CN111762790A - Novel method for modifying white carbon black - Google Patents

Novel method for modifying white carbon black Download PDF

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Publication number
CN111762790A
CN111762790A CN202010644852.XA CN202010644852A CN111762790A CN 111762790 A CN111762790 A CN 111762790A CN 202010644852 A CN202010644852 A CN 202010644852A CN 111762790 A CN111762790 A CN 111762790A
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Prior art keywords
carbon black
white carbon
washing
washing tank
filter cake
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CN202010644852.XA
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Chinese (zh)
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杨英春
曹玉宽
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Jinyang Hi Tech Material Ltd By Share Ltd
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Jinyang Hi Tech Material Ltd By Share Ltd
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Priority to CN202010644852.XA priority Critical patent/CN111762790A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/48Halides, with or without other cations besides aluminium
    • C01F7/50Fluorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention discloses a new method for modifying white carbon black in the technical field of white carbon black, which comprises the following steps: (1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake, and then carrying out filter pressing on the white carbon black filter cake; (2) conveying the filter-pressed white carbon black to a first washing tank, pulping and stirring by using water as a solvent and a pulping stirrer, and then performing suction filtration on the pulp by using a vacuum pump; (3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring; (4) feeding the white carbon black filter cake after the second washing into a third washing tank, injecting alkali liquor into the third washing tank, adjusting the pH value to 6.5-7.5, and drying to obtain modified white carbon black; according to the invention, the first washing tank, the second washing tank and the third washing tank are added, so that the loose packing density of the white carbon black is reduced, the white carbon black is fluffy, the specific surface area and the oil absorption value of the white carbon black are improved, and the quality of the white carbon black is improved.

Description

Novel method for modifying white carbon black
Technical Field
The invention relates to the technical field of white carbon black, in particular to a new method for modifying white carbon black.
Background
White carbon black is a general term for white powdery X-ray amorphous silicic acid and silicate products, mainly referring to precipitated silica, fumed silica and ultrafine silica gel, and also including powdery synthetic aluminum silicate, calcium silicate, and the like. White carbon black is a porous substance, can be dissolved in caustic alkali and hydrofluoric acid, and is not dissolved in water, solvents and acids (except hydrofluoric acid). High-temperature resistance, non-combustion, tastelessness, odorless and good electrical insulation. The white carbon black which is a byproduct can be produced in the process of producing the aluminum fluoride by the fluorosilicic acid method, because in the production process of producing the aluminum fluoride by the fluorosilicic acid method, the whole reaction is under the acidic condition, the white carbon black produced under the acidic condition has certain adsorbability, at the moment, excessive fluosilicic acid in the solution and aluminum hydroxide can generate the aluminum fluosilicate, the aluminum fluosilicate can be attached to the surface of the white carbon black to be continuously hydrolyzed to generate free aluminum fluoride and the white carbon black, and part of the free aluminum fluoride in the solution can be tightly immersed in the pores of the white carbon black to be cooled to form aluminum fluoride crystals, so that the F, Al content in the white carbon black which is a byproduct is too.
In the prior art, the by-product white carbon black is usually dried, crushed and directly sold after suction filtration, but the by-product white carbon black has high F, Al content and low silicon dioxide content, so that the by-product white carbon black has small specific surface area and oil absorption value, low practicability, low quality and low economic benefit; moreover, the by-product white carbon black contains a large amount of F, Al and cannot be recycled, so that the waste of resources is caused.
Therefore, a new method for modifying white carbon black is provided to solve the problems.
Disclosure of Invention
The invention aims to provide a new method for modifying white carbon black, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides a new method for modifying white carbon black, which specifically comprises the following steps:
(1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake, and then carrying out filter pressing on the white carbon black filter cake;
(2) delivering the filtered white carbon black to a first washing tank, taking water as a solvent, pulping and stirring by using a pulping stirrer, controlling the temperature to be 60-80 ℃, stirring for 8-15min at the rotating speed of 200-400r/min, and then performing suction filtration on the slurry by using a vacuum pump;
(3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring;
(4) and feeding the white carbon black filter cake after the second washing into a third washing tank, injecting alkali liquor into the third washing tank, adjusting the pH value to 6.5-7.5, and drying to obtain the modified white carbon black.
Preferably, the filtrate obtained after suction filtration in the steps (1), (2) and (3) is introduced into a crystallization tank, and crystallization is continued in the crystallization tank.
Preferably, the temperature in the step (2) is 65-78 ℃, the rotating speed is 250-350r/min, and the stirring time is 9-12 min.
Preferably, the temperature in the step (2) is 75 ℃, the rotating speed is 300r/min, and the stirring time is 10 min.
Preferably, the temperature, the rotation speed and the stirring time in the step (3) are the same as those in the second step.
Preferably, the alkali solution in the step (4) is ammonia water with the concentration of 1%.
Preferably, the pH in the step (4) is 7.
Preferably, the washing water after the first washing is transferred to a second washing tank for reuse.
The invention has the beneficial effects that:
according to the invention, the water content in the white carbon black filter cake is further reduced by carrying out filter pressing on the basis of suction filtration, and a large amount of fluorine aluminum is carried away by water, so that the fluorine aluminum content in the white carbon black filter cake is further reduced, the water quantity required by subsequent washing and the suction filtration times are reduced, and the input cost is greatly reduced;
according to the invention, the white carbon black filter cake is beaten, stirred and washed twice by adding the first washing tank, the second washing tank and the third washing tank in the first washing tank and the second washing tank by using hot water as a solvent, the white carbon black is insoluble to the hot water, and the hot water dissolves and takes away aluminum fluoride crystals adsorbed in the white carbon black pores, so that the content of fluorine aluminum in the white carbon black is further reduced, then the white carbon black filter cake is soaked in the third washing tank, the PH of the white carbon black is adjusted to be neutral, the content of silicon dioxide is increased, the loose packing density of the white carbon black is favorably reduced, the white carbon black is more fluffy, the specific surface area and the oil absorption value of the white carbon black are increased, the quality of the white carbon black is improved, the practicability is stronger;
according to the invention, the washing water in the first washing tank is injected into the second washing tank, so that the washing water is recycled, the generation amount of waste water is reduced, and the full utilization of resources is ensured;
according to the invention, the filtrate obtained after suction filtration in the steps (1), (2) and (3) is pumped into the crystallization tank for crystallization, and finally, aluminum fluoride is generated by crystallization, so that the yield of aluminum fluoride is increased, the aluminum loss is reduced and avoided, and the economic benefit is increased.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A new method for modifying white carbon black specifically comprises the following steps:
(1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake, and then carrying out filter pressing on the white carbon black filter cake;
(2) conveying the filter-pressed white carbon black to a first washing tank, pulping and stirring by using water as a solvent and a pulping stirrer, controlling the temperature to be 60 ℃, stirring for 8min at a rotating speed of 200r/min, and then performing suction filtration on the slurry by using a vacuum pump;
(3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring;
(4) and feeding the white carbon black filter cake after the second washing into a third washing tank, injecting ammonia water with the concentration of 1% into the third washing tank, adjusting the pH value to be 6.5, and drying to obtain the modified white carbon black.
Pumping the filtrate obtained after suction filtration in the steps (1), (2) and (3) into a crystallization tank, and continuously crystallizing in the crystallization tank; the temperature, the rotating speed and the stirring time in the step (3) are the same as those in the step two; and conveying the washing water after the first washing to a second washing tank for recycling.
Example two
A new method for modifying white carbon black specifically comprises the following steps:
(1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake, and then carrying out filter pressing on the white carbon black filter cake;
(2) conveying the filter-pressed white carbon black to a first washing tank, pulping and stirring by using water as a solvent and a pulping stirrer, controlling the temperature to be 70 ℃, stirring for 10min at the rotating speed of 300r/min, and then performing suction filtration on the slurry by using a vacuum pump;
(3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring;
(4) and feeding the white carbon black filter cake after the second washing into a third washing tank, injecting ammonia water with the concentration of 1% into the third washing tank, adjusting the pH value to be 7, and drying to obtain the modified white carbon black.
Pumping the filtrate obtained after suction filtration in the steps (1), (2) and (3) into a crystallization tank, and continuously crystallizing in the crystallization tank; the temperature, the rotating speed and the stirring time in the step (3) are the same as those in the step two; and conveying the washing water after the first washing to a second washing tank for recycling.
EXAMPLE III
A new method for modifying white carbon black specifically comprises the following steps:
(1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake, and then carrying out filter pressing on the white carbon black filter cake;
(2) conveying the filter-pressed white carbon black to a first washing tank, pulping and stirring by using water as a solvent and a pulping stirrer, controlling the temperature to be 80 ℃, stirring for 15min at a rotating speed of 400r/min, and then performing suction filtration on the slurry by using a vacuum pump;
(3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring;
(4) and feeding the white carbon black filter cake after the second washing into a third washing tank, injecting ammonia water with the concentration of 1% into the third washing tank, adjusting the pH value to 7.5, and drying to obtain the modified white carbon black.
Pumping the filtrate obtained after suction filtration in the steps (1), (2) and (3) into a crystallization tank, and continuously crystallizing in the crystallization tank; the temperature, the rotating speed and the stirring time in the step (3) are the same as those in the step two; and conveying the washing water after the first washing to a second washing tank for recycling.
Comparative example 1
A new method for modifying white carbon black specifically comprises the following steps:
(1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake;
(2) conveying the filter-pressed white carbon black to a first washing tank, pulping and stirring by using water as a solvent and a pulping stirrer, controlling the temperature to be 70 ℃, stirring for 10min at the rotating speed of 300r/min, and then performing suction filtration on the slurry by using a vacuum pump;
(3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring;
(4) and feeding the white carbon black filter cake after the second washing into a third washing tank, injecting ammonia water with the concentration of 1% into the third washing tank, adjusting the pH value to be 7, and drying to obtain the modified white carbon black.
Pumping the filtrate obtained after suction filtration in the steps (1), (2) and (3) into a crystallization tank, and continuously crystallizing in the crystallization tank; the temperature, the rotating speed and the stirring time in the step (3) are the same as those in the step two; and conveying the washing water after the first washing to a second washing tank for recycling.
Comparative example No. two
A new method for modifying white carbon black specifically comprises the following steps:
(1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake, and then carrying out filter pressing on the white carbon black filter cake;
(2) conveying the filter-pressed white carbon black to a first washing tank, pulping and stirring by using water as a solvent and a pulping stirrer, controlling the temperature to be 70 ℃, stirring for 10min at the rotating speed of 300r/min, and then performing suction filtration on the slurry by using a vacuum pump;
(3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring;
(4) and drying the white carbon black filter cake after the second washing to obtain the modified white carbon black.
Pumping the filtrate obtained after suction filtration in the steps (1), (2) and (3) into a crystallization tank, and continuously crystallizing in the crystallization tank; the temperature, the rotating speed and the stirring time in the step (3) are the same as those in the step two; and conveying the washing water after the first washing to a second washing tank for recycling.
Performance detection
The silica content in 1g of white carbon black in each example and comparative example was determined by chemical analysis, and the control group was 1g of white carbon black which was not treated by the method of the present application, and the specific detection results are shown in the following table.
Epi-silica content
Group of Silicon dioxide content/%)
Example 1 95
Example 2 94
Example 3 96
Comparative example 1 90
Comparative example 2 94
Control group 80
In summary, it can be seen from the table that the silica content of 1g of white carbon black in each group of examples and comparative examples is much greater than that of 1g of white carbon black in the comparative group, which indicates that the white carbon black produced by the method of the present application has low content of aluminum fluoride and high silica content, and the produced white carbon black has better quality, and is beneficial to recovery of aluminum fluoride and resource saving.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not exhaustive and do not limit the method of making a high strength caliper seal to the specific embodiments described. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (8)

1. The new method for modifying the white carbon black is characterized by comprising the following steps of:
(1) carrying out suction filtration on the filtered white carbon black by using a vacuum pump to obtain a white carbon black filter cake, and then carrying out filter pressing on the white carbon black filter cake;
(2) delivering the filtered white carbon black to a first washing tank, taking water as a solvent, pulping and stirring by using a pulping stirrer, controlling the temperature to be 60-80 ℃, stirring for 8-15min at the rotating speed of 200-400r/min, and then performing suction filtration on the slurry by using a vacuum pump;
(3) feeding the white carbon black filter cake after the first washing into a second washing tank again for pulping and stirring;
(4) and feeding the white carbon black filter cake after the second washing into a third washing tank, injecting alkali liquor into the third washing tank, adjusting the pH value to 6.5-7.5, and drying to obtain the modified white carbon black.
2. The new method for modifying white carbon black according to claim 1, wherein the filtrates obtained by suction filtration in the steps (1), (2) and (3) are fed into a crystallization tank, and crystallization is continued in the crystallization tank.
3. The new method for modifying white carbon black according to claim 1, wherein the temperature in the step (2) is 65-78 ℃, the rotation speed is 250-350r/min, and the stirring time is 9-12 min.
4. The new method for modifying white carbon black according to claim 3, wherein the temperature in the step (2) is 75 ℃, the rotation speed is 300r/min, and the stirring time is 10 min.
5. The new method for modifying white carbon black according to claim 1, wherein the temperature, the rotation speed and the stirring time in the step (3) are the same as those in the second step.
6. The new method for modifying white carbon black according to claim 1, wherein the alkali solution in the step (4) is 1% ammonia water.
7. The method for modifying white carbon black according to claim 1, wherein the pH in the step (4) is 7.
8. The new method for modifying white carbon black according to claim 1, wherein the washing water after the first washing is delivered to the second washing tank for recycling.
CN202010644852.XA 2020-07-07 2020-07-07 Novel method for modifying white carbon black Pending CN111762790A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114873901A (en) * 2022-05-07 2022-08-09 广州诺冠环保科技有限公司 Preparation method of novel sludge conditioner applied to plate-and-frame filter press

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114873901A (en) * 2022-05-07 2022-08-09 广州诺冠环保科技有限公司 Preparation method of novel sludge conditioner applied to plate-and-frame filter press

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