CN111661849A - Method for preparing food-grade white carbon black by inorganic acid fractional precipitation method - Google Patents
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000006229 carbon black Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 48
- 238000001556 precipitation Methods 0.000 title claims abstract description 27
- 150000007522 mineralic acids Chemical class 0.000 title claims abstract description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000725 suspension Substances 0.000 claims abstract description 31
- 230000032683 aging Effects 0.000 claims abstract description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 18
- 239000000654 additive Substances 0.000 claims abstract description 12
- 230000000996 additive effect Effects 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000008118 PEG 6000 Substances 0.000 claims abstract description 10
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 claims abstract description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 230000006911 nucleation Effects 0.000 claims abstract description 8
- 238000010899 nucleation Methods 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 230000012010 growth Effects 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000003916 acid precipitation Methods 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 239000010703 silicon Substances 0.000 claims abstract description 3
- 239000012065 filter cake Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 6
- 235000013305 food Nutrition 0.000 claims description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims 2
- 239000011707 mineral Substances 0.000 claims 2
- 239000002202 Polyethylene glycol Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 229920001223 polyethylene glycol Polymers 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 230000019635 sulfation Effects 0.000 claims 1
- 238000005670 sulfation reaction Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000004581 coalescence Methods 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 14
- 239000003921 oil Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 230000008859 change Effects 0.000 description 9
- 238000005273 aeration Methods 0.000 description 8
- 238000012544 monitoring process Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 229910001868 water Inorganic materials 0.000 description 8
- 230000003247 decreasing effect Effects 0.000 description 7
- 230000002572 peristaltic effect Effects 0.000 description 7
- 230000020477 pH reduction Effects 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 239000001692 EU approved anti-caking agent Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910007156 Si(OH)4 Inorganic materials 0.000 description 1
- 229910020489 SiO3 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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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
-
- 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
-
- 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
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- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for preparing food-grade white carbon black by an inorganic acid sectional precipitation method, which belongs to the technical field of white carbon black production and comprises the following steps: taking 20-90 g/L high-purity sodium silicate as a silicon source, adding 1-6 g/L additive PEG6000, adjusting the temperature to 60-90 ℃, adding 10% dilute sulfuric acid by mass into a reactor, stopping adding the dilute sulfuric acid into the solution when the pH of the solution is reduced to about 9.5, and introducing CO into the reactor2And N2Mixed gas (containing 25% -40% CO)2And the gas speed is 0.4-1.2L/min), and stopping introducing gas until the pH value of the solution is reduced to about 8, thus obtaining the suspension. And aging, acidifying, filtering, washing, drying and grinding the suspension to obtain the food-grade white carbon black. The invention controls SiO in sections by fast nucleation of early-stage sulfuric acid precipitation and slow growth of later-stage carbonization2The nucleation, growth and coalescence processes of the colloidal particles can realize the regulation and control of the surface structure and the distribution of hydroxyl groups of the white carbon black particles, and a new method is provided for the controlled synthesis of the food-grade white carbon black.
Description
Technical Field
The invention belongs to the field of white carbon black production, and particularly relates to a method for preparing food-grade white carbon black by an inorganic acid sectional precipitation method.
Background
The food-grade white carbon black is widely applied to the fields of drying agents, anti-caking agents, loosening agents, fresh keeping and the like of foods due to the excellent properties of the food-grade white carbon black. The production of food-grade white carbon black generally adopts a gas phase method, but the technology is complex, the raw material silicon tetrachloride or silane is toxic, the equipment requirement is high, the energy consumption is high, the cost is high, and further treatment is needed in some applications. In recent years, some enterprises adopt a precipitation method to produce food-grade white carbon black, and the specific preparation process comprises the steps of reacting inorganic acid (such as sulfuric acid, hydrochloric acid, nitric acid, carbonic acid, mixed acid and the like) with water glass to generate hydrated precipitated silica, and drying to obtain the finished product of white carbon black. The typical carbonation process principle is as follows:
Si(OH)4+(OH)4Si→(OH)3Si-O-Si(OH)3+H2O
the precipitation method has simple production process and low cost, but certain properties of the white carbon black prepared by the precipitation method are inferior to those of the white carbon black prepared by the gas phase method, and the performance requirements of the food-grade white carbon black cannot be met. For example, the white carbon black prepared by the sulfuric acid precipitation method has higher specific surface area, but the DBP oil absorption is lower, and the minimum requirement of food-grade white carbon black of 2.6cm cannot be met3The DBP prepared by the carbonization method has higher oil absorption, but lower specific surface area. The reason is that the properties of the white carbon black produced by the precipitation method, such as specific surface area, oil absorption value and the like, depend on the particle size of nucleation particles and the growth and agglomeration of the particles in the precipitation process. The sulfuric acid is strong acid, the grain size of nucleation particles is small, and the particles grow up and are seriously agglomerated in the later stage of precipitation, so the specific surface area of the product is higher, but the DBP oil absorption is lower. In the carbonization precipitation method, CO2Weak acid after being introduced into the solution, slow nucleation rate, large particle size of primary particles and relatively weak post-agglomerationTherefore, the specific surface area of the product is lower, but the DBP oil absorption is higher. The white carbon black is produced by combining the characteristics of a sulfuric acid method and a carbonization method and a sectional acidification precipitation method, so that a food-grade white carbon black product with better comprehensive performance can be produced. At present, relevant researches on the preparation of the white carbon black through segmented acidification and precipitation at home and abroad are not reported and lack of relevant researches. The present invention has been made in view of this situation.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a method for preparing food-grade white carbon black by an inorganic acid sectional precipitation method, wherein a high-purity sodium silicate solution is used as a silicon source, an additive is added, and the processes of nucleation, growth, agglomeration and the like of white carbon black particles are controlled in a sectional manner by a process of early-stage sulfuric acid precipitation, later-stage carbonization precipitation, aging, acidification, filtration, washing and drying, so that the food-grade white carbon black is prepared, wherein the specific surface area of the white carbon black is 75-300 m2The oil absorption value of the DBP is 2.6-3.5 cm3The concentration/g is regulated and controlled.
In order to solve the technical problems, the invention adopts the technical scheme that:
a method for preparing food-grade white carbon black by an inorganic acid fractional precipitation method comprises the following specific process steps:
1. high-purity sodium silicate (analytically pure Na) with the mass concentration of 20-90 g/L2SiO3·9H2O configuration) adding the solution into a reactor, and adding an additive PEG6000 with the mass concentration of 1-6 g/L when the temperature is adjusted to 60-90 ℃.
2. The reactor was charged with 10% dilute sulfuric acid while monitoring the solution pH change. When the pH value of the solution is reduced to 9-10, stopping adding dilute sulfuric acid into the solution, and introducing CO into the reactor2And N2Mixed gas (containing 25% -40% CO)2And the gas velocity of the mixed gas is 0.4-1.2L/min), and the pH change of the solution is continuously monitored.
3. When the pH of the suspension is reduced to about 8, the aeration is stopped to obtain the suspension. And aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid. Aging the solution for 30-60 min, filtering, repeatedly washing the filter cake with deionized water for 3-4 times, and removing N in the filter cakea+、Cl-、CO3 2-、SO4 2-And plasma impurity ions.
4. Preparing the filter cake into suspension with the mass concentration of 10%, introducing the suspension into a spray dryer, performing spray drying in airflow at 240-270 ℃, and grinding to obtain the food-grade white carbon black.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects.
1. The white carbon black is prepared by inorganic acid fractional precipitation, the performance of the white carbon black is far higher than that of rubber-grade white carbon black, the level of food-grade white carbon black is reached, and the additional value of the white carbon black is greatly improved.
2. SiO control by staged precipitation reaction2The processes of nucleation, growth and coalescence of colloidal particles can realize the regulation and control of the surface structure and the distribution of hydroxyl groups of the white carbon black particles. According to the requirements, the specific surface area and DBP oil absorption value of the white carbon black can be respectively controlled to be 180-250 m2The sum of the amounts of the components is 2.6-3 cm3Between/g. The method provides a new method for the controlled synthesis of the food-grade white carbon black.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention to its proper form. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a schematic process flow diagram of the present invention.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention. The following examples are given in the specific process flow illustrated in FIG. 1.
Example 1:
1L of high-purity sodium silicate solution with the mass concentration of 40g/L is added into a reactor with a jacket, and circulating water with a certain temperature is introduced into the jacket of the reactor. When the temperature of the sodium silicate solution was adjusted to 60 ℃, 2g of additive PEG6000 were added to the reactor, and stirring was started while keeping the stirring rate constant. A peristaltic pump was used to add dilute sulfuric acid at a mass concentration of 10% to the reactor at a rate of 10mL/min while monitoring the change in solution pH. When the pH of the solution decreased to 9.5, the addition of dilute sulfuric acid to the solution was stopped while CO was fed to the reactor at a rate of 0.4L/min2-N2Mixed gas (CO)225%) was added to the solution, and the solution pH was continuously monitored for changes. When the pH of the solution was reduced to about 8, the aeration was stopped to obtain a suspension. And (3) aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid with the mass fraction of 10%. Aging the solution for 30-60 min, filtering, repeatedly washing and filtering a filter cake for 3-4 times by using deionized water, and removing Na in the filter cake+、Cl-、CO3 2-、SO4 2-And plasma impurity ions. Preparing the filter cake into suspension with mass concentration of 10%, introducing into a spray dryer, spray drying at 260 deg.C in air flow, grinding to obtain a product with specific surface area and DBP oil absorption value of 206.4m2G and 2.86cm3Food-grade white carbon black per gram.
Example 2:
1L of high-purity sodium silicate solution with the mass concentration of 80g/L is added into a reactor with a jacket, and circulating water with a certain temperature is introduced into the jacket of the reactor. When the temperature of the sodium silicate solution was adjusted to 60 ℃, 2g of additive PEG6000 were added to the reactor, and stirring was started while keeping the stirring rate constant. A peristaltic pump was used to add dilute sulfuric acid at a mass concentration of 10% to the reactor at a rate of 10mL/min while monitoring the change in solution pH. When the pH of the solution decreased to 9.5, the addition of diluent to the solution was stoppedSulfuric acid, while feeding CO into the reactor at a rate of 0.4L/min2-N2Mixed gas (CO)225%) was added to the solution, and the solution pH was continuously monitored for changes. When the pH of the solution was reduced to about 8, the aeration was stopped to obtain a suspension. And (3) aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid with the mass fraction of 10%. Aging the solution for 30-60 min, filtering, repeatedly washing and filtering a filter cake for 3-4 times by using deionized water, and removing Na in the filter cake+、Cl-、CO3 2-、SO4 2-And plasma impurity ions. Preparing the filter cake into suspension with mass concentration of 10%, introducing into a spray dryer, spray drying at 260 deg.C in air flow, grinding to obtain product with specific surface area and DBP oil absorption value of 235.7m2G and 2.64cm3Food-grade white carbon black per gram.
Example 3:
1L of high-purity sodium silicate solution with the mass concentration of 40g/L is added into a reactor with a jacket, and circulating water with a certain temperature is introduced into the jacket of the reactor. When the temperature of the sodium silicate solution was adjusted to 90 ℃, 2g of additive PEG6000 were added to the reactor, and stirring was started while keeping the stirring rate constant. A peristaltic pump was used to add dilute sulfuric acid at a mass concentration of 10% to the reactor at a rate of 10mL/min while monitoring the change in solution pH. When the pH of the solution decreased to 9.5, the addition of dilute sulfuric acid to the solution was stopped while CO was fed to the reactor at a rate of 0.4L/min2-N2Mixed gas (CO)225%) was added to the solution, and the solution pH was continuously monitored for changes. When the pH of the solution was reduced to about 8, the aeration was stopped to obtain a suspension. And (3) aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid with the mass fraction of 10%. Aging the solution for 30-60 min, filtering, repeatedly washing and filtering a filter cake for 3-4 times by using deionized water, and removing Na in the filter cake+、Cl-、CO3 2-、SO4 2-And plasma impurity ions. Preparing the filter cake into suspension with mass concentration of 10%, introducing into a spray dryer, spray drying at 260 deg.C in air flow, grinding to obtain specific surface area and DBP oil absorption value of 191.2m2G and 2.92cm3Food/gAnd (3) grade white carbon black.
Example 4:
1L of high-purity sodium silicate solution with the mass concentration of 80g/L is added into a reactor with a jacket, and circulating water with a certain temperature is introduced into the jacket of the reactor. When the temperature of the sodium silicate solution was adjusted to 90 ℃, 2g of additive PEG6000 were added to the reactor, and stirring was started while keeping the stirring rate constant. A peristaltic pump was used to add dilute sulfuric acid at a mass concentration of 10% to the reactor at a rate of 10mL/min while monitoring the change in solution pH. When the pH of the solution decreased to 9.5, the addition of dilute sulfuric acid to the solution was stopped while CO was fed to the reactor at a rate of 0.4L/min2-N2Mixed gas (CO)225%) was added to the solution, and the solution pH was continuously monitored for changes. When the pH of the solution was reduced to about 8, the aeration was stopped to obtain a suspension. And (3) aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid with the mass fraction of 10%. Aging the solution for 30-60 min, filtering, repeatedly washing and filtering a filter cake for 3-4 times by using deionized water, and removing Na in the filter cake+、Cl-、CO3 2-、SO4 2-And plasma impurity ions. Preparing the filter cake into suspension with mass concentration of 10%, introducing into a spray dryer, spray drying at 260 deg.C in air flow, grinding to obtain product with specific surface area and DBP oil absorption value of 210.5m2G and 2.81cm3Food-grade white carbon black per gram.
Example 5:
1L of high-purity sodium silicate solution with the mass concentration of 40g/L is added into a reactor with a jacket, and circulating water with a certain temperature is introduced into the jacket of the reactor. When the temperature of the sodium silicate solution was adjusted to 60 ℃, 6g of additive PEG6000 were added to the reactor, and stirring was started while keeping the stirring rate constant. A peristaltic pump was used to add dilute sulfuric acid at a mass concentration of 10% to the reactor at a rate of 10mL/min while monitoring the change in solution pH. When the pH of the solution decreased to 9.5, the addition of dilute sulfuric acid to the solution was stopped while CO was fed to the reactor at a rate of 0.4L/min2-N2Mixed gas (CO)225%) was added to the solution, and the solution pH was continuously monitored for changes. Stopping aeration when the pH of the solution is reduced to about 8 to obtain a suspension. And (3) aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid with the mass fraction of 10%. Aging the solution for 30-60 min, filtering, repeatedly washing and filtering a filter cake for 3-4 times by using deionized water, and removing Na in the filter cake+、Cl-、CO3 2-、SO4 2-And plasma impurity ions. Preparing the filter cake into suspension with mass concentration of 10%, introducing into a spray dryer, spray drying at 260 deg.C in air flow, grinding to obtain specific surface area and DBP oil absorption value of 198.5m2G and 2.72cm3Food-grade white carbon black per gram.
Example 6:
1L of high-purity sodium silicate solution with the mass concentration of 40g/L is added into a reactor with a jacket, and circulating water with a certain temperature is introduced into the jacket of the reactor. When the temperature of the sodium silicate solution was adjusted to 60 ℃, 2g of additive PEG6000 were added to the reactor, and stirring was started while keeping the stirring rate constant. A peristaltic pump was used to add dilute sulfuric acid at a mass concentration of 10% to the reactor at a rate of 10mL/min while monitoring the change in solution pH. When the solution pH decreased to 9.5, the addition of dilute sulfuric acid to the solution was stopped while CO was fed to the reactor at a rate of 1.2L/min2-N2Mixed gas (CO)225%) was added to the solution, and the solution pH was continuously monitored for changes. When the pH of the solution was reduced to about 8, the aeration was stopped to obtain a suspension. And (3) aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid with the mass fraction of 10%. Aging the solution for 30-60 min, filtering, repeatedly washing and filtering a filter cake for 3-4 times by using deionized water, and removing Na in the filter cake+、Cl-、CO3 2-、SO4 2-And plasma impurity ions. Preparing the filter cake into suspension with mass concentration of 10%, introducing into a spray dryer, spray drying at 260 deg.C in air flow, grinding to obtain a product with specific surface area and DBP oil absorption value of 224.7m2G and 2.72cm3Food-grade white carbon black per gram.
Example 7:
adding 1L of high-purity sodium silicate solution with the mass concentration of 40g/L into a reactor with a clamp sleeve, and introducing circulating water with a certain temperature into the reactorIn the reactor jacket. When the temperature of the sodium silicate solution was adjusted to 60 ℃, 2g of additive PEG6000 were added to the reactor, and stirring was started while keeping the stirring rate constant. A peristaltic pump was used to add dilute sulfuric acid at a mass concentration of 10% to the reactor at a rate of 10mL/min while monitoring the change in solution pH. When the pH of the solution decreased to 9.5, the addition of dilute sulfuric acid to the solution was stopped while CO was fed to the reactor at a rate of 0.4L/min2-N2Mixed gas (CO)240%) was added to the solution, and the solution pH was continuously monitored for changes. When the pH of the solution was reduced to about 8, the aeration was stopped to obtain a suspension. And (3) aging the suspension for 30-60 min, and adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid with the mass fraction of 10%. Aging the solution for 30-60 min, filtering, repeatedly washing and filtering a filter cake for 3-4 times by using deionized water, and removing Na in the filter cake+、Cl-、CO3 2-、SO4 2-And plasma impurity ions. Preparing the filter cake into suspension with mass concentration of 10%, introducing into a spray dryer, spray drying at 260 deg.C in air flow, grinding to obtain powder with specific surface area and DBP oil absorption value of 216.5m2G and 2.77cm3Food-grade white carbon black per gram.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A method for preparing food-grade white carbon black by an inorganic acid fractional precipitation method is characterized by comprising the following steps:
step (1), preparing food-grade white carbon black precipitate: using 20-90 g/L high-purity sodium silicate as silicon source, adding additive, and adjusting temperature to 60 ℃Adding 10% dilute sulfuric acid at 90 deg.C, stopping adding dilute sulfuric acid when pH of the solution is reduced to about 9.5, and introducing CO into the reactor2And N2Mixing gas until the pH value of the solution is reduced to about 8, and stopping introducing gas to obtain a suspension;
and (2) food-grade white carbon black precipitation post-treatment: and aging the suspension for 30-60 min, adjusting the pH value of the solution to about 7 by using dilute hydrochloric acid, aging the solution for 30-60 min, filtering, repeatedly washing a filter cake for 3-4 times by using deionized water to remove impurity ions, preparing the filter cake into suspension with the mass concentration of 10%, drying, and grinding to obtain the food-grade white carbon black.
2. The method for preparing food-grade white carbon black by using the inorganic acid fractional precipitation method according to claim 1, wherein the additive in the step (1) is polyethylene glycol PEG6000, and the mass concentration is 1-6 g/L.
3. The method for preparing food grade white carbon black by using the inorganic acid fractional precipitation method according to claim 1, wherein CO in the step (1)2And N2The mixed gas contains 25 to 40 volume percent of CO2The gas velocity of the mixed gas is 0.4-1.2L/min.
4. The method for preparing food grade white carbon black by the mineral acid fractional precipitation method according to claim 1, wherein in the step (1), rapid nucleation is performed by using sulfuric acid precipitation in the early stage, slow growth is performed by using carbonization precipitation in the later stage, and the pH of the solution at the end point of the sulfation precipitation is 9.5.
5. The method for preparing food grade white carbon black by using the mineral acid fractional precipitation method according to claim 1, wherein the impurity ions comprise Na+、Cl-、CO3 2-、SO4 2-。
6. The method for preparing food grade white carbon black by using the inorganic acid fractional precipitation method according to claim 1, wherein the drying conditions in the step (2) are as follows: introducing the mixture into a spray dryer for spray drying in air flow at 240-270 ℃.
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