CN105000563A - Method for preparing sodium fluosilicate by using fluorine-containing silicon slag - Google Patents
Method for preparing sodium fluosilicate by using fluorine-containing silicon slag Download PDFInfo
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- CN105000563A CN105000563A CN201510400070.0A CN201510400070A CN105000563A CN 105000563 A CN105000563 A CN 105000563A CN 201510400070 A CN201510400070 A CN 201510400070A CN 105000563 A CN105000563 A CN 105000563A
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Abstract
The invention relates to industrial waste slag comprehensive utilization technologies, and specifically relates to a method for preparing sodium fluosilicate by using fluorine-containing silicon slag. The method comprises: fulling mixing the fluorine-containing silicon slag and sodium hydroxide with a concentration of 5% to 30%, adjusting microwave power to a metal temperature of 70 to 120 DEG C for microwave reaction for 3 to 60 min, and after a cooling temperature is 30 to 55 DEG C, obtaining solid sodium fluosilicate after solid-liquid separation and drying treatment . According to the process of the invention, waste fluorine-containing silicon slag is combined with the microwave technology, and sodium fluosilicate is generated in one step. Production costs are low and the process is simple, and harm of acidic silicon slag on the environment is eliminated. The invention is low-carbon environmental, and actually achieve an effect of fluorine-containing silicon slag environment friendly and high effective utilization and development.
Description
Technical field
The present invention relates to a kind of method that fluorine-containing white residue prepares Sodium Silicofluoride, belong to chemical production technical field.
Background technology
All the fluoro-gas such as a large amount of silicon tetrafluoride, hydrogen fluoride can be produced in the process of Rock Phosphate (72Min BPL) decomposition, Phosphoric Acid Concentration, potassium bearing rock process, hydrogen fluoride production, enterprise of large department adopts water to absorb and generates fluorine-containing white residue at present, but this method produces a large amount of white residue piles up, and then cause serious environmental issue, so the recycling of fluoro-gas becomes problem demanding prompt solution.
Sodium Silicofluoride has good application market, and it is applied to building materials field, can be used as moisture adsorbent, retardant, sanitas etc.; Be applied to latex product field, can be used as opacifier, fusing assistant etc.; Be applied to agriculture field, can be used as sterilant, therefore, Sodium Silicofluoride has good work, agricultural application is worth.
At present, in the existing production technology of Sodium Silicofluoride, auxiliary reagent is many, produces a large amount of trade effluent, and processing step is complicated, and preparation condition is harsh.As the patent No. for disclose albite treated, point solve fluoro-gas, again through hydrolysis, acidleach, obtain pickling liquor, through crystallization and sodium sulfate hybrid reaction, utilize gravity settling technology to carry out being separated, drying treatment, obtain Sodium Silicofluoride product, this method cost is low, pollute little, but product quality is poor, performance is low.
For solving the problems of the technologies described above, this technique is that the recycling of fluoro-gas and the production of Sodium Silicofluoride provide a kind of new approaches.
Summary of the invention
For solving the problem of complex utilization of prior art problem and related industries waste residue, this technique adopts microwave reaction technique, and a step generates Sodium Silicofluoride.
Its technical scheme, comprises the following steps:
(1) be that 5%-30% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to be under the condition of 70-120 DEG C to material temperature, carry out microwave reaction 3-60min;
(2) product of microwave reaction being cooled to temperature is after 30-55 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after 1-8 washing, drying step, obtains Sodium Silicofluoride.
Described fluorine-containing white residue is the fluoro-gas produced in Rock Phosphate (72Min BPL) decomposition, Phosphoric Acid Concentration, potassium bearing rock process, hydrogen fluoride production process, through absorbing process, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:1-8, and the mix and blend time is 5-70min.
Described microwave power is 1-25kw, and the microwave reaction time is 5-20min.
Described solid-liquid separation adopts centrifugation.
The described centrifugation time is 10-30min, and rotating speed is 5000-10000r/min; The preferred centrifugation time is 18min, and rotating speed is 8000r/min.
In described step (2), liquid is sodium aluminum fluoride, Sodium Fluoride product.
Described washing adopts deionized water or distilled water to wash.
Described time of drying is 1-5h, and drying temperature is 50-130 DEG C.
Beneficial effect of the present invention
The present invention utilizes microwave technology, the fluorine-containing white residue of one step process generates Sodium Silicofluoride, substantially reduce the reaction times, reduce energy consumption, wherein microwave power, effective control of microwave time and material temperature, promote storeroom reaction, the result of Sodium Silicofluoride content is detected in conjunction with traditional detection mode, the Sodium Silicofluoride content of this product reaches more than 99%, far above Sodium Silicofluoride prepared by traditional method, in summary, Sodium Silicofluoride prepared by the present invention has product benefit of fine quality, again because the present invention utilizes the fluorine-containing white residue of trade waste to prepare Sodium Silicofluoride, reduce raw materials cost, fluorine resource in waste is effectively recycled, so the invention enables fluorine-containing white residue to utilize with obtaining efficient low energy.
The present invention is by appropriately adjusting technical parameter in processing step and related process, the mass volume ratio of the fluorine-containing white residue of strict control and sodium hydroxide is 1:1-8, make the reaction of fluorine-containing white residue and sodium hydroxide more abundant, enhance particle Interaction Force, and then Improving The Quality of Products; The present invention carries out solid-liquid separation after product cooling, is conducive to the abundant reaction between material; The present invention adopts deionized water to wash, effective removal product surface ionic impurity, adopt distilled water to wash, can free acid content be reduced, in conjunction with the quality measurements of Sodium Silicofluoride, this product Sodium Silicofluoride content is far above traditional method for making, free acid content about about 0.15%, reach Sodium Silicofluoride one-level quality, dry technology state modulator plays stable product structure, so this product has good quality-guarantee.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the fluorine-containing white residue of the present invention prepares Sodium Silicofluoride.
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Embodiment 1
Fluorine-containing white residue prepares a method for Sodium Silicofluoride, and it comprises the following steps:
(1) be that 28% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to be, under 16kw is the condition of 71 DEG C to material temperature, carry out microwave reaction 6min;
(2) product of microwave reaction being cooled to temperature is after 48 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after dry 3h under 7 washings, temperature are 70 DEG C of conditions, obtains Sodium Silicofluoride.
Described fluorine-containing white residue is the fluoro-gas produced in potassium bearing rock treating processes, through absorbing process, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:6, and the mix and blend time is 7min.
Described solid-liquid separation adopts centrifugation.
The described centrifugation time is 13min, and rotating speed is 5500r/min.
In described step (2), liquid is sodium aluminum fluoride, Sodium Fluoride product.
Described washing adopts distilled water water to wash.
In described Sodium Silicofluoride, Sodium Silicofluoride content (butt meter) is 99.3%, and free acid content is 0.13%.
Embodiment 2
Fluorine-containing white residue prepares a method for Sodium Silicofluoride, and it comprises the following steps:
(1) be that 17% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to be, under 3kw is the condition of 118 DEG C to material temperature, carry out microwave reaction 10min;
(2) product of microwave reaction being cooled to temperature is after 32 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after dry 1h under 3 washings, temperature are 100 DEG C of conditions, obtains Sodium Silicofluoride.
Described fluorine-containing white residue is the fluoro-gas produced in hydrogen fluoride production process, through absorbing process, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:6, and the mix and blend time is 55min.
Described solid-liquid separation adopts centrifugation.
The described centrifugation time is 23min, and rotating speed is 7000r/min.
In described step (2), liquid is sodium aluminum fluoride, Sodium Fluoride product.
Described washing adopts distilled water to wash.
In described Sodium Silicofluoride, Sodium Silicofluoride content (butt meter) is 98.6%, and free acid content is 0.2%.
Embodiment 3
Fluorine-containing white residue prepares a method for Sodium Silicofluoride, and it comprises the following steps:
(1) be that 6% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to be, under 21kw is the condition of 83 DEG C to material temperature, carry out microwave reaction 18min;
(2) product of microwave reaction being cooled to temperature is after 39 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after dry 2.5h under 5 washings, temperature are 58 DEG C of conditions, obtains Sodium Silicofluoride.
Described fluorine-containing white residue is the fluoro-gas that Rock Phosphate (72Min BPL) decomposes and produces in Phosphoric Acid Concentration process, through absorbing process, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:1, and the mix and blend time is 7min.
Described solid-liquid separation adopts centrifugation.
The described centrifugation time is 18min, and rotating speed is 8000r/min.
In described step (2), liquid is sodium aluminum fluoride, Sodium Fluoride product.
Described washing adopts deionized water to wash.
In described Sodium Silicofluoride, Sodium Silicofluoride content (butt meter) is 99.6%, and free acid content is 0.17%.
Embodiment 4
Fluorine-containing white residue prepares a method for Sodium Silicofluoride, and it comprises the following steps:
(1) be that 23% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to be, under 20kw is the condition of 96 DEG C to material temperature, carry out microwave reaction 17min;
(2) product of microwave reaction being cooled to temperature is after 46 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after dry 4.8h under 3 washings, temperature are 76 DEG C of conditions, obtains Sodium Silicofluoride.
Described fluorine-containing white residue is the fluoro-gas produced in Rock Phosphate (72Min BPL) decomposition course, through absorbing process, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:1, and the mix and blend time is 62min.
Described solid-liquid separation adopts centrifugation.
The described centrifugation time is 17min, and rotating speed is 9600r/min.
In described step (2), liquid is sodium aluminum fluoride, Sodium Fluoride product.
Described washing adopts distilled water to wash.
In described Sodium Silicofluoride, Sodium Silicofluoride content (butt meter) is 97.9%, and free acid content is 0.11%.
Embodiment 5
Fluorine-containing white residue prepares a method for Sodium Silicofluoride, and it comprises the following steps:
(1) be that 22% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to be, under 13kw is the condition of 75 DEG C to material temperature, carry out microwave reaction 8min;
(2) product of microwave reaction being cooled to temperature is after 36 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after dry 5h under 5 washings, temperature are 116 DEG C of conditions, obtains Sodium Silicofluoride.
Described fluorine-containing white residue is the fluoro-gas produced in Rock Phosphate (72Min BPL) decomposition, Phosphoric Acid Concentration, potassium bearing rock process, hydrogen fluoride production process, through absorbing process, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:7, and the mix and blend time is 43min.
Described solid-liquid separation adopts centrifugation.
The described centrifugation time is 29min, and rotating speed is 6900r/min.
In described step (2), liquid is sodium aluminum fluoride, Sodium Fluoride product.
Described washing adopts deionized water to wash.
In described Sodium Silicofluoride, Sodium Silicofluoride content (butt meter) is 98.2%, and free acid content is 0.15%.
Embodiment 6
Fluorine-containing white residue prepares a method for Sodium Silicofluoride, and it comprises the following steps:
(1) be that 10% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to be, under 16kw is the condition of 86 DEG C to material temperature, carry out microwave reaction 17min;
(2) product of microwave reaction being cooled to temperature is after 40 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after dry 3h under 8 washings, temperature are 52 DEG C of conditions, obtains Sodium Silicofluoride.
Described fluorine-containing white residue is the fluoro-gas produced in Rock Phosphate (72Min BPL) decomposition, potassium bearing rock process, hydrogen fluoride production process, through absorbing process, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:8, and the mix and blend time is 35min.
Described solid-liquid separation adopts centrifugation.
The described centrifugation time is 30min, and rotating speed is 10000r/min.
In described step (2), liquid is sodium aluminum fluoride, Sodium Fluoride product.
Described washing adopts deionized water to wash.
In described Sodium Silicofluoride, Sodium Silicofluoride content (butt meter) is 99%, and free acid content is 0.13%.
Claims (9)
1. fluorine-containing white residue prepares a method for Sodium Silicofluoride, and it comprises the following steps:
(1) be that 5%-30% sodium hydroxide carries out mix and blend by fluorine-containing white residue and concentration, be placed in microwave reaction kettle, regulate microwave power to material temperature to be 70-120 DEG C, carry out microwave reaction 3-60min;
(2) product of microwave reaction being cooled to temperature is after 30-55 DEG C, through solid-liquid separation, obtains solid and liquid, by solid after 1-8 washing, drying step, obtains Sodium Silicofluoride.
2. fluorine-containing white residue according to claim 1 prepares the method for Sodium Silicofluoride, it is characterized in that, described fluorine-containing white residue is absorb fluoro-gas in Rock Phosphate (72Min BPL) decomposition, Phosphoric Acid Concentration, potassium bearing rock process, hydrogen fluoride production process to obtain acid solid.
3. fluorine-containing white residue according to claim 1 prepares the method for Sodium Silicofluoride, it is characterized in that, described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1:1-8, and the mix and blend time is 5-70min.
4. fluorine-containing white residue according to claim 1 prepares the method for Sodium Silicofluoride, it is characterized in that, described microwave power is 1-25kw, and the microwave reaction time is 5-20min.
5. fluorine-containing white residue according to claim 1 prepares the method for Sodium Silicofluoride, it is characterized in that, described solid-liquid separation adopts centrifugation.
6. fluorine-containing white residue according to claim 5 prepares the method for Sodium Silicofluoride, it is characterized in that, the described centrifugation time is 10-30min, and rotating speed is 5000-10000r/min.
7. the fluorine-containing white residue according to claim 5 or 6 prepares the method for Sodium Silicofluoride, it is characterized in that, the described centrifugation time is 18min, and rotating speed is 8000r/min.
8. fluorine-containing white residue according to claim 1 prepares the method for Sodium Silicofluoride, it is characterized in that, described washing adopts deionized water or distilled water to wash.
9. fluorine-containing white residue according to claim 1 prepares the method for Sodium Silicofluoride, it is characterized in that, described time of drying is 1-5h, and drying temperature is 50-130 DEG C.
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Cited By (5)
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| CN105858676A (en) * | 2016-04-11 | 2016-08-17 | 福建瓮福蓝天氟化工有限公司 | Production method for coproducing sodium silicate and sodium fluoride |
| CN105883836A (en) * | 2016-04-11 | 2016-08-24 | 福建瓮福蓝天氟化工有限公司 | Co-production method of sodium metasilicate and sodium fluoride |
| CN113856654A (en) * | 2021-11-20 | 2021-12-31 | 福州大学 | Method for preparing dye adsorbent by using slag |
| CN115818669A (en) * | 2022-11-22 | 2023-03-21 | 大连鼎燕医药化工有限公司 | Recycling method of aromatic hydrogen fluoride diazonium salt pyrolysis fluoro reaction waste |
| CN115869950A (en) * | 2022-12-21 | 2023-03-31 | 贵州大学 | Method for preparing Fenton-like catalyst and byproduct villiaumite product from fluorine-containing silicon slag |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858676A (en) * | 2016-04-11 | 2016-08-17 | 福建瓮福蓝天氟化工有限公司 | Production method for coproducing sodium silicate and sodium fluoride |
| CN105883836A (en) * | 2016-04-11 | 2016-08-24 | 福建瓮福蓝天氟化工有限公司 | Co-production method of sodium metasilicate and sodium fluoride |
| CN113856654A (en) * | 2021-11-20 | 2021-12-31 | 福州大学 | Method for preparing dye adsorbent by using slag |
| CN115818669A (en) * | 2022-11-22 | 2023-03-21 | 大连鼎燕医药化工有限公司 | Recycling method of aromatic hydrogen fluoride diazonium salt pyrolysis fluoro reaction waste |
| CN115869950A (en) * | 2022-12-21 | 2023-03-31 | 贵州大学 | Method for preparing Fenton-like catalyst and byproduct villiaumite product from fluorine-containing silicon slag |
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Address after: 554200 Transforming Industrial Park in Wanshan District, Tongren City, Guizhou Province Patentee after: Guizhou Kaisheng Potassium Technology Co., Ltd. Address before: 554200 Transforming Industrial Park in Wanshan District, Tongren District, Guizhou Province Patentee before: GUIZHOU YUANSHENG POTASSIUM TECHNOLOGY CO., LTD. |