CN105883836A - Co-production method of sodium metasilicate and sodium fluoride - Google Patents
Co-production method of sodium metasilicate and sodium fluoride Download PDFInfo
- Publication number
- CN105883836A CN105883836A CN201610220270.2A CN201610220270A CN105883836A CN 105883836 A CN105883836 A CN 105883836A CN 201610220270 A CN201610220270 A CN 201610220270A CN 105883836 A CN105883836 A CN 105883836A
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- Prior art keywords
- sodium
- fluorine
- sodium fluoride
- sodium metasilicate
- mass percent
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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
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
Abstract
The invention discloses a co-production method of sodium metasilicate and sodium fluoride. The method comprises the following steps: a sodium hydroxide solution with the concentration being 15%-50% in percentage by mass and fluorine-containing silicon slag are mixed in the mass ratio being (1-6):1 and stirred to have a reaction for 15-150 min; after the reaction temperature is reduced to 50-60 DEG C, the mixed solution is filtered, and a filter cake and filtrate are obtained; the filter cake is washed with a sodium hydroxide solution with the concentration being 5%-15% in percentage by mass and process water sequentially and dried until the water content is 0-1.5% after washing, and a sodium fluoride product is obtained; the molar ratio of the filtrate is adjusted to be 1 with a conventional method, evaporated and concentrated until the concentration of sodium metasilicate is 55%-60% in percentage by mass and finally cooled, crystalized and dried with the conventional method, and a sodium metasilicate product is obtained. The co-production method has the characteristics of simple process, small device and little corrosion.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the production method of a kind of sodium metasilicate coproduction sodium fluoride.
Background technology
China Patent Publication No. CN101234763, invention entitled " white residue prepares the method for waterglass and sodium metasilicate " on August 6th, 2008 disclose a kind of utilize white residue and NaOH for raw material through reaction and concentration prepare waterglass and the method for metasilicic acid product, technique is simple；China Patent Publication No. CN1772608, invention entitled " utilizing the method that waste industrial silicone gel produces metasilicate pentahydrate sodium " on May 17th, 2006 disclose a kind of dissolves through NaOH with Industrial waste, decolour, concentrate, crystallize, the dry method preparing metasilicate pentahydrate sodium, cost is relatively low.Visible, in many published technical schemes, it is substantially and utilizes silica containing discarded object and NaOH reaction to prepare sodium metasilicate or sodium metasilicate.
Utilizing fluosilicic acid to produce in the technical process of hydrogen fluoride and can produce fluorine-containing white residue, fluorine therein is presented in fluosilicic acid or high silicic acid.Fluorine has free fluorine and lattice fluorine in white residue, the most long-term stacking, and the lattice fluorine in fluorine-containing white residue can gradually separate out from silicon dioxide lattice, and the corrosivity of fluosilicic acid is strong, can produce environment and pollute.At present, not yet having the recovery technology of lattice fluorine, the resource of fluorine-containing white residue recycles extremely urgent.And utilize fluorine-containing white residue to reclaim fluorine, silicon resource, prepare sodium metasilicate and the most not yet have been reported that.
Summary of the invention
It is an object of the invention to provide the production method of the sodium metasilicate coproduction sodium fluoride that a kind of technique is simple, device is little, corrosivity is little.
The production method of a kind of sodium metasilicate coproduction sodium fluoride of the present invention, comprises the following steps:
(1) sodium hydroxide solution that mass percent concentration is 15-50% is mixed according to mass ratio 1-6:1 with fluorine-containing white residue, stirring reaction 15-150min；
(2) when question response temperature is down to 50-60 DEG C, mixed solution is filtered, obtain filter cake and filtrate respectively；
(3) it is that the sodium hydroxide solution of 5-15%, fresh water (FW) wash that filter cake passes sequentially through mass percent concentration；The washing amount of described NaOH is 0.5-1.5 times of sodium fluoride yield, and described fresh water (FW) leaching requirement is 0.5-1.0 times of sodium fluoride yield；It is 0-1.5% by filtration cakes torrefaction to water content after washing, obtains sodium fluoride product；
(4) by filtrate mode transfer in conventional manner to modulus be 1, to be concentrated into sodium metasilicate mass percent concentration be 55-60% to re-evaporation, finally cool down through conventional method, crystallize, be dried, obtain sodium metasilicate product.
The production method of above-mentioned a kind of sodium metasilicate coproduction sodium fluoride, wherein: in described fluorine-containing white residue, the mass percent of fluorine is 5-25%.
The present invention is compared with prior art, there is obvious beneficial effect, as can be known from the above technical solutions: the production method of sodium metasilicate coproduction sodium fluoride provided by the present invention, sodium metasilicate is prepared for raw material with fluorine-containing white residue, while fluorine-containing white residue is carried out effective resource recycling, can also efficiently prepare sodium fluoride on the basis of producing high-quality sodium metasilicate, be killing three birds with one stone；This method does not the most produce refuse and waste gas in whole technical process, the separation of two kinds of products is the simplest, the waste water produced in production process can also recycle, as the wash water in the reaction raw materials in step (1) or step (3), obtained washings can have the advantages that production technology is simple, operation is convenient, corrosivity is little and environmental pollution is little again according to variable concentrations.
Detailed description of the invention
Embodiment
1
The production method of a kind of sodium metasilicate coproduction sodium fluoride, comprises the following steps:
(1) being mixed according to mass ratio 1:1 with fluorine-containing white residue by the sodium hydroxide solution that mass percent concentration is 15%, stirring reaction 15min, in described fluorine-containing white residue, the mass percent of fluorine is 5%；
(2) when question response temperature is down to 50 DEG C, mixed solution is filtered, obtain filter cake and filtrate respectively；
(3) filter cake passes sequentially through sodium hydroxide solution that mass percent concentration is 15%, fresh water (FW) washs；The washing amount of described NaOH is 1.5 times of sodium fluoride yield, and described fresh water (FW) leaching requirement is 1.0 times of sodium fluoride yield；It is 1.5% by filtration cakes torrefaction to water content after washing, obtains sodium fluoride product；
(4) by filtrate mode transfer in conventional manner to modulus be 1, to be concentrated into sodium metasilicate mass percent concentration be 55% to re-evaporation, finally cool down through conventional method, crystallize, be dried, obtain sodium metasilicate product.
Embodiment
2
The production method of a kind of sodium metasilicate coproduction sodium fluoride, comprises the following steps:
(1) being mixed according to mass ratio 6:1 with fluorine-containing white residue by the sodium hydroxide solution that mass percent concentration is 50%, stirring reaction 150min, in described fluorine-containing white residue, the mass percent of fluorine is 25%；
(2) when question response temperature is down to 60 DEG C, mixed solution is filtered, obtain filter cake and filtrate respectively；
(3) filter cake passes sequentially through sodium hydroxide solution that mass percent concentration is 5%, fresh water (FW) washs；The washing amount of described NaOH is 0.5 times of sodium fluoride yield, and described fresh water (FW) leaching requirement is 0.5 times of sodium fluoride yield；By filtration cakes torrefaction to moisture-free after washing, obtain sodium fluoride product；
(4) by filtrate mode transfer in conventional manner to modulus be 1, to be concentrated into sodium metasilicate mass percent concentration be 60% to re-evaporation, finally cool down through conventional method, crystallize, be dried, obtain sodium metasilicate product.
Embodiment
3
The production method of a kind of sodium metasilicate coproduction sodium fluoride, comprises the following steps:
(1) being mixed according to mass ratio 3.5:1 with fluorine-containing white residue by the sodium hydroxide solution that mass percent concentration is 32.5%, stirring reaction 82.5min, in described fluorine-containing white residue, the mass percent of fluorine is 15%；
(2) when question response temperature is down to 55 DEG C, mixed solution is filtered, obtain filter cake and filtrate respectively；
(3) filter cake passes sequentially through sodium hydroxide solution that mass percent concentration is 10%, fresh water (FW) washs；The washing amount of described NaOH is 1 times of sodium fluoride yield, and described fresh water (FW) leaching requirement is 0.75 times of sodium fluoride yield；It is 0.75% by filtration cakes torrefaction to water content after washing, obtains sodium fluoride product；
(4) be that i.e. to adjust the molar ratio of silica and sodium oxide molybdena be 1 to 1(by filtrate mode transfer in conventional manner to modulus), to be concentrated into sodium metasilicate mass percent concentration be 57.5% to re-evaporation, finally cool down through conventional method, crystallize, be dried, obtain sodium metasilicate product.
The above, it it is only presently preferred embodiments of the present invention, not the present invention is done any pro forma restriction, any without departing from technical solution of the present invention content, the any simple modification equivalent variations made above example according to the technical spirit of the present invention and modification, all still fall within the range of technical solution of the present invention.
Claims (2)
1. a production method for sodium metasilicate coproduction sodium fluoride, comprises the following steps:
(1) sodium hydroxide solution that mass percent concentration is 15-50% is mixed according to mass ratio 1-6:1 with fluorine-containing white residue, stirring reaction 15-150min；
(2) when question response temperature is down to 50-60 DEG C, mixed solution is filtered, obtain filter cake and filtrate respectively；
(3) it is that the sodium hydroxide solution of 5-15%, fresh water (FW) wash that filter cake passes sequentially through mass percent concentration；The washing amount of described NaOH is 0.5-1.5 times of sodium fluoride yield, and described fresh water (FW) leaching requirement is 0.5-1.0 times of sodium fluoride yield；It is 0-1.5% by filtration cakes torrefaction to water content after washing, obtains sodium fluoride product；
(4) by filtrate mode transfer in conventional manner to modulus be 1, to be concentrated into sodium metasilicate mass percent concentration be 55-60% to re-evaporation, finally cool down through conventional method, crystallize, be dried, obtain sodium metasilicate product.
The production method of a kind of sodium metasilicate coproduction sodium fluoride the most as claimed in claim 1, wherein: in described fluorine-containing white residue, the mass percent of fluorine is 5-25%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610220270.2A CN105883836A (en) | 2016-04-11 | 2016-04-11 | Co-production method of sodium metasilicate and sodium fluoride |
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| CN201610220270.2A CN105883836A (en) | 2016-04-11 | 2016-04-11 | Co-production method of sodium metasilicate and sodium fluoride |
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| CN105883836A true CN105883836A (en) | 2016-08-24 |
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| CN201610220270.2A Pending CN105883836A (en) | 2016-04-11 | 2016-04-11 | Co-production method of sodium metasilicate and sodium fluoride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698479A (en) * | 2017-01-24 | 2017-05-24 | 陈可 | Non-aqueous complete-dissolution refining method of sodium fluoride containing organic impurities |
| CN115893449A (en) * | 2022-11-29 | 2023-04-04 | 福建省龙德新能源有限公司 | Method for producing electronic-grade sodium fluoride from industrial-grade sodium-alkali mixed liquor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3968197A (en) * | 1969-05-29 | 1976-07-06 | Onoda Chemical Industry Company, Limited | Process for treating sodium silico fluoride |
| CN101717097A (en) * | 2009-11-11 | 2010-06-02 | 云南云天化国际化工股份有限公司 | Method for separating sodium fluoride crystals from silicon dioxide |
| CN104911715A (en) * | 2015-07-02 | 2015-09-16 | 瓮福（集团）有限责任公司 | Method for preparing calcium silicate crystal whisker from fluorine-contained silicon slag |
| CN105000563A (en) * | 2015-07-09 | 2015-10-28 | 贵州远盛钾业科技有限公司 | Method for preparing sodium fluosilicate by using fluorine-containing silicon slag |
-
2016
- 2016-04-11 CN CN201610220270.2A patent/CN105883836A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3968197A (en) * | 1969-05-29 | 1976-07-06 | Onoda Chemical Industry Company, Limited | Process for treating sodium silico fluoride |
| CN101717097A (en) * | 2009-11-11 | 2010-06-02 | 云南云天化国际化工股份有限公司 | Method for separating sodium fluoride crystals from silicon dioxide |
| CN104911715A (en) * | 2015-07-02 | 2015-09-16 | 瓮福（集团）有限责任公司 | Method for preparing calcium silicate crystal whisker from fluorine-contained silicon slag |
| CN105000563A (en) * | 2015-07-09 | 2015-10-28 | 贵州远盛钾业科技有限公司 | Method for preparing sodium fluosilicate by using fluorine-containing silicon slag |
Non-Patent Citations (3)
| Title |
|---|
| 乐志强 等: "《无机精细化学品手册》", 31 January 2001 * |
| 戴志成等: "《硅化合物的生产与应用》", 31 May 1994 * |
| 薛彦辉 等: ""氟硅酸钙法制氟化氢联产偏硅酸钠新工艺研究"", 《无机盐工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698479A (en) * | 2017-01-24 | 2017-05-24 | 陈可 | Non-aqueous complete-dissolution refining method of sodium fluoride containing organic impurities |
| CN106698479B (en) * | 2017-01-24 | 2017-12-12 | 陈一可 | The non-aqueous complete molten process for purification of sodium fluoride containing organic impurities |
| CN115893449A (en) * | 2022-11-29 | 2023-04-04 | 福建省龙德新能源有限公司 | Method for producing electronic-grade sodium fluoride from industrial-grade sodium-alkali mixed liquor |
| CN115893449B (en) * | 2022-11-29 | 2023-08-29 | 福建省龙德新能源有限公司 | Method for producing electronic grade sodium fluoride by using industrial grade sodium-alkali mixed solution |
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