CN105439150A - Method for preparing sodium fluosilicate by adopting potassium feldspar decomposed gas absorption liquid - Google Patents
Method for preparing sodium fluosilicate by adopting potassium feldspar decomposed gas absorption liquid Download PDFInfo
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- CN105439150A CN105439150A CN201510851097.1A CN201510851097A CN105439150A CN 105439150 A CN105439150 A CN 105439150A CN 201510851097 A CN201510851097 A CN 201510851097A CN 105439150 A CN105439150 A CN 105439150A
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- potassium feldspar
- absorption liquid
- gas absorption
- sodium silicofluoride
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Abstract
The invention relates to a method for preparing sodium fluosilicate by adopting a potassium feldspar decomposed gas absorption liquid. The method comprises the following steps: potassium feldspar, fluorite and concentrated sulfuric acid are taken as the raw materials for preparation of silicon fluoride gas, then the silicon fluoride gas is subjected to hydrolysis and absorption, fluosilicic acid is prepared, fluosilicic acid and sodium chloride react with a precipitation method to produce a finished sodium fluosilicate product. One novel technology for preparing sodium fluosilicate is provided, the potassium feldspar resource utilization rate is increased, and the preparation technology is simple.
Description
Technical field
The present invention relates to a kind of method preparing Sodium Silicofluoride, specifically, relate to the method utilizing potassium feldspar decomposition gas absorption liquid to prepare Sodium Silicofluoride.
Background technology
The potash feldspar ore reserves of China are extremely abundant, mainly be distributed in the provinces such as Yunnan, Guizhou, Sichuan, containing the abundant composition such as potassium, aluminium, silicon in potassium felspar sand, and under normal temperature, only have HF can break the lattice of potassium felspar sand, so usually adopt fluorine-containing auxiliary agent to carry out decomposing of potassium feldspar in potassium feldspar decomposition technique, process often produces the acidic solutions such as silicofluoric acid.And in China, because fluorine resource belongs to national strategy reserved resources, country has also carried out quota restriction measure to the exploitation of fluorine resource.And, carrying out the producer produced for utilizing potassium felspar sand resource, also must reclaim fluorine and realizing recycle and could reduce enterprise's production cost, reduce the waste of fluorine resource.
Sodium Silicofluoride is building, the maximum silicofluoride kind of building materials industry consumption, is extensively used as coagulant aids, solubility promoter and additive and uses.The processing method that tradition prepares Sodium Silicofluoride normally utilizes in sodium carbonate and the method for silicofluoric acid obtains described Sodium Silicofluoride, and complex process, utilization rate of raw materials are not high.
Summary of the invention
The technical solution adopted in the present invention is: utilize potassium feldspar decomposition gas absorption liquid to prepare the method for Sodium Silicofluoride, specifically comprise the following steps:
Step one, join in reactor by potassium felspar sand, fluorite, the vitriol oil successively, react under temperature is 200 DEG C ~ 300 DEG C and autogenous pressure, generate gas and solid residue, its reaction principle is:
CaF
2+H
2SO
4=2HF↑+CaSO
4，
2K[AlSi
3O
8]+24HF+4H
2SO
4=K
2SO
4+Al
2(SO
4)
3+6SiF
4+16H
2O，
Wherein, the mass ratio of potassium felspar sand, fluorite, the vitriol oil is 1:3 ~ 3.5:3.5 ~ 4, and the vitriol oil that the vitriol oil is 98% by massfraction calculates;
Step 2, under condition of negative pressure, volume ratio is adopted by described gas to be that the industrial alcohol of 1:3 ~ 5 and the mixing solutions of water carry out absorption hydrolysis, controlled hydrolysis temperature is at 5 DEG C ~ 10 DEG C, obtain filtrate and precipitated product through ageing, filtration after hydrolysis terminates, its reaction principle is mainly:
3SiF
4+2H
2O=2H
2SiF
6+SiO
2↓；
Step 3, under temperature is 5 DEG C ~ 10 DEG C conditions, adding massfraction in described filtrate after filtering to described step 2 is that 20% ~ 35% sodium-chlor reacts, control pH=4 ~ 5 of reaction soln, obtain Sodium Silicofluoride through ageing, filtration, oven dry after reaction terminates, its reaction principle is mainly:
H
2SiF
6+2NaCl=Na
2SiF
6↓+2HCl。
Based on above-mentioned, under temperature is 90 DEG C ~ 110 DEG C conditions, adopt massfraction be 8% ~ 10% sulphuric acid soln the described solid residue in described step one is leached, slurries after leaching obtain leaching filtered liquid after filtering, crystal seed stirring and dissolving is added to described leaching filtered liquid, slowly be down to room temperature and carry out ageing, generate calcium sulfate crystal whiskers, after filtration, dry obtained calcium sulfate crystal whiskers byproduct.
Based on above-mentioned, the described precipitated product obtained in described step 2 is obtained white carbon black byproduct after washing, oven dry.
Hinge structure of the present invention has outstanding substantive distinguishing features and significant progress, specifically, the present invention is directed to the problem that element silicon that potassium felspar sand contains belongs to insoluble potassium resource, a kind of fluorine-containing auxiliary agent decomposing of potassium feldspar is proposed, reacted gas is generated silicofluoric acid after dehydrated alcohol and water absorb, then adopt sodium-chlor and silicofluoric acid to react, and then generate Sodium Silicofluoride finished product.The invention provides a kind of thinking producing Sodium Silicofluoride newly, solve the problem that China utilizes the fluorine resource reclaim in the long decomposition course of potassium, production process produces without the three wastes, and energy consumption is low, output is high, the rate of recovery is high, achieves production serialization.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
The present embodiment provides the method utilizing potassium feldspar decomposition gas absorption liquid to prepare Sodium Silicofluoride, and concrete steps comprise:
Step one, join in converter reactor by potassium felspar sand, Neutral ammonium fluoride, the vitriol oil successively, react under temperature is 200 DEG C and autogenous pressure, generate gas and solid residue, its reaction principle is:
CaF
2+H
2SO
4=2HF↑+CaSO
4，
2K[AlSi
3O
8]+24HF+4H
2SO
4=K
2SO
4+Al
2(SO
4)
3+6SiF
4+16H
2O，
Wherein, the mass ratio of potassium felspar sand, Neutral ammonium fluoride, the vitriol oil is 1:3.5:4, and the vitriol oil that the vitriol oil is 98% by massfraction calculates;
Step 2, under temperature is 10 DEG C and condition of negative pressure, adopt volume ratio to be that the industrial alcohol of 1:5 and the mixing solutions of water carry out absorptions hydrolysis to described gas, obtain filtrate and precipitated product through ageing, filtration after hydrolysis terminates, its reaction principle is mainly:
3SiF
4+2H
2O=2H
2SiF
6+SiO
2↓；
Step 3, under temperature is 10 DEG C of conditions, in described step 2 filter after described filtrate in add massfraction be 20% sodium-chlor react, control the pH=5 of reaction soln, obtain Sodium Silicofluoride through ageing, filtration, oven dry after reaction terminates, its reaction principle is mainly:
H
2SiF
6+2NaCl=Na
2SiF
6↓+2HCl。
Embodiment 2
The present embodiment provides the method utilizing potassium feldspar decomposition gas absorption liquid to prepare Sodium Silicofluoride, and concrete steps are roughly the same with embodiment 1, and difference is:
Step one, join in converter reactor by potassium felspar sand, Neutral ammonium fluoride, the vitriol oil successively, react under temperature is 250 DEG C and autogenous pressure, generate gas and solid residue, its reaction principle is,
CaF
2+H
2SO
4=2HF↑+CaSO
4，
2K[AlSi
3O
8]+24HF+4H
2SO
4=K
2SO
4+Al
2(SO
4)
3+6SiF
4+16H
2O，
Wherein, the mass ratio of potassium felspar sand, Neutral ammonium fluoride, the vitriol oil is 1:3.3:4, and the vitriol oil that the vitriol oil is 98% by massfraction calculates.Described solid residue is at 110 DEG C, and employing massfraction is the sulphuric acid soln leaching of 10%, and the slurries after leaching obtain filtered liquid after filtering, crystal seed stirring and dissolving is added to described filtered liquid, slowly be down to room temperature and carry out ageing, generate calcium sulfate crystal whiskers, after filtration, dry obtained calcium sulfate crystal whiskers;
Step 2, under temperature is 5 DEG C and condition of negative pressure, volume ratio is adopted to be that the industrial alcohol of 1:4 and the mixing solutions of water carry out absorption hydrolysis to the described gas that described step one generates, filtrate and precipitated product is obtained through ageing, filtration after hydrolysis terminates, described precipitated product is obtained white carbon black byproduct after washing, oven dry, and its reaction principle is mainly:
3SiF
4+2H
2O=2H
2SiF
6+SiO
2↓。
Embodiment 3
The present embodiment provides the method utilizing potassium feldspar decomposition gas absorption liquid to prepare Sodium Silicofluoride, concrete steps are roughly the same with embodiment 1, and difference is: in the described step one of the present embodiment, the mass ratio of potassium felspar sand, fluorite, the vitriol oil is 1:3:3.5; Absorption liquid employing volume ratio in described step 2 is industrial alcohol and the water mixed solution of 1:3, and controlled hydrolysis temperature is 10 DEG C.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (3)
1. utilize potassium feldspar decomposition gas absorption liquid to prepare the method for Sodium Silicofluoride, specifically comprise the following steps:
Step one, successively potassium felspar sand, fluorite, the vitriol oil are joined in reactor, react under temperature is 200 DEG C ~ 300 DEG C and autogenous pressure, generate gas and solid residue, wherein, the mass ratio of potassium felspar sand, fluorite, the vitriol oil is 1:3 ~ 3.5:3.5 ~ 4;
Step 2, under condition of negative pressure, to be adopted by described gas volume ratio to be that the industrial alcohol of 1:3 ~ 5 and the mixing solutions of water carry out absorption hydrolysis, controlled hydrolysis temperature is 5 DEG C ~ 10 DEG C, after hydrolysis terminates through ageing, filter and obtain filtrate and precipitated product;
Step 3, under temperature is 5 DEG C ~ 10 DEG C conditions, adding massfraction in the described filtrate after filtering to described step 2 is that 20% ~ 35% sodium chloride aqueous solution reacts, and obtains Sodium Silicofluoride after reaction terminates through ageing, filtration, oven dry.
2. the method utilizing potassium feldspar decomposition gas absorption liquid to prepare Sodium Silicofluoride according to claim 1, it is characterized in that, it is also included in temperature is under 90 DEG C ~ 110 DEG C conditions, adopt massfraction be 8% ~ 10% sulphuric acid soln the described solid residue in described step one is leached, slurries after leaching obtain leaching filtered liquid after filtering, crystal seed stirring and dissolving is added to described leaching filtered liquid, slowly be down to room temperature and carry out ageing, generate calcium sulfate crystal whiskers, after filtration, dry obtained calcium sulfate crystal whiskers byproduct.
3. the method utilizing potassium feldspar decomposition gas absorption liquid to prepare Sodium Silicofluoride according to claim 1, is characterized in that, the described precipitated product obtained in described step 2 is obtained white carbon black byproduct after washing, oven dry.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103145131A (en) * | 2013-02-26 | 2013-06-12 | 贵州金正大生态工程有限公司 | Resource comprehensive utilization method for recovering fluorine from wet-process phosphoric acid |
| CN103172074A (en) * | 2013-01-17 | 2013-06-26 | 洛阳氟钾科技有限公司 | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization |
| CN103274418A (en) * | 2013-06-27 | 2013-09-04 | 重庆龙瑞化工有限公司 | Method for preparing sodium fluosilicate with industrial wastes, namely fluosilicic acid and sodium chloride |
-
2015
- 2015-11-30 CN CN201510851097.1A patent/CN105439150A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103172074A (en) * | 2013-01-17 | 2013-06-26 | 洛阳氟钾科技有限公司 | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization |
| CN103145131A (en) * | 2013-02-26 | 2013-06-12 | 贵州金正大生态工程有限公司 | Resource comprehensive utilization method for recovering fluorine from wet-process phosphoric acid |
| CN103274418A (en) * | 2013-06-27 | 2013-09-04 | 重庆龙瑞化工有限公司 | Method for preparing sodium fluosilicate with industrial wastes, namely fluosilicic acid and sodium chloride |
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