CN104211068B - A kind of preparation method of macrobead potassium silicofluoride - Google Patents
A kind of preparation method of macrobead potassium silicofluoride Download PDFInfo
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- CN104211068B CN104211068B CN201410477110.7A CN201410477110A CN104211068B CN 104211068 B CN104211068 B CN 104211068B CN 201410477110 A CN201410477110 A CN 201410477110A CN 104211068 B CN104211068 B CN 104211068B
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Abstract
The invention belongs to the production technical field of Chemicals, be specifically related to a kind of preparation method of macrobead potassium silicofluoride.Preparation method is: first add potassium silicofluoride mother liquor to synthesis groove, drop into silicate fluoride solution and Klorvess Liquid at 70 DEG C, complete and feed intake for the first time; Then complete second time at 65 DEG C, 55 DEG C, 50 DEG C respectively by previous operation, for the third time, feed intake for the 4th time, the 5th time.Does is potassium silicofluoride grain graininess of the present invention
Description
Technical field
The invention belongs to the production technical field of Chemicals, be specifically related to a kind of preparation method of macrobead potassium silicofluoride.
Background technology
Potassium silicofluoride be mainly used in wood preservation, pottery manufacture and aluminium and magnesium smelting, agricultural sterilant, also for opticglass manufacture, synthetic mica and enamel manufacture etc.Existing potassium silicofluoride mainly originates from fluoride salt manufacturing enterprise and phosphorous chemical industry enterprise, at present, the useless Repone K that the production of potassium silicofluoride adopts the silicofluoric acid of phosphorous chemical industry or Acid of Hydrofluoric Acid Production enterprise by-product and organic fluorination process to produce mostly reacts, generation potassium silicofluoride precipitates, and obtains potassium silicofluoride product after treatment.
But traditional potassium silicofluoride production technique still exists some problems: 1) the production method productive rate of potassium silicofluoride is lower, the production yield of current potassium silicofluoride only has about 85%; 2) potassium silicofluoride product chloride ion content is higher; 3) product granularity is thin,
poor fluidity, dries and easily lumps, not easily dry, easy to change, and when oven dry, use, dust is large.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of macrobead potassium silicofluoride is provided.Preparation method provided by the present invention is simple, does not need specific installation, has good economic benefit; And mother liquid coming is recycled, reduce cost for wastewater treatment; Obtained product particle is large, and good fluidity, possesses the market competitiveness.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for macrobead potassium silicofluoride, comprises the following steps:
(1) first potassium silicofluoride mother liquor is added to synthesis groove;
(2) open steam, stir and be warming up to 70 DEG C;
(3) magnesium sulfate is added, open silicate fluoride solution and Klorvess Liquid feed valves simultaneously, mixing speed is regulated to be 30 ~ 40 revs/min, calibration charging capacity and rate of feeding feed intake, feed intake after terminating, continue stirring reaction after 5 ~ 10 minutes, stop stirring, standing sedimentation 7 ~ 12 minutes, releases supernatant liquid;
(4) regulate temperature of reaction to be 65 DEG C, complete second time by the operation of step (3) and feed intake;
(5) regulate temperature of reaction to be 60 DEG C, complete feeding intake for the third time by the operation of step (3);
(6) regulate temperature of reaction to be 55 DEG C, complete the 4th time by the operation of step (3) and feed intake;
(7) regulate temperature of reaction to be 50 DEG C, complete the 5th time by the operation of step (3) and feed intake, continue stirring reaction, when temperature is down to 40 DEG C, stop stirring standing sedimentation 10 ~ 20 minutes, release supernatant liquid, open baiting valve, open and stir blowing;
(8) open suction filtration machine suction filtration, after mother liquor pumps, put into clear water and rinse to material to be white, then to carry out centrifugal drying operation;
(9) concentration of fluorine in wastewater silicic acid and Repone K in periodic detection potassium silicofluoride crystallizing pond, control fluorine in wastewater silicate content 0.1wt% ~ 0.5wt%, silicone content is 0.02wt% ~ 0.06wt%.
The massfraction of described silicate fluoride solution is 10 ~ 30%, and the massfraction of Klorvess Liquid is 12 ~ 25%, silicofluoric acid in amount of substance excess coefficient for 1.01 ~ 1.2; The rate of feeding of silicate fluoride solution is 15-30kg/ minute, and the rate of feeding of Klorvess Liquid is 15-30kg/ minute.
Potassium silicofluoride mother liquor described in step (1) is that step (8) suction filtration obtains; Silicofluoric acid content 0.1wt% ~ 0.5wt% in mother liquor, fluohydric acid content is 0.01wt% ~ 0.05wt%, and KCE content is 0.01wt% ~ 0.8wt%.
In step (3), (4), (5), (6), (7), the consumption of additive is the 1%-5% of product potassium silicofluoride Theoretical Mass.
In step (3), at the end of reaction, silicate fluoride solution, Klorvess Liquid feed intake complete simultaneously.
Step (3), (4), (5), (6), (7) reinforced process do not need out steam heating to keep temperature.
Step (8) drying temperature≤320 DEG C.
The macrobead potassium silicofluoride that preparation method as above obtains, the purity of potassium silicofluoride product is greater than 98wt%, and grain graininess is:
yield is for being greater than 92%.
Beneficial effect of the present invention is:
1, potassium silicofluoride grain graininess of the present invention is
, have in production operation and be convenient to suction filtration, be convenient to during oven dry dry, do not lump, nondiscoloration;
2, oarse-grained potassium silicofluoride is more suitable for for fields such as opticglass manufactures, and good fluidity, is evenly distributed, and during use, dust is few, possesses the market competitiveness;
3, in synthesis groove, drop into silicofluoric acid, Klorvess Liquid several times in preparation technology, be conducive to replacement(metathesis)reaction and fully carry out, improve the yield of product, yield is greater than 92%; And mother liquid coming to be carried out time
Receive and utilize, reduce cost for wastewater treatment, possess the market competitiveness.
Embodiment
The present invention's the following example further illustrates the present invention, but protection scope of the present invention is not limited to the following example.
The situation that table 1 embodiment 1-3 feeds intake (5 times)
embodiment 1
A preparation method for macrobead potassium silicofluoride, comprises the following steps:
(1) first 200kg potassium silicofluoride mother liquor is added to synthesis groove;
(2) open steam, stir and be warming up to 70 DEG C;
(3) add magnesium sulfate, open silicate fluoride solution and Klorvess Liquid feed valves, turn on agitator simultaneously, regulate mixing speed to be 30 revs/min, calibration charging capacity and rate of feeding, the rate of feeding of silicofluoric acid is 21.1kg/ minute, the rate of feeding of Repone K is 20kg/ minute, feeds intake after terminating; Continue stirring reaction after 5 minutes, stop stirring, standing sedimentation 7 minutes, releases supernatant liquid;
(4) regulate temperature of reaction to be 65 DEG C, complete second time by the operation of step (3) and feed intake;
(5) regulate temperature of reaction to be 60 DEG C, complete feeding intake for the third time by the operation of step (3);
(6) regulate temperature of reaction to be 55 DEG C, complete the 4th time by the operation of step (3) and feed intake;
(7) regulate temperature of reaction to be 50 DEG C, complete the 5th time by the operation of step (3) and feed intake, continue stirring reaction, when temperature is down to 40 DEG C, stop stirring standing sedimentation 10 minutes, release supernatant liquid, open baiting valve, open and stir blowing;
(8) open suction filtration machine suction filtration, after mother liquor pumps, put into clear water and rinse to material to be white, then to carry out centrifugal drying (300 DEG C) operation;
(9) concentration of silicofluoric acid and Repone K in mother liquid coming in periodic detection potassium silicofluoride crystallizing pond, controls fluorine in wastewater silicate content 0.1wt% ~ 0.5wt%;
The massfraction of the silicate fluoride solution described in step (3) is 17.15%, and the massfraction of Klorvess Liquid is 16.4%;
The charging capacity of step (3), (4), (5), (6), (7) is silicofluoric acid 872kg, Repone K 826kg.
embodiment 2
A preparation method for macrobead potassium silicofluoride, comprises the following steps:
(1) first 200kg potassium silicofluoride mother liquor is added to synthesis groove;
(2) open steam, stir and be warming up to 70 DEG C;
(3) magnesium sulfate is added, open silicate fluoride solution and Klorvess Liquid feed valves simultaneously, turn on agitator, regulates mixing speed to be 40 revs/min, calibration charging capacity and rate of feeding, the rate of feeding of silicofluoric acid is 28.31kg/ minute, the rate of feeding of Repone K is 15kg/ minute, feeds intake after terminating, and stops stirring, standing sedimentation 10 minutes, releases supernatant liquid;
(4) regulate temperature of reaction to be 65 DEG C, complete second time by the operation of step (3) and feed intake;
(5) regulate temperature of reaction to be 60 DEG C, complete feeding intake for the third time by the operation of step (3);
(6) regulate temperature of reaction to be 55 DEG C, complete the 4th time by the operation of step (3) and feed intake;
(7) regulate temperature of reaction to be 50 DEG C, complete the 5th time by the operation of step (3) and feed intake, continue stirring reaction, when temperature is down to 40 DEG C, stop stirring standing sedimentation 15 minutes, release supernatant liquid, open baiting valve, open and stir blowing;
(8) open suction filtration machine suction filtration, after mother liquor pumps, put into clear water and rinse to material to be white, then to carry out centrifugal drying (280 DEG C) operation;
(9) concentration of silicofluoric acid and Repone K in mother liquid coming in periodic detection potassium silicofluoride crystallizing pond, control fluorine in wastewater silicate content 0.1wt% ~ 0.5wt%, silicone content is 0.02wt% ~ 0.06wt%;
The massfraction of the silicate fluoride solution described in step (3) is 18.82%, and the massfraction of Klorvess Liquid is 23.3%;
The charging capacity of step (3), (4), (5), (6), (7) is silicofluoric acid 872kg and Repone K 616kg.
embodiment 3
A preparation method for macrobead potassium silicofluoride, comprises the following steps:
(1) first 300kg potassium silicofluoride mother liquor is added to synthesis groove;
(2) open steam, stir and be warming up to 70 DEG C;
(3) magnesium sulfate is added, open silicate fluoride solution and Klorvess Liquid feed valves, turn on agitator simultaneously, regulate mixing speed to be 35 revs/min, calibration charging capacity and rate of feeding, the rate of feeding of silicofluoric acid is 15kg/ minute, and the rate of feeding of Repone K is 15.5kg/ minute, feeds intake after terminating, continue stirring reaction after 7 minutes, stop stirring, standing sedimentation 12 minutes, releases supernatant liquid;
(4) regulate temperature of reaction to be 65 DEG C, complete second time by the operation of step (3) and feed intake;
(5) regulate temperature of reaction to be 60 DEG C, complete feeding intake for the third time by the operation of step (3);
(6) regulate temperature of reaction to be 55 DEG C, complete the 4th time by the operation of step (3) and feed intake;
(7) regulate temperature of reaction to be 50 DEG C, complete the 5th time by the operation of step (3) and feed intake, continue stirring reaction, when temperature is down to 40 DEG C, stop stirring standing sedimentation 20 minutes, release supernatant liquid, open baiting valve, open and stir blowing;
(8) open suction filtration machine suction filtration, after mother liquor pumps, put into clear water and rinse to material to be white, then to carry out centrifugal drying (250 DEG C) operation;
(9) concentration of silicofluoric acid and Repone K in mother liquid coming in periodic detection potassium silicofluoride crystallizing pond, controls fluorine in wastewater silicate content 0.1wt% ~ 0.5wt%;
The massfraction of the silicate fluoride solution described in step (3) is 17.8%, and the massfraction of Klorvess Liquid is 16%;
The charging capacity of step (3), (4), (5), (6), (7) is silicofluoric acid 821kg and Repone K 846kg.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (8)
1. a preparation method for macrobead potassium silicofluoride, is characterized in that: comprise the following steps:
(1) first potassium silicofluoride mother liquor is added to synthesis groove;
(2) open steam, stir and be warming up to 70 DEG C;
(3) magnesium sulfate is added, open silicate fluoride solution and Klorvess Liquid feed valves simultaneously, mixing speed is regulated to be 30 ~ 40 revs/min, calibration charging capacity and rate of feeding feed intake, feed intake after terminating, then continue stirring reaction after 5 ~ 10 minutes, stop stirring, standing sedimentation 7 ~ 12 minutes, releases supernatant liquid;
(4) regulate temperature of reaction to be 65 DEG C, complete second time by the operation of step (3) and feed intake;
(5) regulate temperature of reaction to be 60 DEG C, complete feeding intake for the third time by the operation of step (3);
(6) regulate temperature of reaction to be 55 DEG C, complete the 4th time by the operation of step (3) and feed intake;
(7) regulate temperature of reaction to be 50 DEG C, complete the 5th time by the operation of step (3) and feed intake, continue stirring reaction, when temperature is down to 40 DEG C, stop stirring standing sedimentation 10 ~ 20 minutes, release supernatant liquid, open baiting valve, open and stir blowing;
(8) open suction filtration machine suction filtration, after mother liquor pumps, put into clear water and rinse to material to be white, then to carry out centrifugal drying operation.
2. the preparation method of macrobead potassium silicofluoride according to claim 1, is characterized in that: the potassium silicofluoride mother liquor described in step (1) is that step (8) suction filtration obtains; Silicofluoric acid content 0.1wt% ~ 0.5wt% in mother liquor, fluohydric acid content is 0.01wt% ~ 0.05wt%, and KCE content is 0.01wt% ~ 0.8wt%.
3. the preparation method of macrobead potassium silicofluoride according to claim 1, it is characterized in that: the massfraction of the silicate fluoride solution described in step (3) is 10 ~ 30%, the massfraction of Klorvess Liquid is 12 ~ 25%, silicofluoric acid in amount of substance excess coefficient for 1.01 ~ 1.2; The rate of feeding of silicate fluoride solution is 15-30kg/ minute, and the rate of feeding of Klorvess Liquid is 15-30kg/ minute.
4. the preparation method of macrobead potassium silicofluoride according to claim 1, is characterized in that: the quality such as number is that feed intake of step (3), (4), (5), (6), (7).
5. the preparation method of macrobead potassium silicofluoride according to claim 1, is characterized in that: in step (3) (4), (5), (6), (7), the consumption of magnesium sulfate is respectively the 1%-5% of product potassium silicofluoride Theoretical Mass.
6. the preparation method of macrobead potassium silicofluoride according to claim 1, is characterized in that: in step (3), and at the end of reaction, silicate fluoride solution, Klorvess Liquid feed intake complete simultaneously.
7. the preparation method of macrobead potassium silicofluoride according to claim 1, is characterized in that: in step (3), (4), (5), (6), (7) reinforced process, do not need steam heating to keep temperature.
8. the preparation method of macrobead potassium silicofluoride according to claim 1, is characterized in that: step (8) drying temperature≤320 DEG C.
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| CN105174269B (en) * | 2015-09-14 | 2017-07-28 | 福建省漳平市九鼎氟化工有限公司 | A kind of technique that potassium fluosilicate is reclaimed in potassium fluotitanate production process |
| CN105752991A (en) * | 2016-03-30 | 2016-07-13 | 云南铁坦新材料科技股份有限公司 | Method for preparing coarse granular potassium fluosilicate |
| CN111675223A (en) * | 2020-07-24 | 2020-09-18 | 昆明合起工贸有限公司 | Production process of manganese fluosilicate |
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| CN1396113A (en) * | 2002-07-03 | 2003-02-12 | 夏克立 | Process for continuously preparing big-crystal sodium (or potassium) fluosilicate |
| CN101708832A (en) * | 2009-11-02 | 2010-05-19 | 山东红日阿康化工股份有限公司 | Method for producing defluorinated ammonium phosphate |
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Effective date of registration: 20180606 Address after: 365002 yellow sand new material industrial park, three yuan, Sanming City, Fujian Patentee after: Fujian Sanming Jin Fluorine Chemical Technology Co., Ltd. Address before: 364400 Building 5, East Hang Hang Road, Zhangping, Longyan, Fujian Province, 5 Patentee before: FUJIAN ZHANGPING ZHANPENG CHEMICAL CO., LTD. |
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