CN1065440A - White carbon black prepared by solulion induced concentrated acid - Google Patents
White carbon black prepared by solulion induced concentrated acid Download PDFInfo
- Publication number
- CN1065440A CN1065440A CN 91102200 CN91102200A CN1065440A CN 1065440 A CN1065440 A CN 1065440A CN 91102200 CN91102200 CN 91102200 CN 91102200 A CN91102200 A CN 91102200A CN 1065440 A CN1065440 A CN 1065440A
- Authority
- CN
- China
- Prior art keywords
- carbon black
- white carbon
- water glass
- value
- sio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000006229 carbon black Substances 0.000 title claims abstract description 20
- 239000002253 acid Substances 0.000 title description 9
- 238000000034 method Methods 0.000 claims abstract description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 9
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000007171 acid catalysis Methods 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 235000019241 carbon black Nutrition 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
-
- 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
- C01P2006/10—Solid density
-
- 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
- C01P2006/11—Powder tap density
-
- 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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- 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
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Silicon Compounds (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a kind of method of producing white carbon black, use the vitriol oil and catalytic liquid, under certain temperature and pH value condition in and water glass obtain the white carbon black of excellent performance.Present method can the realization response condition optimal control, conservation is simplified production technique, shortens the reaction times, minimizing equipment and corrosion of pipe and pollution problem.Product whiteness is good, particle diameter is little, and specific surface area is big, and the pH value is 6.7～7.5, apparent density 0.18～0.21g/cm
3, true density 2g/cm
3, SiO
2Content＞90%, free water content≤6%, specific refractory power 1.45～1.46, oil-absorption(number) 2.4～2.7ml/g.
Description
The invention provides a kind of with in the sulphuric acid catalysis and the method for multiple use white carbon blacks such as water glass system rubber reinforcing filler, papermaking filler, paint matting agent.
The precipitator method are with in the diluted acid and water glass or sodium silicate solution a kind of method of producing white carbon black.(see GB2,169,129A; SU326,847).This method need be prepared dilute acid soln, uses sodium-chlor or sodium sulfate to make dispersion agent.Along with the continuous adding of acid, pH value is reduced to about 8 gradually by 12.Therefore, in this process, all there is the white carbon black precipitation to generate all the time, reduced product performance, prolonged the reaction times, generally need about 3 hours.Make the white carbon black of excellent performance, also need to select a kind of processing the in the following method: (1). add organic solvent after critical pressure force method or azeotropic distillation; (2). freeze-drying; (3). after additive polarity solvent and the non-polar solvent conventional processing, high-temperature activation again.
For improve this production method exist operation steps many, expend starting material, carry diluted acid corrosion pipeline and equipment, waste water not to meet disadvantages such as emission standard.Invented the method for white carbon black prepared by solulion induced concentrated acid.
The present invention is a catalytic liquid with the mother liquor of white carbon black, give heat after, with the vitriol oil with contain SiO
2Water glass be metered into and carry out neutralization reaction, its reaction formula is:
Wherein: m represents the modulus of water glass
N represents the molecule number of combination water
Like this, guarantee that white carbon black is to separate out at PH all the time at 7～9 o'clock.The add-on of water glass is 0.6～1.0 times of mother liquor volume, can guarantee the performance of product in the case, and the reaction times also is reduced to original 50%, and then, heating up keeps for some time, adds the vitriol oil again, makes the pH value of reaction solution continue to reduce to 2～4.Neutralization reaction finishes, and filters (mother liquor is standby), uses the hot wash product, drying, packing.
Whole technology is fairly simple.The technical indicator that makes white carbon black with this method is:
Outward appearance: white loose meal;
SiO
2Content:＞90%;
Water-content :≤6%;
Apparent density: 0.18～0.21 gram per centimeter
3;
PH value (100% suspension liquid): 6.7～7.5;
Calcination loss (950 ℃, 2 hours) :≤9%;
Oil-absorption(number): 2.4～2.7 milliliters/gram;
Particle diameter: 7～100nm;
Sodium ions content :≤1%;
Fe
2O
3Content :≤0.1%;
Specific surface area: 〉=250 meters
2/ gram;
Fineness: 200 screen residues 0%;
Specific refractory power: 1.45～1.46;
True density: 2 gram per centimeters
3;
The vitriol oil provided by the invention brings out in the solution and water glass system white carbon black, owing to used the vitriol oil, rather than preparation dilute acid soln, after handling routinely, needn't adopt freeze-drying again, critical pressure force method or azeotropic distillation and high-temperature activation are handled, thereby have simplified operation steps, have reduced equipment and corrosion of pipe.Neutralization reaction is to have utilized the mother liquor that last time prepares white carbon black to be catalytic liquid, thereby has special effect, does not need to add dispersion agent again, has so just saved former material, has shortened preparation technology's production cycle.Also because mother liquor is utilized, the pH value of washings just can reach national specified discharge standard more than 6, has overcome many shortcomings that the diluted acid neutralisation is brought.
Embodiment
The mother liquor of white carbon black as catalytic liquid, is given heat to 20～60 ℃, under agitation, add and contain SiO
2Concentration is 8～20% water glass, and making the pH value of solution is 7～9, is warmed up to and is no more than 70 ℃, is metered into the water glass and the vitriol oil of above-mentioned concentration more simultaneously, keeps the pH value of solution constant.The water glass add-on is 0.6～1.0 times of mother liquor volume, and the time is 20 minutes, and regulating pH value is 7～10, is warming up to 70～100 ℃, keeps 40 minutes.Then, add the vitriol oil again, making the pH value of solution is 2～5, stops heating, filters after 10 minutes, and the mother liquor that leaches is standby.
Filter also with 80～100 ℃ of water purification washings of 1.2 times of entire reaction liquor capacities again, send the spray-dryer drying, the finished product pack.
Claims (3)
1, a kind of with in the concentrated acid catalysis method and the method for water glass system white carbon black, the mother liquor that it is characterized in that using each production white carbon black will contain SiO as catalytic liquid
2Water glass join in the catalytic liquid, with the vitriol oil under agitation, pH value remains in 7～10 scopes, neutralization makes the white carbon black of excellent performance.
2, by the described method of claim 1, it is characterized in that catalytic liquid need give heat to 20～60 ℃, under agitation, add 8～20%SiO again
2Water glass, with in 83～98% vitriol oils and prepare white carbon black.
3,, when it is characterized in that neutralization system white carbon black, be metered into 83～98% vitriol oils and 8～20%SiO simultaneously by claim 1,2 described methods
2Water glass, keep the pH value of solution constant.Regulate pH value then 7～10,, kept 40 minutes at 70～100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91102200 CN1065440A (en) | 1991-04-03 | 1991-04-03 | White carbon black prepared by solulion induced concentrated acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91102200 CN1065440A (en) | 1991-04-03 | 1991-04-03 | White carbon black prepared by solulion induced concentrated acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1065440A true CN1065440A (en) | 1992-10-21 |
Family
ID=4905472
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91102200 Pending CN1065440A (en) | 1991-04-03 | 1991-04-03 | White carbon black prepared by solulion induced concentrated acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1065440A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039219C (en) * | 1993-12-21 | 1998-07-22 | 冯中一 | Technology for combination production of sodium silicate, aquation silica acid and zeolite catalyst by mirabilite method |
| CN102602946A (en) * | 2012-03-21 | 2012-07-25 | 陈君华 | Method for preparing high-specific-surface white carbon black by circularly utilizing waste water including sodium sulfate |
| CN103466644A (en) * | 2013-09-07 | 2013-12-25 | 安徽确成硅化学有限公司 | Method for preparing hydrophobic white carbon black |
| CN103466643A (en) * | 2013-08-21 | 2013-12-25 | 安徽确成硅化学有限公司 | Method for preparing white carbon black by circularly using mother liquor |
-
1991
- 1991-04-03 CN CN 91102200 patent/CN1065440A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039219C (en) * | 1993-12-21 | 1998-07-22 | 冯中一 | Technology for combination production of sodium silicate, aquation silica acid and zeolite catalyst by mirabilite method |
| CN102602946A (en) * | 2012-03-21 | 2012-07-25 | 陈君华 | Method for preparing high-specific-surface white carbon black by circularly utilizing waste water including sodium sulfate |
| CN102602946B (en) * | 2012-03-21 | 2022-04-08 | 安徽科技学院 | Method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate |
| CN103466643A (en) * | 2013-08-21 | 2013-12-25 | 安徽确成硅化学有限公司 | Method for preparing white carbon black by circularly using mother liquor |
| CN103466644A (en) * | 2013-09-07 | 2013-12-25 | 安徽确成硅化学有限公司 | Method for preparing hydrophobic white carbon black |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |