CN106145172A - A kind of water purification agent and preparation method thereof - Google Patents
A kind of water purification agent and preparation method thereof Download PDFInfo
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- CN106145172A CN106145172A CN201610497458.1A CN201610497458A CN106145172A CN 106145172 A CN106145172 A CN 106145172A CN 201610497458 A CN201610497458 A CN 201610497458A CN 106145172 A CN106145172 A CN 106145172A
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- water
- water purification
- purification agent
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
- C01F7/765—Ammonium aluminium sulfates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
Disclosed herein is a kind of water purification agent and preparation method thereof, belong to water purification agent preparing technical field, fall within solid waste process and utilize field.Raw material used in the present invention is particle diameter < the microspheroidal catalytic cracking spent catalyst of 200 μm, mainly comprising as silicon oxide and aluminium oxide of this dead catalyst.Concrete operations include: (1) < the microspheroidal catalytic cracking spent catalyst of 200 μm is pulled an oar together with water, and stirring (2) is 20%～65% according to course of reaction acid concentration, and the ratio of solid-to-liquid ratio 1:2 6 adds sulphuric acid by particle diameter；(3) regulating reaction temperature after acid adding is 90 150 DEG C, reacts 1 6h at this temperature；(4) reaction is diluted with water to 2～3 times of original volume after terminating, and when temperature is not less than 90 DEG C, centrifugal filtration obtains filtrate；(5) in filtrate, it is passed through ammonia or adds ammonium sulfate, being cooled to 0～60 DEG C, filtering, washing, obtain water purifying granular agent Burnt ammonium alum crude product after drying；(6) technical grade Burnt ammonium alum is obtained after recrystallization.The present invention utilizes catalytic cracking spent catalyst produced by each refinery to prepare water purification agent for raw material production, has both obtained new product, solves again a process difficult problem for solid waste, economy environmental protection again.
Description
Technical field
The present invention relates to a kind of water purification agent and preparation method thereof, belong to water purification agent technical field, fall within solid waste
Process utilizes field.
Background technology
Water purification agent is a kind of medicament can put into and react with other impurity in water in water, because it is of a great variety,
Preparation method also differs the biggest.
In recent years, along with the increase of industrial waste generation amount, Many researchers utilizes the industrial waste containing aluminum to prepare respectively
Plant the product of relevant aluminum, these products have a lot all about water purification agent.
Chinese patent CN104803438A discloses and a kind of utilizes coal ash for manufacturing to obtain for the method for water purification agent, the method
Harmful substance in polluted-water can be carried out adsorbing, flocculate, precipitate and separating by water purification agent effectively, it is achieved purifying water effect.
Chinese patent CN102887578A discloses a kind of method utilizing dead catalyst production waste flocculant, the method
Selecting the high magnetic catalyst after Magneto separate is that polyaluminium chloride flocculant prepared by raw material, and the process both having solved dead catalyst is difficult
Topic, achieves again the production of flocculant.
Chinese patent CN102560129A discloses a kind of method preparing high purity aluminium oxide from useless aluminium-based catalyst, should
Method is Roasting And Leaching dealuminzation from the useless aluminium-based catalyst containing noble metal, first obtains Burnt ammonium alum, and after recrystallization, calcining obtains height
Pure alumina.
Though there being many reports to reclaim the aluminum method for water purification agent from waste material, but there are no report to be mainly composed of
Aluminium oxide and silicon oxide, < the microspheroidal catalytic cracking spent catalyst of 200 μm is the method that raw material preparation synthesizes water purification agent to particle diameter.
The granule of this particle diameter suspends contaminated air in atmosphere, increases haze and produces probability, therefore, be badly in need of working out a kind of simple easily
This particle diameter that solves of row is that < process of the microspheroidal catalytic cracking spent catalyst of 200 μm utilizes.
Summary of the invention
For the problems referred to above, the technical problem to be solved in the present invention is to provide a kind of by particle diameter < the microspheroidal catalysis of 200 μm
Cracking dead catalyst prepares the method for water purification agent.
The invention mainly comprises following step:
(1) by particle diameter, < the microspheroidal catalytic cracking spent catalyst of 200 μm is pulled an oar together with water, stirs 30min；
(2) being 20%～65% according to course of reaction acid concentration, the ratio of solid-to-liquid ratio 1:2-6 adds sulphuric acid；
(3) regulate reaction temperature after acid adding and be 90-150 DEG C, react 1-6h at this temperature；
(4) reaction is diluted with water to 2～3 times of original volume after terminating, and when temperature is not less than 90 DEG C, centrifugal filtration obtains
Filtrate；
(5) in filtrate, it is passed through ammonia or adds ammonium sulfate, being cooled to 0～60 DEG C, filtering, washing, obtain after drying
Granular purifying agent Burnt ammonium alum crude product；
(6) technical grade Burnt ammonium alum is obtained after Burnt ammonium alum crude product being carried out recrystallization.
The advantage of the present invention is: < the microspheroidal catalytic cracking spent catalyst of 200 μm prepares water purification agent, by stone to utilize particle diameter
The granular solids garbage that oiling factory produces carries out processing utilization, has obtained the water purification agent that can be used for purifying sewage, has solved
The fixed-end forces problem of puzzlement petroleum chemical enterprise, it is to avoid its graininess solid waste is to soil and the pollution of air.
Accompanying drawing explanation
Fig. 1 is the mass analysis data of gained water purification agent product in each embodiment；
Fig. 2 is the water purification experiment effect data of gained water purification agent product in each embodiment.
Detailed description of the invention
Embodiment 1
The preparation flow of water purification agent is as follows:
(1) < it is pulled an oar together with water by the microspheroidal catalytic cracking spent catalyst of 200 μm, stirs to weigh 100g particle diameter
Mix 30min；
(2) being 20% according to acid concentration in course of reaction, solid-to-liquid ratio is that the ratio of 1:6 adds sulphuric acid, for safety may be used
Control acid adding speed；
(3) regulating reaction temperature after acid adding is 140 DEG C, reacts 4h at this temperature；
(4) reaction is diluted with water to 2 times of original volume after terminating, and centrifugal filtration while hot obtains filtrate；
(5) in filtrate, it is passed through ammonia, is cooled to 10 DEG C, filter, washing, obtain water purifying granular agent aluminum sulfate after drying
Ammonium crude product；
(6) technical grade water purification agent Burnt ammonium alum is obtained after Burnt ammonium alum crude product being carried out recrystallization.
In the present embodiment, the mass analysis data of water purification agent is shown in Fig. 1, the water purification effect of gained water purification agent sample in the present embodiment
Fruit sees Fig. 2.
Embodiment 2
The preparation flow of water purification agent is as follows:
(1) < it is pulled an oar together with water by the microspheroidal catalytic cracking spent catalyst of 40 μm, stirring to weigh 100g particle diameter
30min；
(2) being 30% according to acid concentration in course of reaction, solid-to-liquid ratio is that the ratio of 1:5 adds sulphuric acid, for the sake of peace safety
Acid adding speed can be controlled；
(3) regulating reaction temperature after acid adding is 130 DEG C, reacts 4h at this temperature；
(4) reaction is diluted with water to 2 times of original volume after terminating, and centrifugal filtration while hot obtains filtrate；
(5) in filtrate, it is passed through ammonia, is cooled to 50 DEG C, filter, washing, obtain water purifying granular agent aluminum sulfate after drying
Ammonium crude product；
(6) technical grade water purification agent Burnt ammonium alum is obtained after Burnt ammonium alum crude product being carried out recrystallization.
In the present embodiment, the mass analysis data of water purification agent is shown in Fig. 1, the water purification effect of gained water purification agent sample in the present embodiment
Fruit sees Fig. 2.
Embodiment 3
The preparation flow of water purification agent is as follows:
(1) < it is pulled an oar together with water by the microspheroidal catalytic cracking spent catalyst of 20 μm, stirring to weigh 100g particle diameter
30min；
(2) being 40% according to acid concentration in course of reaction, solid-to-liquid ratio is that the ratio of 1:4 adds sulphuric acid, for the sake of peace safety
Acid adding speed can be controlled；
(3) regulating reaction temperature after acid adding is 140 DEG C, reacts 4h at this temperature；
(4) reaction is diluted with water to 2 times of original volume after terminating, and centrifugal filtration while hot obtains filtrate；
(5) in filtrate, it is passed through ammonia, is cooled to 20 DEG C, filter, washing, obtain water purifying granular agent aluminum sulfate after drying
Ammonium crude product；
(6) technical grade water purification agent Burnt ammonium alum is obtained after Burnt ammonium alum crude product being carried out recrystallization.
In the present embodiment, the mass analysis data of water purification agent is shown in Fig. 1, the water purification effect of gained water purification agent sample in the present embodiment
Fruit sees Fig. 2.
Embodiment 4
The preparation flow of water purification agent is as follows:
(1) < it is pulled an oar together with water by the microspheroidal catalytic cracking spent catalyst of 150 μm, stirs to weigh 100g particle diameter
Mix 30min；
(2) being 50% according to acid concentration in course of reaction, solid-to-liquid ratio is that the ratio of 1:3 adds sulphuric acid, for the sake of peace safety
Acid adding speed can be controlled；
(3) regulating reaction temperature after acid adding is 130 DEG C, reacts 3h at this temperature；
(4) reaction is diluted with water to 3 times of original volume after terminating, and centrifugal filtration while hot obtains filtrate；
(5) in filtrate, it is passed through ammonia, is cooled to 10 DEG C, filter, washing, obtain water purifying granular agent aluminum sulfate after drying
Ammonium crude product；
(6) technical grade water purification agent Burnt ammonium alum is obtained after Burnt ammonium alum crude product being carried out recrystallization.
In the present embodiment, the mass analysis data of water purification agent is shown in Fig. 1, the water purification effect of gained water purification agent sample in the present embodiment
Fruit sees Fig. 2.
Embodiment 5
The preparation flow of water purification agent is as follows:
(1) < it is pulled an oar together with water by the microspheroidal catalytic cracking spent catalyst of 200 μm, stirs to weigh 100g particle diameter
Mix 30min；
(2) being 60% according to acid concentration in course of reaction, solid-to-liquid ratio is that the ratio of 1:3 adds sulphuric acid, for the sake of peace safety
Acid adding speed can be controlled；
(3) regulating reaction temperature after acid adding is 140 DEG C, reacts 3h at this temperature；
(4) reaction is diluted with water to 3 times of original volume after terminating, and centrifugal filtration while hot obtains filtrate；
(5) in filtrate, it is passed through ammonia, is cooled to 30 DEG C, filter, washing, obtain water purifying granular agent aluminum sulfate after drying
Ammonium crude product；
(6) technical grade water purification agent Burnt ammonium alum is obtained after Burnt ammonium alum crude product being carried out recrystallization.
In the present embodiment, the mass analysis data of water purification agent is shown in Fig. 1, the water purification effect of gained water purification agent sample in the present embodiment
Fruit sees Fig. 2.
Claims (4)
1. water purification agent and preparation method thereof, it is characterised in that concrete operation step is:
(1) by particle diameter, < the microspheroidal catalytic cracking spent catalyst of 200 μm pulls an oar together with water, stir and obtain solidliquid mixture；
(2) sulphuric acid is joined in the solidliquid mixture in (1) carry out dissolve reaction；
(3) reaction is diluted with water to 2～3 times of original volume after terminating, and at a temperature of being not less than 90 DEG C, centrifugal filtration obtains filtrate；
(4) in filtrate, it is passed through ammonia or adds ammonium sulfate, carrying out after being cooled to 0～60 DEG C filtering, washing, the filter cake that will obtain
Obtain water purifying granular agent Burnt ammonium alum crude product after drying；
(5) technical grade Burnt ammonium alum is obtained after Burnt ammonium alum crude product being carried out recrystallization.
2., according to described in claim 1, the solid-to-liquid ratio of the solidliquid mixture described in step (1) is 1:2～6.
3., according to described in claim 1, preferably in step (2), cool the filtrate to 0～30 DEG C.
4., according to described in claim 1, the recrystallization condition described in step (5) is: Burnt ammonium alum: water=1:1；Dissolve
Temperature is 102 DEG C, and recrystallization temperature is 0～10 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610497458.1A CN106145172A (en) | 2016-06-29 | 2016-06-29 | A kind of water purification agent and preparation method thereof |
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| CN201610497458.1A CN106145172A (en) | 2016-06-29 | 2016-06-29 | A kind of water purification agent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055583A (en) * | 2017-05-02 | 2017-08-18 | 常熟理工学院 | The method that ammonia-alum is prepared by raw material of dead catalyst |
| CN108328638A (en) * | 2018-03-26 | 2018-07-27 | 武汉理工大学 | A method of preparing alum from FCC dead catalyst |
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| CN1673094A (en) * | 2005-02-01 | 2005-09-28 | 山东师范大学 | Synthesis process of nano zinc oxide material |
| CN1887720A (en) * | 2006-07-26 | 2007-01-03 | 中国科学院上海硅酸盐研究所 | Prepn process of nanometer Zinc oxide powder |
| CN102531037A (en) * | 2012-01-16 | 2012-07-04 | 沭阳县飞宏金属新材料有限公司 | Chemical preparation method of nanoscale zinc oxide powder |
| CN104445362A (en) * | 2014-11-03 | 2015-03-25 | 苏州市泽镁新材料科技有限公司 | Preparation method of nano zinc carbonate |
| CN105236467A (en) * | 2014-08-01 | 2016-01-13 | 阜阳师范学院 | Mass preparation process of nano-grade zinc oxide, and application of nano-grade zinc oxide |
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2016
- 2016-06-29 CN CN201610497458.1A patent/CN106145172A/en active Pending
Patent Citations (5)
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| CN1673094A (en) * | 2005-02-01 | 2005-09-28 | 山东师范大学 | Synthesis process of nano zinc oxide material |
| CN1887720A (en) * | 2006-07-26 | 2007-01-03 | 中国科学院上海硅酸盐研究所 | Prepn process of nanometer Zinc oxide powder |
| CN102531037A (en) * | 2012-01-16 | 2012-07-04 | 沭阳县飞宏金属新材料有限公司 | Chemical preparation method of nanoscale zinc oxide powder |
| CN105236467A (en) * | 2014-08-01 | 2016-01-13 | 阜阳师范学院 | Mass preparation process of nano-grade zinc oxide, and application of nano-grade zinc oxide |
| CN104445362A (en) * | 2014-11-03 | 2015-03-25 | 苏州市泽镁新材料科技有限公司 | Preparation method of nano zinc carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055583A (en) * | 2017-05-02 | 2017-08-18 | 常熟理工学院 | The method that ammonia-alum is prepared by raw material of dead catalyst |
| CN108328638A (en) * | 2018-03-26 | 2018-07-27 | 武汉理工大学 | A method of preparing alum from FCC dead catalyst |
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