CN105000563B - A kind of method that fluorine-containing white residue prepares prodan - Google Patents
A kind of method that fluorine-containing white residue prepares prodan Download PDFInfo
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- CN105000563B CN105000563B CN201510400070.0A CN201510400070A CN105000563B CN 105000563 B CN105000563 B CN 105000563B CN 201510400070 A CN201510400070 A CN 201510400070A CN 105000563 B CN105000563 B CN 105000563B
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Abstract
The present invention relates to industrial residue comprehensive utilization technique, the method that specifically related to a kind of fluorine-containing white residue prepares prodan, by fluorine-containing white residue, after concentration is sufficiently mixed for 5% 30% sodium hydroxides, it is 70 120 DEG C to adjust microwave power to material temperature, carry out after the 60min of microwave reaction 3, temperature to be cooled is 30 55 DEG C, through separation of solid and liquid, after drying process, obtain solid prodan, present invention process utilizes discarded fluorine-containing white residue combination microwave technology, one step generates prodan, production cost is low, technique is simple, eliminate the harm that acid white residue is produced to environment, low-carbon environment-friendly, it is truly realized fluorine-containing white residue environmentally friendly, it is efficient to develop effect.
Description
Technical field
The present invention relates to a kind of method that fluorine-containing white residue prepares prodan, belong to chemical production technical field.
Background technology
A large amount of tetrafluorides can be produced during rock phosphate in powder decomposition, Phosphoric Acid Concentration, potassium bearing rock processing, hydrogen fluoride production
The fluoro-gas such as silicon, hydrogen fluoride, enterprise of big department absorbs the fluorine-containing white residue of generation using water at present, but the method produces a large amount of white residue heaps
Product, in turn results in serious environmental issue, so, the recycling of fluoro-gas turns into urgent problem to be solved.
Prodan has good application market, and it is applied to building materials field, can be used as hygroscopic agent, retarder, anti-corrosion
Agent etc.；Applied to latex product field, opalizer, fluxing agent etc. can be used as；Applied to agriculture field, can as insecticide, because
This, prodan has good work, agriculture application value.
At present, in the existing production technology of prodan, auxiliary reagent is more, produces a large amount of industrial wastewaters, and processing step is multiple
Miscellaneous, preparation condition is harsh.As Patent No. discloses albite through handling, decompose and to obtain fluoro-gas, then through hydrolysis, acidleach, obtain
Pickle liquor, it is crystallized with sodium sulphate hybrid reaction, separated using gravity settling technology, drying process, acquisition fluosilicic acid
Sodium product, this method cost is low, pollutes small, but product quality is poor, performance is low.
In order to solve the above technical problems, this technique, which is the recycling of fluoro-gas and the production of prodan, provides one kind
New approaches.
The content of the invention
To solve the problem of complex utilization of prior art problem and related industries waste residue, this technique uses microwave reaction work
Skill, step generation prodan.
Its technical scheme, comprises the following steps：
(1) it is that 5%-30% sodium hydroxides are mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts
It is under conditions of 70-120 DEG C, to carry out microwave reaction 3-60min to save microwave power to material temperature；
(2) product of microwave reaction is cooled to temperature after 30-55 DEG C, through separation of solid and liquid, to obtain solid and liquid, will
Solid obtains prodan after 1-8 washing, drying steps.
Described fluorine-containing white residue is generation during rock phosphate in powder decomposition, Phosphoric Acid Concentration, potassium bearing rock processing, hydrogen fluoride production
Fluoro-gas, handled through absorption, obtain acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：1-8, the mixing time is 5-70min.
Described microwave power is 1-25kw, and the microwave reaction time is 5-20min.
Described separation of solid and liquid is using centrifugation.
The described centrifugation time is 10-30min, and rotating speed is 5000-10000r/min；It is preferred that the time of centrifugation is
18min, rotating speed is 8000r/min.
Liquid is ice crystal, sodium fluoride product in described step (2).
Described washing is washed using deionized water or distilled water.
Described drying time is 1-5h, and drying temperature is 50-130 DEG C.
Beneficial effects of the present invention
The present invention utilizes microwave technology, and the fluorine-containing white residue generation prodan of step processing substantially reduces the reaction time, dropped
Low effective control of energy resource consumption, wherein microwave power, microwave time and material temperature, has promoted storeroom reaction, with reference to biography
Detection mode of uniting detects the result of prodan content, and the prodan content of this product is up to more than 99%, far above tradition side
Prodan prepared by method, in summary, prodan prepared by the present invention have the excellent benefit of quality, and because of present invention utilization
The fluorine-containing white residue of trade waste prepares prodan, reduces cost of material, the fluorine resource in discarded object is effectively returned
Receive and utilize, so being utilized with obtaining efficient low energy the invention enables fluorine-containing white residue.
The present invention strictly controls fluorine-containing white residue by appropriately being adjusted to technical parameter in processing step and related process
Mass volume ratio with sodium hydroxide is 1：1-8 so that the reaction of fluorine-containing white residue and sodium hydroxide is more abundant, is enhanced between particle
Interaction force, and then Improving The Quality of Products；The present invention is conducive to abundant between material after carrying out separation of solid and liquid after product cooling
Reaction；The present invention is washed using deionized water, is effectively removed product surface ionic impurity, is washed using distilled water,
Free acid content can be reduced, with reference to the quality measurements of prodan, this product prodan content is far above traditional preparation method,
Free acid content about 0.15% or so, reaches prodan one-level quality, and dry technology state modulator plays stable product structure
Effect, so, this product has good quality assurance.
Brief description of the drawings
Fig. 1 is the process chart that fluorine-containing white residue of the invention prepares prodan.
Embodiment
Limited with reference to specific embodiment technical scheme is further, but claimed
Scope is not only limited to made description.
Embodiment 1
A kind of method that fluorine-containing white residue prepares prodan, it comprises the following steps：
(1) it is that 28% sodium hydroxide is mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts micro-
It is under conditions of 71 DEG C, to carry out microwave reaction 6min that wave power, which is 16kw to material temperature,；
(2) product of microwave reaction is cooled to temperature after 48 DEG C, through separation of solid and liquid, to obtain solid and liquid, will be solid
Body through 7 times washing, temperature be 70 DEG C under the conditions of dry 3h after, obtain prodan.
Described fluorine-containing white residue is the fluoro-gas produced in potassium bearing rock processing procedure, is handled through absorption, obtains acidity
Solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：6, the mixing time is 7min.
Described separation of solid and liquid is using centrifugation.
The described centrifugation time is 13min, and rotating speed is 5500r/min.
Liquid is ice crystal, sodium fluoride product in described step (2).
Described washing is washed using distilled water water.
Prodan content (butt meter) is 99.3% in described prodan, and free acid content is 0.13%.
Embodiment 2
A kind of method that fluorine-containing white residue prepares prodan, it comprises the following steps：
(1) it is that 17% sodium hydroxide is mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts micro-
It is under conditions of 118 DEG C, to carry out microwave reaction 10min that wave power, which is 3kw to material temperature,；
(2) product of microwave reaction is cooled to temperature after 32 DEG C, through separation of solid and liquid, to obtain solid and liquid, will be solid
Body through 3 times washing, temperature be 100 DEG C under the conditions of dry 1h after, obtain prodan.
Described fluorine-containing white residue is the fluoro-gas produced during hydrogen fluoride production, is handled through absorption, obtains acid solid
Body.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：6, the mixing time is 55min.
Described separation of solid and liquid is using centrifugation.
The described centrifugation time is 23min, and rotating speed is 7000r/min.
Liquid is ice crystal, sodium fluoride product in described step (2).
Described washing is washed using distilled water.
Prodan content (butt meter) is 98.6% in described prodan, and free acid content is 0.2%.
Embodiment 3
A kind of method that fluorine-containing white residue prepares prodan, it comprises the following steps：
(1) it is that 6% sodium hydroxide is mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts micro-
It is under conditions of 83 DEG C, to carry out microwave reaction 18min that wave power, which is 21kw to material temperature,；
(2) product of microwave reaction is cooled to temperature after 39 DEG C, through separation of solid and liquid, to obtain solid and liquid, will be solid
Body through 5 times washing, temperature be 58 DEG C under the conditions of dry 2.5h after, obtain prodan.
Described fluorine-containing white residue is the fluoro-gas that rock phosphate in powder is decomposed and produced during Phosphoric Acid Concentration, is handled through absorption,
Obtain acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：1, the mixing time is 7min.
Described separation of solid and liquid is using centrifugation.
The described centrifugation time is 18min, and rotating speed is 8000r/min.
Liquid is ice crystal, sodium fluoride product in described step (2).
Described washing is washed using deionized water.
Prodan content (butt meter) is 99.6% in described prodan, and free acid content is 0.17%.
Embodiment 4
A kind of method that fluorine-containing white residue prepares prodan, it comprises the following steps：
(1) it is that 23% sodium hydroxide is mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts micro-
It is under conditions of 96 DEG C, to carry out microwave reaction 17min that wave power, which is 20kw to material temperature,；
(2) product of microwave reaction is cooled to temperature after 46 DEG C, through separation of solid and liquid, to obtain solid and liquid, will be solid
Body through 3 times washing, temperature be 76 DEG C under the conditions of dry 4.8h after, obtain prodan.
Described fluorine-containing white residue is the fluoro-gas produced in rock phosphate in powder decomposable process, is handled through absorption, obtains acid solid
Body.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：1, the mixing time is 62min.
Described separation of solid and liquid is using centrifugation.
The described centrifugation time is 17min, and rotating speed is 9600r/min.
Liquid is ice crystal, sodium fluoride product in described step (2).
Described washing is washed using distilled water.
Prodan content (butt meter) is 97.9% in described prodan, and free acid content is 0.11%.
Embodiment 5
A kind of method that fluorine-containing white residue prepares prodan, it comprises the following steps：
(1) it is that 22% sodium hydroxide is mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts micro-
It is under conditions of 75 DEG C, to carry out microwave reaction 8min that wave power, which is 13kw to material temperature,；
(2) product of microwave reaction is cooled to temperature after 36 DEG C, through separation of solid and liquid, to obtain solid and liquid, will be solid
Body through 5 times washing, temperature be 116 DEG C under the conditions of dry 5h after, obtain prodan.
Described fluorine-containing white residue is generation during rock phosphate in powder decomposition, Phosphoric Acid Concentration, potassium bearing rock processing, hydrogen fluoride production
Fluoro-gas, handled through absorption, obtain acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：7, the mixing time is 43min.
Described separation of solid and liquid is using centrifugation.
The described centrifugation time is 29min, and rotating speed is 6900r/min.
Liquid is ice crystal, sodium fluoride product in described step (2).
Described washing is washed using deionized water.
Prodan content (butt meter) is 98.2% in described prodan, and free acid content is 0.15%.
Embodiment 6
A kind of method that fluorine-containing white residue prepares prodan, it comprises the following steps：
(1) it is that 10% sodium hydroxide is mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts micro-
It is under conditions of 86 DEG C, to carry out microwave reaction 17min that wave power, which is 16kw to material temperature,；
(2) product of microwave reaction is cooled to temperature after 40 DEG C, through separation of solid and liquid, to obtain solid and liquid, will be solid
Body through 8 times washing, temperature be 52 DEG C under the conditions of dry 3h after, obtain prodan.
Described fluorine-containing white residue be rock phosphate in powder decompose, potassium bearing rock processing, produce during hydrogen fluoride production contain fluorine gas
Body, is handled through absorption, obtains acid solid.
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：8, the mixing time is 35min.
Described separation of solid and liquid is using centrifugation.
The described centrifugation time is 30min, and rotating speed is 10000r/min.
Liquid is ice crystal, sodium fluoride product in described step (2).
Described washing is washed using deionized water.
Prodan content (butt meter) is 99% in described prodan, and free acid content is 0.13%.
Claims (7)
1. a kind of method that fluorine-containing white residue prepares prodan, it comprises the following steps：
(1) it is that 5%-30% sodium hydroxides are mixed by fluorine-containing white residue and concentration, is placed in microwave reaction kettle, adjusts micro-
Wave power to material temperature is 70-120 DEG C, carries out microwave reaction 3-60min；
(2) product of microwave reaction is cooled to temperature after 30-55 DEG C, through separation of solid and liquid, solid and liquid to be obtained, by solid
After 1-8 washing, drying steps, prodan is obtained；
Described microwave power is 1-25kw, and the microwave reaction time is 5-20min；
Described fluorine-containing white residue and the mass volume ratio of sodium hydroxide are 1：1-8, the mixing time is 5-70min.
2. the method that fluorine-containing white residue according to claim 1 prepares prodan, it is characterised in that described fluorine-containing white residue
Obtain acid solid to absorb fluoro-gas during rock phosphate in powder decomposition, Phosphoric Acid Concentration, potassium bearing rock processing, hydrogen fluoride production
Body.
3. the method that fluorine-containing white residue according to claim 1 prepares prodan, it is characterised in that described separation of solid and liquid
Using centrifugation.
4. the method that fluorine-containing white residue according to claim 3 prepares prodan, it is characterised in that described centrifugation
Time is 10-30min, and rotating speed is 5000-10000r/min.
5. the method that the fluorine-containing white residue according to claim 3 or 4 prepares prodan, it is characterised in that described centrifugation
Disengaging time is 18min, and rotating speed is 8000r/min.
6. the method that fluorine-containing white residue according to claim 1 prepares prodan, it is characterised in that described washing is to adopt
Washed with deionized water or distilled water.
7. the method that fluorine-containing white residue according to claim 1 prepares prodan, it is characterised in that described drying time
For 1-5h, drying temperature is 50-130 DEG C.
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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 |
| CN115869950B (en) * | 2022-12-21 | 2023-07-18 | 贵州大学 | Method for preparing Fenton-like catalyst from fluorine-containing silicon slag and preparing byproduct fluoride salt product |
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| 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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| 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 |
| CN104445210A (en) * | 2014-11-28 | 2015-03-25 | 嵩县中科孵化器有限公司 | Preparation method of sodium fluosilicate |
| CN104591189A (en) * | 2015-02-10 | 2015-05-06 | 湖南有色氟化学科技发展有限公司 | Recycling method for purifying cryolite waste acid |
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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. |