CN102491347B - Method for improving quality of white carbon black product - Google Patents
Method for improving quality of white carbon black product Download PDFInfo
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- CN102491347B CN102491347B CN 201110395114 CN201110395114A CN102491347B CN 102491347 B CN102491347 B CN 102491347B CN 201110395114 CN201110395114 CN 201110395114 CN 201110395114 A CN201110395114 A CN 201110395114A CN 102491347 B CN102491347 B CN 102491347B
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Abstract
The invention discloses a method for improving quality of a white carbon black product, which comprises the following steps: performing secondary countercurrent washing to the white carbon black product with content of N to be 1-3% and content of F to be 1-4% through thin ammonium fluoride solution having the quality which is 3-4 times that of a wet basis white carbon black product; utilizing thin ammonia water having the quality which is 3-4 times that of the wet basis white carbon black product to wash the white carbon black product after countercurrent washing; using thin fluorosilicic acid of 1% to 5% to wash the white carbon black product after washing by thin ammonia water, enabling using quantity of the thin fluorosilicic acid to be 0.4-0.7 time of a theoretical using quantity, removing free ammonia in the white carbon black product, and transforming most of free ammonia into ammonium fluoride; using water to wash the white carbon black product after washing by thin fluorosilicic acid, enabling 10-14 tons of water to be used for per ton of wet basis white carbon black product, and further removing ammonia and tiny thin fluorosilicic acid in the product; and drying the white carbon black product. The method for improving the quality of the white carbon black product can effectively reduce content of nitrogen in the white carbon black product and remove pungent odor of ammonia gas in white carbon black.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to a kind of method that improves the white carbon black quality product.
Background technology
At present, be the feedstock production white carbon black with Neutral ammonium fluoride and raw material silicon-dioxide, at first obtain ammonium silicofluoride through dissolving raw material silicon-dioxide, separate out precipitated silica product and ammonium fluoride solution with ammonia precipitation ammonium silicofluoride again.In order to precipitate ammonium silicofluoride fully, ammonia must be excessive, is dissolved with more ammonia in the ammonium fluoride aqueous solution.When separating Neutral ammonium fluoride and white carbon black product, ammoniacal liquor can be mixed in the white carbon black product, cause the nitrogen content in the white carbon black product too high, and the strong impulse smell arranged, simultaneously, Neutral ammonium fluoride can produce weak ammonia in concentration process, because the quantity discharged of this weak ammonia is big, thereby the environmental issue that produces also makes very headache of enterprise, therefore need manage to recycle.US5266289 " by the technology of utilizing the reaction of raw material silicon-dioxide and Neutral ammonium fluoride to produce high-purity silicon dioxide " (process for producing high-purity silicon by reacting crude silica with ammonium fluoride) and US5458864 " by the technology of utilizing the reaction of raw material silicon-dioxide and Neutral ammonium fluoride to produce high-purity silicon dioxide " (process for producing high-purity silica by reacting crude silica with ammonium fluoride) disclose nitrogenous height on November 30th, 1993 with in October 17 nineteen ninety-five respectively, the white carbon black product that irritating smell is arranged, dilute sulphuric acid washing with 2%, remove ammonia, improve the white carbon black quality product, but introduced new impurity sulfuric acid or ammonium sulfate.The method that existing report is produced the white carbon black product is that water washs the pungency that white carbon black is removed ammonia basically, and the clearance of ammonia is low, the wash water consumption big, the ammonia-containing water difficult treatment.
Summary of the invention
The objective of the invention is to overcome above-mentioned shortcoming and nitrogen content in a kind of effective reduction white carbon black product is provided, removes the method for the raising white carbon black quality product of the stimulation nature and flavor of ammonia in the white carbon black.
Purpose of the present invention is achieved by following technical proposals.
The invention provides a kind of method that improves the white carbon black quality product, comprise the steps:
(1) N content is 1-3%, and F content is that the white carbon black product of 1-4% is wet basis white carbon black quality product 3-4 2 countercurrent washings of rare ammonium fluoride solution doubly through quality;
(2) will be wet basis white carbon black quality product 3-4 weak ammonia washing doubly through the white carbon black product quality of countercurrent washing;
(3) with the rare silicofluoric acid washing of the white carbon black product after the weak ammonia washing with 1%-5%, the 0.4-0.7 that rare silicofluoric acid consumption is theoretical consumption doubly removes the free ammonia in the white carbon black product, and most of free ammonia is converted into Neutral ammonium fluoride;
(4) the white carbon black product after rare silicofluoric acid washing is washed with water, the consumption of water is 10-14 ton/ton wet basis white carbon black product, further removes ammonia and micro-rare silicofluoric acid in the product;
(5) dry white carbon black product.
The method of above-mentioned raising white carbon black quality product, wherein: the mass concentration of water is 60-75% in the wet basis white carbon black product.
The method of above-mentioned raising white carbon black quality product, wherein: make dioxide-containing silica more than or equal to 90%, N smaller or equal to 0.25%, F content is smaller or equal to 0.3% white carbon black product.
The present invention compared with prior art has tangible beneficial effect, and as can be known from the above technical solutions: the present invention has taken full advantage of the weak ammonia that Neutral ammonium fluoride device process produces, and reduces the quantity discharged of device weak ammonia.And utilize rare silicofluoric acid and be mixed in that weak ammonia can react in the white carbon black product, and the solubleness of Neutral ammonium fluoride in water changes into Neutral ammonium fluoride than the big principle of the solubleness of ammonia in water with weak ammonia, reduces the nitrogen content in the white carbon black product.Thereby make the present invention not only effectively remove ammonia, and in the white carbon black product, do not introduce new impurity, improve the quality of white carbon black product.
Embodiment
Embodiment 1
A kind of method that improves the white carbon black quality product comprises the steps:
(1) N content is that 3%, F content is that 2% wet basis white carbon black product is 2 countercurrent washings of rare Neutral ammonium fluoride of 3 times of wet basis white carbon black quality producies through quality;
(2) will be the weak ammonia washing of 3 times of wet basis white carbon black quality producies through the white carbon black product quality in the countercurrent washing; N content in the wet basis white carbon black is that 2.6%, F content is 0.7% at this moment;
(3) with the rare silicofluoric acid washing of 1 ton of wet basis white carbon black product after the weak ammonia washing with 3 ton 1%, remove the free ammonia in the white carbon black product, most of free ammonia is converted into Neutral ammonium fluoride;
(4) with 1 ton of wet basis white carbon black product after the washing of rare silicofluoric acid with 10 tons of water washings, further remove ammonia and micro-rare silicofluoric acid in the product, N content in the product is 0.092%, makes dioxide-containing silica after drying and be 91.02%, N content is 0.25%, the white carbon black product of the non-stimulated nature and flavor of F content 0.2%.
Embodiment 2
A kind of method that improves the white carbon black quality product comprises the steps:
(1) N content is that 3%, F content is that 2% wet basis white carbon black product is 2 countercurrent washings of rare Neutral ammonium fluoride of 3 times of wet basis white carbon black quality producies through quality;
(2) will be the weak ammonia washing of 3 times of wet basis white carbon black quality producies through the white carbon black product quality in the countercurrent washing; N content in the wet basis white carbon black is that 2.5%, F content is 0.7% at this moment;
(3) with the rare silicofluoric acid washing of 1 ton of wet basis white carbon black product after the weak ammonia washing with 3 ton 1%, remove the free ammonia in the white carbon black product, most of free ammonia is converted into Neutral ammonium fluoride;
(4) with 1 ton of wet basis white carbon black product in the rare silicofluoric acid washing back with 14 tons of water washings, further remove ammonia and micro-rare silicofluoric acid in the product, N content in the product is 0.072%, makes dioxide-containing silica after drying and be 90.51 %, N content and be 0.17%, F content is 0.16%, the white carbon black product of non-stimulated nature and flavor.
Embodiment 3
A kind of method that improves the white carbon black quality product comprises the steps:
(1) N content is that 3%, F content is that 2% wet basis white carbon black product is 2 countercurrent washings of rare Neutral ammonium fluoride of 3 times of wet basis white carbon black quality producies through quality;
(2) will be the weak ammonia washing of 3 times of wet basis white carbon black quality producies through the white carbon black product quality in the countercurrent washing; N content in the wet basis white carbon black is that 2.5%, F content is 0.7% at this moment;
(3) with the rare silicofluoric acid washing of 1 ton of wet basis white carbon black product after the weak ammonia washing with 1.5 ton 5%, remove the free ammonia in the white carbon black product, most of free ammonia is converted into Neutral ammonium fluoride;
(4) with 1 ton of wet basis white carbon black product in the rare silicofluoric acid washing back with 10 tons of water washings, further remove ammonia and micro-rare silicofluoric acid in the product, N content in the product is 0.044%, makes dioxide-containing silica after drying and be 91.72%, N content is 0.1%, F content is 0.26%, the white carbon black product of non-stimulated nature and flavor.
Embodiment 4
A kind of method that improves the white carbon black quality product comprises the steps:
(1) N content is that 3%, F content is that 4% white carbon black product is 2 countercurrent washings of rare Neutral ammonium fluoride of 4 times of wet basis white carbon black quality producies through quality;
(2) will be the weak ammonia washing of 4 times of wet basis white carbon black quality producies through the white carbon black product quality in the countercurrent washing; N content in the wet basis white carbon black is that 2.7%, F content is 1.5% at this moment;
(3) with the rare silicofluoric acid washing white carbon black of 1 ton of wet basis white carbon black in the weak ammonia washing back with 1 ton 3%, remove the free ammonia in the white carbon black product, most of free ammonia is converted into Neutral ammonium fluoride;
(4) with 1 ton of wet basis white carbon black product in the rare silicofluoric acid washing back with 14 tons of water washings, further remove ammonia and micro-rare silicofluoric acid in the product, N content in the product is 0.075%, makes dioxide-containing silica after drying and be 93 %, N content and be 0.18%, F content is 0.3%, the white carbon black product of non-stimulated nature and flavor.
Embodiment 5
A kind of method that improves the white carbon black quality product comprises the steps:
(1) N content is that 1%, F content is that 1% white carbon black product is 2 countercurrent washings of rare Neutral ammonium fluoride of 4 times of wet basis white carbon black quality producies through quality;
(2) will be the weak ammonia washing of 4 times of wet basis white carbon black quality producies through the white carbon black product quality in the countercurrent washing; N content in the wet basis white carbon black is that 0.6%, F content is 0.5% at this moment;
(3) with the rare silicofluoric acid washing white carbon black of 1 ton of wet basis white carbon black in the weak ammonia washing back with 1 ton 3%, remove the free ammonia in the white carbon black product, most of free ammonia is converted into Neutral ammonium fluoride;
(4) with 1 ton of wet basis white carbon black product in the rare silicofluoric acid washing back with 14 tons of water washings, further remove ammonia and micro-rare silicofluoric acid in the product, N content in the product is trace, substantially can not detect with common method, make dioxide-containing silica after drying and be 92.1 %, N content and be 0.07%, F content is 0.1%, the white carbon black product of non-stimulated nature and flavor.
Of the present inventionly be not limited to the embodiment described in the embodiment, those skilled in the art's technical scheme according to the present invention draws other embodiment, belongs to technological innovation scope of the present invention equally.Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (3)
1. a method that improves the white carbon black quality product comprises the steps:
(1) N content is 1-3%, and F content is that the wet basis white carbon black product of 1-4% is wet basis white carbon black quality product 3-4 2 countercurrent washings of rare ammonium fluoride solution doubly through quality;
(2) will be wet basis white carbon black quality product 3-4 weak ammonia washing doubly through the white carbon black product quality of countercurrent washing;
(3) with the rare silicofluoric acid washing of the white carbon black product after the weak ammonia washing with 1%-5%, the 0.4-0.7 that rare silicofluoric acid consumption is theoretical consumption doubly;
(4) the white carbon black product after rare silicofluoric acid washing is washed with water, the consumption of water is 10-14 ton/ton wet basis white carbon black product, further removes ammonia and micro-rare silicofluoric acid in the product;
(5) dry white carbon black product.
2. improve the method for white carbon black quality product according to claim 1, wherein: the mass concentration of water is 60-75% in the wet basis white carbon black product.
3. improve the method for white carbon black quality product as claimed in claim 1 or 2, wherein: make dioxide-containing silica more than or equal to 90%, N smaller or equal to 0.25%, F content is smaller or equal to 0.3% white carbon black product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5458864A (en) * | 1989-11-16 | 1995-10-17 | Nissan Chemical Industries Ltd. | Process for producing high-purity silica by reacting crude silica with ammonium fluoride |
| CN101585538A (en) * | 2008-05-23 | 2009-11-25 | 四川大学 | Method for preparing ultra-pure silicon dioxide micropowder |
| CN101708852A (en) * | 2009-09-04 | 2010-05-19 | 铁生年 | Method for purifying liquid phase silica recovered from solar polysilicon tail gas |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5458864A (en) * | 1989-11-16 | 1995-10-17 | Nissan Chemical Industries Ltd. | Process for producing high-purity silica by reacting crude silica with ammonium fluoride |
| CN101585538A (en) * | 2008-05-23 | 2009-11-25 | 四川大学 | Method for preparing ultra-pure silicon dioxide micropowder |
| CN101708852A (en) * | 2009-09-04 | 2010-05-19 | 铁生年 | Method for purifying liquid phase silica recovered from solar polysilicon tail gas |
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