CN109319793A - A kind of preparation method of Gao Bibiao, high oil absorption white carbon black - Google Patents
A kind of preparation method of Gao Bibiao, high oil absorption white carbon black Download PDFInfo
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- CN109319793A CN109319793A CN201811338751.9A CN201811338751A CN109319793A CN 109319793 A CN109319793 A CN 109319793A CN 201811338751 A CN201811338751 A CN 201811338751A CN 109319793 A CN109319793 A CN 109319793A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/126—Preparation of silica of undetermined type
- C01B33/128—Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses the preparation methods of a kind of Gao Bibiao, high oil absorption white carbon black, this method comprises: being proportionally added into sodium silicate solution, quaternary ammonium salt and water into synthesis reactor, dilute sulfuric acid is added under heating, stirring condition, stop acid adding when solution appearance is slightly cloudy the precipitation of lenticular molecule, it is transferred to insulated and stirred after medial launder, it is spare；It repeats the above steps, but sodium silicate silicate is reduced, continue to heat up, increases stirring rate, uniformly rear acid adding simultaneously adds sodium metasilicate to material stirring, and the stock solution in medial launder is at the uniform velocity added, acid adding carries out synthetic reaction, so reacts by more precipitation, again through filters pressing, washing, white carbon black wet cake is obtained, is scattered in n-butanol, azeotropic drying is carried out and obtains final products.White carbon black specific surface area prepared by the present invention is up to 200~250m2/ g, oil factor is up to 3.00~3.50cm3/ g, for being easily dispersed in paint, stability is good, has good extinction performance.
Description
Technical field
The present invention relates to white carbon black technical field, it is specifically related to the preparation method of a kind of Gao Bibiao, high oil absorption white carbon black.
Background technique
Superfine silicon dioxide also known as white carbon black are a kind of important fine inorganic chemicals products, because its it is brilliant it is reinforcing,
The properties such as thickening property, extinction are widely used for rubber, plastics, coating, paint, ink, papermaking, medicine, pesticide, dailyization
Learn many fields such as articles.
Currently, the preparation method of white carbon black mainly has vapor phase method and liquid phase method.Wherein, vapor phase method is original using silicon halide
Material, product are directly obtained by gas phase, and there is no dry problems, therefore properties of product are fabulous, and powder granule is fine, are free of salt,
But it is big to consume the energy, and technology is complicated, valuable product.And liquid phase method, although low in cost, product quality is poor, wherein making
It for the white carbon black product of paint delustering agent, even more requires have higher oil factor and specific surface area, therefore develops one kind
It is low in cost, it prepares Gao Bibiao, the method for high oil absorption value white carbon black product can promote the development in paint field, there is weight
Want meaning.
Summary of the invention
The purpose of the invention is to overcome the shortcomings of above-mentioned background technique, a kind of Gao Bibiao, high oil absorption hard charcoal are provided
Black preparation method, to promote dispersibility, extinction performance of the white carbon black in paint.
To achieve the above object, the present invention carries out multistep reaction using sodium metasilicate and sulfuric acid, dry through filters pressing, washing, azeotropic
Final products are obtained after dry, specifically, including following reaction step:
(1) sodium silicate solution is refined；
(2) sodium silicate solution of 0.3~0.5mol/L obtained by quaternary ammonium salt, water and step (1) is added in reaction kettle, is stirred
Mix, then be added dilute sulfuric acid react to solution occur it is slightly cloudy have lenticular molecule precipitation when, stop acid adding, generate at this time
It is white carbon black primary particle, material is transferred to medial launder, insulated and stirred is spare；
(3) content of step (2) is repeated in a kettle, but controls 0.1~0.15mol/L of sodium silicate silicate, reaction
There is lenticular molecule to stop acid adding when being precipitated to solution appearance is slightly cloudy, keeps the temperature；
(4) continue to heat up on the basis of step (3), stir, while medial launder in sodium silicate solution and step (2) is added
Sulfuric acid is added in the spare material of gained, stops that sodium silicate solution is added after reaction 1.5~2 hours, continuously adds sulfuric acid acidification, protect
Temperature ageing discharges after cooling to slurry vessel, is re-fed into filter press and carries out filters pressing, washing, obtains white carbon black wet cake；
(5) it dispersing white carbon black wet cake obtained by step (4) in n-butanol, heating carries out azeotropic drying, moisture is removed,
Up to Gao Bibiao, high oil absorption white carbon black.
Preferably, the method for step (1) the purification sodium silicate solution is that waterglass and water are added in static pressure dissolution kettle,
It is passed through water vapour, pressure maintaining is dissolved after pressurization, steam discharge, discharging to lye storage tank, takes supernatant liquor after precipitating, water is added to deploy, filter
Afterwards to obtain the final product.
Further, it is described purification sodium silicate solution method in waterglass be 3.4~3.5 moduluses solid water glass,
The hot water that water is 60~70 DEG C；Preferably, the quality of waterglass and water is 1:3~1:4.
Further, stop being passed through steam after being forced into 0.5~0.7MPa in the method for the purification sodium silicate solution, protect
Steam discharge after pressure solution solution 5~7 hours.
Preferably, the dosage of quaternary ammonium salt is sodium silicate solution quality 0.25-0.35% in the step (2), preferably
0.3%, the hot water that water is 45~55 DEG C；Still more preferably, the quaternary ammonium salt is cetyl trimethylammonium bromide.
It is further preferred that the rate stirred in the step (2) is 50~80r/min, the temperature of material is kept when stirring
Degree is 45~55 DEG C.
It is further preferred that the concentration of dilute sulfuric acid is 1.0-2.0mol/L in the step (2), and with 2.5m3The speed of/h
Rate is added.
Preferably, soaking time is 25~35 minutes, such as 30 minutes in the step (3).
Preferably, it is continuously heating to 80~90 DEG C in the step (4), controls 100~150r/min of stirring rate, simultaneously
Spare material obtained by medial launder is added in the sodium silicate solution and step (2) of 0.5~1.0mol/L.
It is further preferred that sulfuric acid concentration is 2.5~5.0mol/L in the step (4), control sulfuric acid is added rate and is
5m3/ hr, control reaction pH=9~10, stops after sodium silicate solution is added, continuously adds sulfuric acid and be acidified to pH=4~5.
Further, the conductivity of detection washing water obtains hard charcoal until it is lower than 1000uS/cm in the step (4)
Black wet cake.
Further, moisture can be removed substantially when temperature reaches 117 DEG C in the step (5).
Step (2), (3) middle quaternary ammonium salt that is added can be acted on fully with sodium metasilicate in the present invention, instead of in sodium metasilicate
Sodium ion, play the role of sealing end, prevent the further polymerization of primary particle；The acid adding side of sulfuric acid in step (2)-(4)
Formula is acid adding mode under symmetrical Multi-tube synchronous liquid；The azeotropic mixture of water and n-butanol is layered after condensing in step (5), on
Aqueous 8% or so in the n-butanol phase of layer, it can return in distillation system and reuse.
Gao Bibiao of the present invention, high oil absorption white carbon black preparation method acid-base precipitation reaction point multistep is carried out, sir
At the white carbon black primary particle of different-grain diameter as nucleus, it is then lifted out reaction speed, the parameters such as control pH value accelerate white carbon black
The formation of offspring can make white carbon black offspring have flourishing pore structure in this way, and mesoporous and macropore specific gravity rises；
It is played a protective role again using n-butanol as dispersing agent to the pore structure of offspring in the azeotropic drying stage, finally makes product
Obtain higher specific surface area and oil factor.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.Additional aspect and advantage of the invention will be set forth in part in the description, partially will be under
Become obvious in the description in face, or practice through the invention is recognized.It is only used to explain this hair it should be appreciated that being described below
It is bright, it is not intended to limit the present invention.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
To achieve the purpose of the present invention, it according to the summary of the invention of aforementioned present invention, a kind of Gao Bibiao of the present invention, high inhales
The preparation method of oil white carbon black may include following reaction step:
(1) purification of sodium silicate solution: by the solid water glass of 3.4~3.5 moduluses and 60~70 DEG C of hot water by 1:3~
The mass ratio of 1:4 is added in static pressure dissolution kettle, is passed through water vapour, stops being passed through steam after being forced into 0.5~0.7MPa, pressure maintaining is molten
It solves 5~7 hours, steam discharge, discharging to lye storage tank, takes supernatant liquor to be deployed into various concentration dilute alkaline soln after precipitating, after filtering
It is spare；In process water be added 98% the concentrated sulfuric acid be deployed into various concentration dilute sulfuric acid it is spare.
(2) by the sodium silicate solution of 0.3~0.5mol/L, the quaternary ammonium salt of sodium silicate solution quality 0.3%, 45~55 DEG C of heat
Water is proportionally added into reaction kettle, is set stirring rate as 50~80r/min, is kept the temperature of material at 45~55 DEG C, then
With 2.5m3The rate of/hr, which is added 1.0~2.0mol/L dilute sulfuric acid and reacts to solution appearance is slightly cloudy, the analysis of lenticular molecule
When out, stop acid adding, generating at this time is white carbon black primary particle, material is transferred to medial launder, insulated and stirred is spare；
(3) content of step (2) is repeated, but controls 0.1~0.15mol/L of sodium silicate silicate, reaction to solution occurs micro-
Muddiness stops acid adding when having the precipitation of lenticular molecule, and insulated and stirred 30 minutes；
(4) 80~90 DEG C are continuously heating to, controls 100~150r/min of stirring rate, while 0.5~1.0mol/L is added
Sodium silicate solution and step (2) in prepare solution, control sulfuric acid acid addition rate be 5m3/ hr, sulfuric acid concentration are adjusted to 2.5
~5.0mol/L, continues synthetic reaction, and control reaction pH=9~10 stop that sodium metasilicate is added after reaction 1.5~2 hours
Solution continuously adds sulfuric acid and is acidified to pH=4~5, and heat preservation ageing 30 minutes discharges to slurry vessel after cooling, is re-fed into filters pressing
Machine carries out filters pressing, washing, detects the conductivity of washing water, until it is lower than 1000uS/cm, obtains wet cake；
(5) it disperses white carbon black wet cake in n-butanol, heating carries out azeotropic drying, and temperature can base when reaching 117 DEG C
This removing moisture, obtains final products.
Moreover, technical characteristic involved in each embodiment of the present invention as long as they do not conflict with each other can
To be combined with each other.
Embodiment 1
A kind of Gao Bibiao of the present invention, high oil absorption white carbon black preparation method specific steps are as follows:
1, the purification of sodium silicate solution: by the solid water glass of 3.4~3.5 moduluses and 60~70 DEG C of hot water by 1:3~
The mass ratio of 1:4 is added in static pressure dissolution kettle, is passed through water vapour, stops being passed through steam after being forced into 0.5~0.7MPa, pressure maintaining is molten
It solves 5~7 hours, steam discharge, discharging to lye storage tank, takes supernatant liquor to be deployed into various concentration dilute alkaline soln after precipitating, after filtering
It is spare；
2, synthetic reaction: in 50m38m is added in reaction kettle3Hot water, while the silicic acid of deployed 0.4mol/L is added
Sodium solution 0.75m3, the cetyl trimethylammonium bromide of sodium silicate solution quality 0.3% sets stirring rate as 50r/min,
Keep the temperature of material at 50 DEG C or so, then with 2.5m3It is micro- muddy to solution appearance that 2mol/L sulfuric acid reaction is added in the rate of/hr
It is turbid have lenticular molecule precipitation when, stop acid adding, material is transferred to medial launder, insulated and stirred is spare；Again toward reaction
8m is added in kettle3Hot water, while the sodium silicate solution 0.75m of deployed 0.1mol/L is added3, sodium silicate solution quality
0.3% cetyl trimethylammonium bromide sets stirring rate as 50r/min, keeps the temperature of material at 50 DEG C or so, so
Afterwards with 2.5m3When the rate addition 2mol/L sulfuric acid reaction of/hr has lenticular molecule to be precipitated to solution appearance is slightly cloudy, stop
Only acid adding, constant temperature keep the temperature 30 minutes；85 DEG C are continuously heating to, sets stirring rate as 100r/min, while 0.7mol/L is added
Sodium silicate solution and medial launder in stock solution, control sulfuric acid acid addition rate be 5.0m3/ hr, sulfuric acid concentration are adjusted to
4.0mol/L carries out synthetic reaction, controls terminal pH=10, stops that sodium silicate solution is added after reaction 2 hours, continuously adds sulphur
Acid to pH=5, heat preservation ageing 30 minutes stops stirring, material is sent into slurry vessel after cooling；
3, filters pressing, washing: the grout reacted forms filter cake by plate and frame type filter-press filters pressing, washing, and detection is washed
The conductivity of water is washed, until it is lower than 1000 μ S/cm；
4, azeotropic drying: dispersing white carbon black wet cake in n-butanol, and heating carries out azeotropic drying, and temperature reaches 117
DEG C when can remove moisture substantially, obtain final products, wherein the azeotropic mixture of water and n-butanol temperature after condensing becomes room temperature,
N-butanol and water will be layered, and aqueous 8% or so in the n-butanol phase on upper layer, can be returned in distillation system and be reused.
Embodiment 2
A kind of Gao Bibiao of the present invention, high oil absorption white carbon black preparation method specific steps are as follows:
1, the purification of sodium silicate solution: by the solid water glass of 3.4~3.5 moduluses and 60~70 DEG C of hot water by 1:3~
The mass ratio of 1:4 is added in static pressure dissolution kettle, is passed through water vapour, stops being passed through steam after being forced into 0.5~0.7MPa, pressure maintaining is molten
It solves 5~7 hours, steam discharge, discharging to lye storage tank, takes supernatant liquor to be deployed into various concentration dilute alkaline soln after precipitating, after filtering
It is spare；
2, synthetic reaction: in 50m38m is added in reaction kettle3Hot water, while the silicic acid of deployed 0.35mol/L is added
Sodium solution 1.5m3, the cetyl trimethylammonium bromide of sodium silicate solution quality 0.3% sets stirring rate as 80r/min,
Keep the temperature of material at 50 DEG C or so, then with 2.5m3It is micro- to solution appearance that 1.5mol/L sulfuric acid reaction is added in the rate of/hr
Muddiness stops acid adding when having the precipitation of lenticular molecule, material is transferred to medial launder, insulated and stirred is spare；Again toward anti-
It answers and 8m is added in kettle3Hot water, while the sodium silicate solution 0.75m of deployed 0.15mol/L is added3, sodium silicate solution quality
0.3% cetyl trimethylammonium bromide sets stirring rate as 50r/min, keeps the temperature of material at 50 DEG C or so, so
Afterwards with 2.5m3When the rate addition 2mol/L sulfuric acid reaction of/hr has lenticular molecule to be precipitated to solution appearance is slightly cloudy, stop
Only acid adding, constant temperature keep the temperature 30 minutes；90 DEG C are continuously heating to, sets stirring rate as 150r/min, while 0.7mol/L is added
Sodium silicate solution and medial launder in stock solution, control sulfuric acid acid addition rate be 5.0m3/ hr, sulfuric acid concentration are adjusted to
4.0mol/L carries out synthetic reaction, controls terminal pH=10, stops that sodium silicate solution is added after reaction 2 hours, continuously adds sulphur
Acid to pH=5, heat preservation ageing 30 minutes stops stirring, material is sent into slurry vessel after cooling；
3, filters pressing, washing: the grout reacted forms filter cake by plate and frame type filter-press filters pressing, washing, and detection is washed
The conductivity of water is washed, until it is lower than 1000 μ S/cm；
4, azeotropic drying: dispersing white carbon black wet cake in n-butanol, and heating carries out azeotropic drying, and temperature reaches 117
DEG C when can remove moisture substantially, obtain final products, wherein the azeotropic mixture of water and n-butanol temperature after condensing becomes room temperature,
N-butanol and water will be layered, and aqueous 8% or so in the n-butanol phase on upper layer, can be returned in distillation system and be reused.
White carbon black product performance indicator made from both examples above and the white carbon black product of common process preparation are every
The testing result comparison of index is as shown in table 1:
The white carbon black product Testing index comparison of 1 different process of table preparation
| Testing index | Embodiment 1 | Embodiment 2 | Common process product |
| Specific surface area (m2/g) | 228 | 235 | 168 |
| Dioxide-containing silica (%) | 98.93 | 98.54 | 98.32 |
| DBP oil factor (cm3/g) | 3.35 | 3.40 | 2.55 |
| Average grain diameter (μm) | 30.84 | 31.25 | 15.04 |
| PH value | 6.3 | 6.2 | 6.3 |
Note: testing under the conditions of equivalent formulation, and common process preparation is our company ZH-906 type product.The type product
Preparation process is as follows:
(1) in 50m316m is added in reaction kettle3Hot water, while the sodium metasilicate that deployed 0.15-0.25mol/L is added is molten
Liquid 2.25m3, stirring rate is set as 80r/min, keeps the temperature of material at 50 DEG C or so, then with 2.5m3The rate of/hr adds
Enter 1.5mol/L sulfuric acid reaction has lenticular molecule to stop acid adding when being precipitated to solution appearance is slightly cloudy, and insulated and stirred 30 is divided
Clock；90 DEG C are continuously heating to, sets stirring rate as 150r/min, while the sodium silicate solution of 0.7mol/L is added, controls sulphur
Sour acid addition rate is 5.0m3/ hr, sulfuric acid concentration are adjusted to 4.0mol/L, carry out synthetic reaction, control terminal pH=10, reaction 2
Stop that sodium silicate solution is added after hour, continuously add sulfuric acid to pH=5, heat preservation ageing 30 minutes stops stirring, will after cooling
Material is sent into slurry vessel；
(2) filters pressing, washing: the grout reacted forms filter cake by plate and frame type filter-press filters pressing, washing, and detection is washed
The conductivity of water is washed, until it is lower than 1000uS/cm；
(3) expansion drying: white carbon black wet cake is passed through into screw feeder and is sent into flash drying equipment, controls inlet air temperature
480-500 DEG C, 70-75 DEG C of leaving air temp, dry products obtain final products after being crushed, being sieved.
From above-mentioned testing result: acid-base precipitation reaction point multistep being carried out, different temperature, concentration, charging are controlled
Rate and stirring rate are added quaternary ammonium salt, are initially formed the white carbon black primary particle of different-grain diameter as nucleus, are then lifted out reaction
Speed accelerates the formation of white carbon black offspring, white carbon black offspring can be made to have flourishing pore structure in this way, and mesoporous
Rise with macropore specific gravity；Protection is played to the pore structure of offspring using n-butanol as dispersing agent again in the azeotropic drying stage
Effect.Compared to the means of one-step synthesis and expansion drying in common process, the product of new process preparation obtains higher
Specific surface area and oil factor, can satisfy its application in paint.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. the preparation method of a kind of Gao Bibiao, high oil absorption white carbon black, which is characterized in that method includes the following steps:
(1) sodium silicate solution is refined；
(2) sodium silicate solution of 0.3~0.5mol/L obtained by quaternary ammonium salt, water and step (1) is added in reaction kettle, stirring, so
Be added afterwards dilute sulfuric acid react to solution occur it is slightly cloudy have the precipitation of lenticular molecule when, stop acid adding, generate at this time and be
Material is transferred to medial launder by white carbon black primary particle, and insulated and stirred is spare；
(3) content of step (2) is repeated in a kettle, but controls 0.1~0.15mol/L of sodium silicate silicate, is reacted to molten
Liquid appearance is slightly cloudy to have lenticular molecule to stop acid adding when being precipitated, and keeps the temperature；
(4) continue to heat up on the basis of step (3), stir, while being added in sodium silicate solution and step (2) obtained by medial launder
Sulfuric acid is added in material, stops that sodium silicate solution is added after reaction 1.5~2 hours, continuously adds sulfuric acid acidification, and heat preservation ageing is cold
But it is discharged afterwards to slurry vessel, is re-fed into filter press and carries out filters pressing, washing, obtain white carbon black wet cake；
(5) disperse white carbon black wet cake obtained by step (4) in n-butanol, heating carries out azeotropic drying, remove moisture to get
Gao Bibiao, high oil absorption white carbon black.
2. the preparation method of Gao Bibiao according to claim 1, high oil absorption white carbon black, which is characterized in that the step (1)
The method of purification sodium silicate solution is that waterglass and water are added in static pressure dissolution kettle, is passed through water vapour, and pressure maintaining is dissolved after pressurization,
Steam discharge, discharging take supernatant liquor after precipitating to lye storage tank, filter after adding water to deploy to obtain the final product.
3. the preparation method of Gao Bibiao according to claim 2, high oil absorption white carbon black, which is characterized in that the waterglass
For the solid water glass of 3.4~3.5 moduluses, the hot water that water is 60~70 DEG C；Preferably, the quality of waterglass and water be 1:3~
1:4。
4. the preparation method of Gao Bibiao according to claim 2 or 3, high oil absorption white carbon black, which is characterized in that the purification
Stop being passed through steam, steam discharge after pressure maintaining is dissolved 5~7 hours after being forced into 0.5~0.7MPa in the method for sodium silicate solution.
5. the preparation method of Gao Bibiao according to claim 1, high oil absorption white carbon black, which is characterized in that the step (2)
The dosage of middle quaternary ammonium salt is sodium silicate solution quality 0.25-0.35%, such as 0.3%, the hot water that water is 45~55 DEG C；Further
Preferably, the quaternary ammonium salt is cetyl trimethylammonium bromide；Still more preferably, the speed stirred in the step (2)
Rate is 50~80r/min, and it is 45~55 DEG C that the temperature of material is kept when stirring.
6. the preparation method of Gao Bibiao, high oil absorption white carbon black according to claim 1 or 5, which is characterized in that the step
(2) concentration of dilute sulfuric acid is 1.0-2.0mol/L in, and with 2.5m3The rate of/h is added.
7. the preparation method of Gao Bibiao according to claim 1, high oil absorption white carbon black, which is characterized in that the step (3)
Middle soaking time is 25~35 minutes, such as 30 minutes.
8. the preparation method of Gao Bibiao according to claim 1, high oil absorption white carbon black, which is characterized in that the step (4)
In be continuously heating to 80~90 DEG C, control 100~150r/min of stirring rate, while the sodium metasilicate of 0.5~1.0mol/L is added
Spare material obtained by medial launder in solution and step (2).
9. the preparation method of Gao Bibiao, high oil absorption white carbon black according to claim 1 or 8, which is characterized in that the step
(4) sulfuric acid concentration is 2.5~5.0mol/L in, and it is 5m that rate, which is added, in control sulfuric acid3/ hr, control reaction pH=9~10, stops
After sodium silicate solution is added, continuously adds sulfuric acid and be acidified to pH=4~5.
10. the preparation method of Gao Bibiao according to claim 1, high oil absorption white carbon black, which is characterized in that the step
(4) conductivity of detection washing water obtains white carbon black wet cake until it is lower than 1000 μ S/cm in；Preferably, the step
(5) moisture can be removed when temperature reaches 117 DEG C in substantially.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137901A (en) * | 2020-03-10 | 2020-05-12 | 福建省三明巨丰化工有限公司 | Preparation method of high-performance silicon dioxide |
| CN113652004A (en) * | 2021-09-27 | 2021-11-16 | 无锡恒诚硅业有限公司 | White carbon black for green tires and preparation method thereof |
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| CN111137901A (en) * | 2020-03-10 | 2020-05-12 | 福建省三明巨丰化工有限公司 | Preparation method of high-performance silicon dioxide |
| CN113652004A (en) * | 2021-09-27 | 2021-11-16 | 无锡恒诚硅业有限公司 | White carbon black for green tires and preparation method thereof |
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