processed are less than 10000us/cm with former water conductivity difference, obtain much filtrate, containing in much filtrate
Gu amount is between 15% and 30%, such as 20%, 24% and 25% etc., and sulphates content≤3.0%.
The much filtrate transmission that belt conveyor obtains after filtering and wash is used as shown in S110 in Fig. 1
In pulp tank, through the high speed shear of beater impeller, much filtrate is broken into the pulpous state of mobility
Liquid, viscosity controls less than 1000cp such as 400cp, 500cp and 600cp etc., such as S112 in Fig. 1
Shown formation silica slurry.
Can be before mashing step, at least one situation in mashing step or after mashing step
Add polystyrene methyl trimethoxy ammonium salt.Polystyrene methyl trimethoxy ammonium salt was added before mashing step
In the case of, polystyrene methyl trimethoxy ammonium salt and much filtrate are simultaneously introduced in beater, by upper
State slurry step and form the silica slurry containing polystyrene methyl trimethoxy ammonium salt；At mashing step
In the case of middle addition polystyrene methyl trimethoxy ammonium salt, beater is first used to implement the slurry to much filtrate
Change, be subsequently adding polystyrene methyl trimethoxy ammonium salt, re-use beater and complete the pulp to much filtrate；
Add after mashing step in the case of polystyrene methyl trimethoxy ammonium salt, will mashing step be formed
Silica slurry and polystyrene methyl trimethoxy ammonium salt join in agitator, stir 30 minutes,
Ultimately form silica slurry finished product.
The present invention is further illustrated below by embodiment and comparative example.In following example and comparative example
In, all use method described in Publication No. CN102634083A, by what the present invention provided
Silica slurry obtained by method is blended with a kind of natural emulsion, obtains different rubbers.
Embodiment 1
Take prepared silica slurry (solid content is 25%, and viscosity is 400cp) 24.8 kilograms with
200 grams of polystyrene methyl trimethoxy ammonium salts are put into together in agitator and are blended.The silicon dioxide generated
Serosity finished product includes: the silicon dioxide of 25.0%, the high molecular reactive agent of 8 ‰, and remaining is water.
Then, as shown in S114 in Fig. 1, use described in Publication No. CN102634083A
Method and a kind of 20Kg natural emulsion gel content 60% carry out being blended, being dried, and finally give and be dry mixed
Glue.
Embodiment 2
Using method in the same manner as in Example 1 to prepare rubber, it the difference is that only:
In slurry step, the viscosity of the silica slurry finally given is 500cp；And solid content is 20%.
By 65.5 kilograms of silica slurries (solid content is 20%, and viscosity is 500cp) with 400 gram 12
Alkyl sodium sulfate is put into together in agitator and is blended, and the silica slurry finished product generated includes:
20.0% silicon dioxide, the high molecular reactive agent of 6.1 ‰, remaining is water.
Then use method described in Publication No. CN102634083A natural with a kind of 10Kg
Latex gel content 30% carries out being blended, is dried, and finally gives glue is dry mixed.
Embodiment 3
Using method in the same manner as in Example 1 to prepare rubber, it the difference is that only:
In slurry step, the viscosity of the silica slurry finally given is 500cp；And solid content is 24%.
By 79.7 kilograms of silica slurries (solid content is 24%, and viscosity is 500cp) with 300 gram 12
Alkyl sodium sulfate is put into together in agitator and is blended, and the silica slurry finished product generated includes:
20.0% silicon dioxide, the high molecular reactive agent of 3.8 ‰, remaining is water.
Then use method described in Publication No. CN102634083A natural with a kind of 10Kg
Latex gel content 30% carries out being blended, is dried, and finally gives glue is dry mixed.
Embodiment 4
Using method in the same manner as in Example 1 to prepare rubber, it the difference is that only:
In slurry step, the viscosity of the silica slurry finally given is 600cp；And solid content is 20%.
By 99.5 kilograms of silica slurries (solid content is 20%, and viscosity is 600cp) with 500 gram 12
Alkyl sodium sulfate is put into together in agitator and is blended, and the silica slurry finished product generated includes:
20.0% silicon dioxide, the high molecular reactive agent of 5 ‰, remaining is water.
Then method described in Publication No. CN102634083A and a kind of 5Kg genuine milk are used
Glue gel content 60% carries out being blended, is dried, and finally gives glue is dry mixed.
Comparative example 1
10kg natural emulsion (gel content 60% mass ratio) and 14.4kg silica slurry (are contained
Gu amount is 25%, viscosity 300cP) use method described in Publication No. CN102634083A
Carry out being blended, being dried, obtain glue is dry mixed.Silica slurry used in it only uses existing
The silica slurry being not added with high molecular reactive agent of technology manufacture.
The glue that is dry mixed obtained in embodiment 1-4 and comparative example is carried out following test.
Experimental technique 1
Use Akron abrasion machine, according to the method described in GB/T1689-1998, rubber is carried out
The test of abrasion.
Experimental technique 2
Use tensile testing machine, according to method described in ASTM D 412-1998A to rubber
Carry out the test of breaking strength and elongation at break.
Experimental technique 3
Use compression heat generation instrument, according to the method described in ASTM D 623-1999, rubber is entered
The test of row heat.
Experimental technique 4
Use stretching testing machine, according to the method described in ISO 34-1-2010, rubber is torn
The test of resistance to spalling.
Experimental result
More than test result indicate that, with the silica slurry not using method provided by the present invention to prepare
Comparative example compare, the titanium dioxide after the silica slurry and the blend rubber that prepare in embodiment 1-4
The dispersibility of silicon is significantly improved, and then makes the abrasion that glue is dry mixed prepared substantially drop with heat
Low, and compared with comparative example in embodiment 1-4 prepare the breaking strength of glue, elongation at break are dry mixed
And tearing strength is all significantly enhanced.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, all should wrap
Within being contained in protection scope of the present invention.
Claims (24)
1. the method preparing Aerosil 200 serosity, comprises the following steps:
Sulphuric acid and sodium silicate solution is used to react generation silica slurry；
Filter described silica slurry and obtain much filtrate；And
Described much filtrate pulp is obtained silica slurry, wherein, described silica slurry there was added high molecular reactive agent, wherein, the ratio of the quality of described high molecular reactive agent and the gross mass of high molecular reactive agent and silica slurry is between 3 ‰ and 10 ‰, beater is used to implement to obtain described much filtrate pulp the step of silica slurry, and in the step that described much filtrate pulp obtains silica slurry, the viscosity of described silica slurry is between 600cp and 800cp.
Method the most according to claim 1, it is characterised in that before to described much filtrate pulp, in described much filtrate slurrying process and at least one situation after described much filtrate pulp, add described high molecular reactive agent.
Method the most according to claim 1 and 2, it is characterised in that described high molecular reactive agent is cationic high-molecular activating agent.
Method the most according to claim 3, it is characterised in that described cationic high-molecular activating agent includes amino alkyl acrylates copolymer, modified polyethyleneimine, acrylic acid amides copolymer containing quaternary ammonium salt or polystyrene methyl trimethoxy ammonium salt.
Method the most according to claim 1, it is characterised in that the quality of described high molecular reactive agent is 8 ‰ with the ratio of the gross mass of high molecular reactive agent and silica slurry.
6., according to the method described in claim 2, it is characterised in that in the case of after to described much filtrate pulp, after adding described high molecular reactive agent, use agitator that described silica slurry is mixed with described high molecular reactive agent.
Method the most according to claim 6, it is characterised in that the mixing time of described agitator is 30 minutes.
Method the most according to claim 1, it is characterised in that described use sulphuric acid and sodium silicate solution react the step of generation silica slurry and further include steps of
Add the water of the first volume and the mixed solution of sodium silicate solution；And
It is simultaneously introduced the sulphuric acid of the second volume and the sodium silicate solution of third volume.
Method the most according to claim 8, it is characterized in that, after the step of the described sulphuric acid being simultaneously introduced the second volume and the sodium silicate solution of third volume, and the described described silica slurry of filtration and obtain much filtrate step before, farther include: dropping sulphuric acid regulates the pH value of described silica slurry.
Method the most according to claim 9, it is characterised in that reacting at described use sulphuric acid and sodium silicate solution in the step generating silica slurry, reaction temperature is between 70 DEG C and 100 DEG C；Described first volume is between 40% and 50% of reaction vessel volume；After described addition water and sodium silicate solution step, the pH value of described sodium silicate solution is between 9.5 and 10.5；The ratio of described second volume and described third volume is between 1:16 and 1:17；Concentration >=98% of described sulphuric acid；When the pH value of described silica slurry is between 7 and 10, reaction terminating or duration of the reaction are between 80 minutes and 90 minutes；And after the step of described dropping sulphuric acid regulation pH value, the pH value of described silica slurry is between 4.0 and 5.0.
11. according to the method according to any one of claim 1,8-10, it is characterised in that described use sulphuric acid and sodium silicate solution react the step of generation silica slurry to be carried out in a kettle..
12. methods according to claim 11, it is characterised in that described reactor is carried out steam heating；And the stir speed (S.S.) of described reactor is between 20rpm and 25rpm；Described steam-heated force value ＞ 0.3Mpa.
13. methods according to claim 1, it is characterised in that use pressure filter to implement filter described silica slurry and obtain the step of much filtrate, and filter described silica slurry and obtain the step of much filtrate and farther include:
Filter described silica slurry；
Wash described silica slurry；And
Silica slurry described in filter pressing also obtains much filtrate.
14. methods according to claim 13, it is characterised in that described in the step filtering described silica slurry, the pressure of described pressure filter is between 0.4Mpa and 0.6Mpa；Implement the time of filter pressing between 12 minutes and 17 minutes.
15. methods according to claim 13, it is characterised in that silica slurry step described in repeated washing is until washing electrical conductivity of water ＜ 10000 μ s/cm；The pressure of described pressure filter is between 0.6Mpa and 0.8Mpa.
16. methods according to claim 13, it is characterised in that silica slurry described in filter pressing and obtain much filtrate step after, the solid content of described much filtrate is between 20.0% and 25.0%, and content≤3.0% of sulfate in described much filtrate.
17. methods according to claim 1, it is characterised in that react the step generating silica slurry at described use sulphuric acid and sodium silicate solution before, also include: dissolved solid sodium silicate is to form sodium silicate solution.
18. methods according to claim 17, it is characterised in that described dissolved solid sodium silicate with formed sodium silicate solution step in, SiO in described sodium silicate solid2With Na2The weight ratio of O is between 3.0 and 3.7；Add water with dissolved solid sodium silicate；The quality of described sodium silicate solid is 2:1 with the mass ratio of described water；Dissolution time is between 1.5 hours and 2.5 hours；The density of described sodium silicate solution is between 1.1g/cm3And 1.3g/cm3Between.
19. according to the method described in claim 17 or 18, it is characterised in that described dissolved solid sodium silicate is implemented in dissolving static pressure kettle with the step forming sodium silicate solution.
20. methods according to claim 11, it is characterised in that be passed through water vapour in described dissolving static pressure kettle, wherein, the pressure ＞ 0.3Mpa of described water vapour.
21. methods according to claim 17, it is characterised in that described dissolved solid sodium silicate also includes with the step forming sodium silicate solution: filtering precipitate.
22. methods according to claim 21, it is characterised in that use pressure filter to implement described filtering precipitate step.
23. methods according to claim 17, it is characterised in that after the step of described dissolved solid sodium silicate and before described addition sulphuric acid and described sodium silicate react the step generating silicon dioxide, also include: regulation sodium silicate solution concentration.
24. methods according to claim 23, it is characterised in that implement the step of described regulation sodium silicate solution concentration in adjusting tank, and the concentration of sodium silicate solution is adjusted between 2.0mol/L and 2.5mol/L.
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| CN107140643A (en) * | 2017-04-24 | 2017-09-08 | 确成硅化学股份有限公司 | A kind of high reinforcement easily disperses the preparation method of white carbon |
| CN114634186B (en) * | 2020-12-16 | 2023-07-18 | 安徽进化硅纳米材料科技有限公司 | Preparation method of nano silicon dioxide dispersion liquid |
| CN113264531B (en) * | 2021-06-25 | 2024-03-19 | 福建省沙县金沙白炭黑制造有限公司 | Preparation method of granular feed additive silicon dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221393A (en) * | 1996-06-06 | 1999-06-30 | 罗狄亚化学公司 | Silica capable of being used in toothpaste composition |
| CN101417808A (en) * | 2008-12-08 | 2009-04-29 | 核工业理化工程研究院华核新技术开发公司 | Method for preparing silicon dioxide thickening agents for toothpaste |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221393A (en) * | 1996-06-06 | 1999-06-30 | 罗狄亚化学公司 | Silica capable of being used in toothpaste composition |
| CN101417808A (en) * | 2008-12-08 | 2009-04-29 | 核工业理化工程研究院华核新技术开发公司 | Method for preparing silicon dioxide thickening agents for toothpaste |
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