CN105752991A - Method for preparing coarse granular potassium fluosilicate - Google Patents
Method for preparing coarse granular potassium fluosilicate Download PDFInfo
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- CN105752991A CN105752991A CN201610191955.9A CN201610191955A CN105752991A CN 105752991 A CN105752991 A CN 105752991A CN 201610191955 A CN201610191955 A CN 201610191955A CN 105752991 A CN105752991 A CN 105752991A
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- potassium fluosilicate
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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
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
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Abstract
The invention discloses a method for preparing coarse granular potassium fluosilicate.Utilized raw materials are purified respectively, potassium fluotitanate mother liquor is added into a reactor, stirring is conducted while preheating is conducted, purified fluosilicic acid liquid is added into the reactor for a reaction and synthesis, stirring is conducted, and stirring is continued after feeding is ended, so that the reaction can be fully conducted; a mixed solution obtained after the reaction is subjected to static settlement, a synthesis product is filtered, washed and dried, and a qualified potassium fluosilicate product is obtained.The preparation method is simple, no special equipment is needed, and good economical benefits are achieved; residual potassium in potassium fluosilicate production mother liquor is effectively recycled, and the wastewater treatment cost is reduced; a prepared product is large in particle and good in flowing property and has market competitiveness.
Description
Technical field
The present invention relates to chemical products production field, specifically the preparation method of a kind of coarse granule potassium fluosilicate.
Background technology
Potassium fluosilicate is mainly used in wood preservation, pottery manufactures and the insecticide of the smelting of aluminum and magnesium, agricultural, is also used for optical glass manufacture, synthetic mica and enamel manufacture etc..Existing potassium fluosilicate mainly originates from fluoride salt manufacturing enterprise and phosphorous chemical industry enterprise, at present, the useless potassium chloride that the hexafluosilicic acid producing employing phosphorous chemical industry or Acid of Hydrofluoric Acid Production enterprise by-product mostly and organic fluorination process of potassium fluosilicate produce reacts, generation potassium fluosilicate precipitates, and obtains potassium fluosilicate product after treatment.
Tradition potassium fluosilicate produces remaining a part of potassium compound in mother solution and cannot recycle, and amounts to content K2O6-8g/L；Traditional mode of production is with potassium chloride and hexafluosilicic acid for Material synthesis potassium fluosilicate, and granularity is very thin, is typically in about 325 mesh standard sieves.Owing to carefully, production being filtered the problem such as difficulty, product poor fluidity, main content instability thus causing.It is thus desirable to the production method of existing potassium fluosilicate is improved, to meet the needs of actual production.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of coarse granule potassium fluosilicate, with the problem solving to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of preparation method of coarse granule potassium fluosilicate, step is as follows:
(1) raw materials used purify respectively；
(2) by potassium fluotitanate mother solution, join in reactor, stirring while heated to preheating temperature 68～72 DEG C；
(3) the hexafluosilicic acid liquid after purified is joined reacting synthesis in reactor, synthesis temperature is 40～100 DEG C；
(4) the lower synthesis of stirring, generated time 2～6h；
(5) continue stirring 30～60min after reinforced end, make to react completely；
(6) reacted mixed solution is stood, precipitate 20～30min；
(7) synthetic product is through filtering, wash, drying, and obtains qualified potassium fluosilicate product.
As the further scheme of the present invention: further synthesis temperature is 60～80 DEG C.
The present invention is with the potassium fluotitanate (K containing potassium2TiF6) produce mother solution and fluorine silicon acid ion (SiF6 -) solution be raw material, react in a reservoir, reaction equation is as follows:
K2TiF6+SiF6 2-→K2SiF6+TiF6 -
2K++SiF6 2-→K2SiF6
In this course of reaction, potassium fluotitanate produces the potassium ion (K contained in mother solution+) and fluotitanic acid radical ion (TiF6 2-), potassium ion (K+) and hexafluosilicic acid radical ion (SiF6 -) reaction generation potassium fluosilicate precipitation, in the process producing potassium fluosilicate precipitation, by controlling the temperature of reaction, line preheats, it is further continued at 40～100 DEG C and reacts 2～6h, be further continued for stirring 30～60min, then staticly settle 20～30min, the potassium fluosilicate produced fully is precipitated and is accumulated into granule, thus preparing coarse grained potassium fluosilicate.
Compared with prior art, the invention has the beneficial effects as follows: preparation method provided by the present invention is simple, it is not necessary to special installation, there is good economic benefit；The effective potassium fluotitanate that reclaims produces potassium remaining in mother solution, makes the potassium content K of potassium fluosilicate mother liquor residue2O < 0.5g/L, reduces cost for wastewater treatment；Obtained product particle is big, and good fluidity possesses the market competitiveness.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
The preparation process of coarse granule potassium fluosilicate is as follows:
(1) raw materials used purify respectively；
(2) by potassium fluotitanate mother solution 1m3, wherein containing (meter) K2O=6.1g/L, join in reactor, stirring while heated to preheating temperature 70 C；
(3) the hexafluosilicic acid liquid after purified is joined reacting synthesis in reactor, synthesis temperature is 60 DEG C；
(4) the lower synthesis of stirring, generated time 4h；
(5) continue stirring 60min after reinforced end, make to react completely；
(6) reacted mixed solution is stood, precipitate 20min；
(7) synthetic product is through filtering, wash, drying, and obtains qualified potassium fluosilicate product.
Products obtained therefrom detects mutually through XRD thing and confirms as required product potassium fluosilicate, produces the main content 98% of potassium fluosilicate 14kg(wherein product ,+100 orders 44% ,+200 orders 91% ,-325 orders 6%), the potassium content K of potassium fluosilicate mother liquor residue2O is 0.17g/L.
Embodiment 2
The preparation process of coarse granule potassium fluosilicate is as follows:
(1) raw materials used purify respectively；
(2) by potassium fluotitanate mother solution 1m3, wherein containing (meter) K2O=6.1g/L, joins in reactor, stirring while heated to preheating temperature 70 C；
(3) the hexafluosilicic acid liquid after purified is joined reacting synthesis in reactor, synthesis temperature is 70 DEG C；
(4) the lower synthesis of stirring, generated time 3h；
(5) continue stirring 45min after reinforced end, make to react completely；
(6) undertaken staticly settling 25min by reacted mixed solution；
(7) synthetic product is through filtering, wash, drying, and obtains qualified potassium fluosilicate product
Products obtained therefrom detects mutually through XRD thing and confirms as required product potassium fluosilicate, produces the main content 99% of potassium fluosilicate 14kg(wherein product ,+100 orders 45% ,+200 orders 90% ,-325 orders 5%), the potassium content K of potassium fluosilicate mother liquor residue2O is 0.17g/L.
Embodiment 3
The preparation process of coarse granule potassium fluosilicate is as follows:
(1) raw materials used purify respectively；
(2) by potassium fluotitanate mother solution, join in reactor, stirring while heated to preheating temperature 70 C；
(3) the hexafluosilicic acid liquid after purified is joined reacting synthesis in reactor, synthesis temperature is 80 DEG C；
(4) the lower synthesis of stirring, generated time 2h；
(5) continue stirring 30min after reinforced end, make to react completely；
(6) reacted mixed solution is stood, precipitate 30min；
(7) synthetic product is through filtering, wash, drying, and obtains qualified potassium fluosilicate product.
Products obtained therefrom detects mutually through XRD thing and confirms as required product potassium fluosilicate, produces the main content 99% of potassium fluosilicate 14kg(wherein product ,+100 orders 42% ,+200 orders 94% ,-325 orders 5%), the potassium content K of potassium fluosilicate mother liquor residue2O is 0.17g/L.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when without departing substantially from the spirit of the present invention or basic feature, it is possible to realize the present invention in other specific forms.Therefore, no matter from which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the invention rather than described above limits, it is intended that all changes in the implication of the equivalency dropping on claim and scope included in the present invention.
Claims (2)
1. the preparation method of a coarse granule potassium fluosilicate, it is characterised in that step is as follows:
(1) raw materials used purify respectively；
(2) by potassium fluotitanate mother solution, join in reactor, stirring while heated to preheating temperature 68～72 DEG C；
(3) the hexafluosilicic acid liquid after purified is joined reacting synthesis in reactor, synthesis temperature is 40～100 DEG C；
(4) the lower synthesis of stirring, generated time 2～6h；
(5) continue stirring 30～60min after reinforced end, make to react completely；
(6) reacted mixed solution is stood, precipitate 20～30min；
(7) synthetic product is through filtering, wash, drying, and obtains qualified potassium fluosilicate product.
2. the preparation method of coarse granule potassium fluosilicate according to claim 1, it is characterised in that in described step (3), further synthesis temperature is 60～80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610191955.9A CN105752991A (en) | 2016-03-30 | 2016-03-30 | Method for preparing coarse granular potassium fluosilicate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610191955.9A CN105752991A (en) | 2016-03-30 | 2016-03-30 | Method for preparing coarse granular potassium fluosilicate |
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| CN105752991A true CN105752991A (en) | 2016-07-13 |
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| CN201610191955.9A Pending CN105752991A (en) | 2016-03-30 | 2016-03-30 | Method for preparing coarse granular potassium fluosilicate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211068A (en) * | 2014-09-18 | 2014-12-17 | 福建省漳平展鹏化工有限公司 | Preparation method of large granular potassium fluosilicate |
| CN105174269A (en) * | 2015-09-14 | 2015-12-23 | 福建省漳平市九鼎氟化工有限公司 | Process for recycling potassium fluosilicate in process of potassium fluotitanate production |
-
2016
- 2016-03-30 CN CN201610191955.9A patent/CN105752991A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211068A (en) * | 2014-09-18 | 2014-12-17 | 福建省漳平展鹏化工有限公司 | Preparation method of large granular potassium fluosilicate |
| CN105174269A (en) * | 2015-09-14 | 2015-12-23 | 福建省漳平市九鼎氟化工有限公司 | Process for recycling potassium fluosilicate in process of potassium fluotitanate production |
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Application publication date: 20160713 |
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