CN106277009A - A kind of preparation method of aluminum sulfate - Google Patents
A kind of preparation method of aluminum sulfate Download PDFInfo
- Publication number
- CN106277009A CN106277009A CN201610601624.8A CN201610601624A CN106277009A CN 106277009 A CN106277009 A CN 106277009A CN 201610601624 A CN201610601624 A CN 201610601624A CN 106277009 A CN106277009 A CN 106277009A
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- China
- Prior art keywords
- aluminum sulfate
- solid
- preparation
- solidliquid mixture
- catalytic cracking
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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
- C01F7/741—Preparation from elemental aluminium or elemental aluminium containing materials, e.g. foil or dross
Abstract
The invention provides the preparation method of a kind of aluminum sulfate, < the microspheroidal catalytic cracking spent catalyst of 200 μm is as raw material with particle diameter for the method, after carrying out sour molten reaction with sulphuric acid under certain condition, obtain solidliquid mixture, it is centrifuged after carrying out solid-liquid separation, obtain the aluminum sulfate solution containing foreign ion, add a certain proportion of Sodium Dimethyldithiocarbamate in the solution, remove Ni2+, V5+Obtain clean aluminum sulfate solution Deng foreign ion, after evaporative crystallization, obtain aluminum sulfate solid.The granular solids garbage that this invention uses petroleum chemical enterprise to produce carries out the preparation of aluminum sulfate, had both solved petroleum chemical enterprise's process difficult problem about solid waste, and had reclaimed again bauxite resource, economy environmental protection again.
Description
Technical field
The present invention relates to the preparation method of a kind of aluminum sulfate, belong to aluminum sulfate preparing technical field, fall within particulate matter solid
Body offal treatment utilizes field.
Background technology
Aluminum sulfate is a kind of conventional industrial chemical reagent, and its consumption is big, of many uses, may be used for every field, mesh
What front application was most is primarily used for papermaking and water process aspect.Because of the extensive application of aluminum sulfate, prepare various forms of at present
The method of aluminum sulfate has a lot, but traditional method preparing aluminum sulfate is still prepared by bauxite and sulphuric acid compressive reaction,
Raw material of preparing about aluminum sulfate also tended to variation in recent years, including alunite, Kaolin and the material of salic silicon
Deng raw material.Chinese patent CN105417661A discloses a kind of method having aluminum dross to prepare polyaluminium sulfate, and obtain is compound
Aluminum sulfate product flocculating effect is good, water purification ability is strong.Chinese patent CN104250019A discloses one and is produced sulfur by flyash
The technique of acid aluminum, and use ammonia process roasting, leaching, separation of iron in goethite form to obtain aluminum sulfate solution, the aluminum sulfate finally given is molten
In liquid, iron ion content is less than 20mg/L.Chinese patent CN101209850A discloses and a kind of utilizes Kaolin to prepare aluminum sulfate
Method, technique is simple, practical, and the aluminum sulfate solution obtained is limpid, impurity is few.
Catalytic cracking spent catalyst is a kind of dead catalyst that oil refining enterprise's year generation amount is most, and it is mainly composed of oxidation
Aluminum and silicon oxide, possibly together with a certain amount of rare earth and heavy metal element, it is impossible to uses compost, be pyrolyzed and the processing mode such as burning.
Along with the increasing of environmental protection dynamics, bury and have been subjected to strictly control even to prohibit the use of as processing mode currently mainly, because of
Environment, Polluted Soil can be entered along with the immersion Transport And Transformation of rainwater after burying for the heavy metal in catalytic cracking spent catalyst
Earth and river, final harmful to human.Additionally, the particle diameter of catalytic cracking spent catalyst is between 0～149 μm, there is stronger suction
Attached property, easy absorption is carried harmful substance and is suspended for a long time in atmosphere, increases the formation probability of haze, and harm human body is good for
Health.The most effectively process the microspheroidal catalytic cracking spent catalyst utilizing particle diameter to be 0～149 μm and there is great reality
Meaning and environment protection significance.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of aluminum sulfate, with particle diameter < the microspheroidal catalytic cracking of 200 μm
Dead catalyst is raw material, it is achieved the process of solid waste utilizes, and reduces the pollution to environment of the micro-spherical particle catalytic cracking spent catalyst.
For solving above-mentioned purpose, the invention provides a kind of method utilizing catalytic cracking spent catalyst to prepare aluminum sulfate,
Mainly comprise following technical step:
(1) by particle diameter, < the micro-spherical particle catalytic cracking spent catalyst of 200 μm and water carry out the 30min that pulls an oar, and are formed uniformly
Consistent solidliquid mixture；
(2) according to solid-to-liquid ratio 1:6 and reaction acid concentration 20～65%, sulphuric acid is joined in the solidliquid mixture in (1),
Controlling reaction temperature is 90～150 DEG C and response time 1～6h；
(3) use centrifugal mode to carry out solid-liquid separation material after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, obtain the most transparent aluminum sulfate solution after filtration, steam
Aluminum sulfate solid is obtained after sending out crystallization.
Detailed description of the invention
The preparation method of the Solid aluminum sulfate of the present invention is below described for specific embodiment.
Embodiment 1
The preparation method of a kind of aluminum sulfate, comprises the following steps:
(1) by 100g particle diameter, < the micro-spherical particle catalytic cracking spent catalyst of 200 μm and water carry out the 30min that pulls an oar, and are formed
The solidliquid mixture of uniformity；
(2) according to solid-to-liquid ratio 1:6 and reaction acid concentration 20%, sulphuric acid is joined in the solidliquid mixture in (1), control
Reaction temperature is 110 DEG C, response time 2h；
(3) use centrifugal mode to carry out solid-liquid separation material after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, obtain the most transparent aluminum sulfate solution after filtration, steam
Aluminum sulfate solid is obtained after sending out crystallization.
Embodiment 2
The preparation method of a kind of aluminum sulfate, comprises the following steps:
(1) by 100g particle diameter, < the micro-spherical particle catalytic cracking spent catalyst of 40 μm and water carry out the 30min that pulls an oar, and are formed
The solidliquid mixture of uniformity；
(2) according to solid-to-liquid ratio 1:4 and reaction acid concentration 30%, sulphuric acid is joined in the solidliquid mixture in (1), control
Reaction temperature is 120 DEG C, response time 3h；
(3) use centrifugal mode to carry out solid-liquid separation material after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, obtain the most transparent aluminum sulfate solution after filtration, steam
Aluminum sulfate solid is obtained after sending out crystallization.
Embodiment 3
The preparation method of a kind of aluminum sulfate, comprises the following steps:
(1) by 100g particle diameter, < the micro-spherical particle catalytic cracking spent catalyst of 150 μm and water carry out the 30min that pulls an oar, and are formed
The solidliquid mixture of uniformity；
(2) according to solid-to-liquid ratio 1:5 and reaction acid concentration 40%, sulphuric acid is joined in the solidliquid mixture in (1), control
Reaction temperature is 120 DEG C, response time 2h；
(3) use centrifugal mode to carry out solid-liquid separation material after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, obtain the most transparent aluminum sulfate solution after filtration, steam
Aluminum sulfate solid is obtained after sending out crystallization.
Embodiment 4
The preparation method of a kind of aluminum sulfate, comprises the following steps:
(1) by 100g particle diameter, < the micro-spherical particle catalytic cracking spent catalyst of 200 μm and water carry out the 30min that pulls an oar, and are formed
The solidliquid mixture of uniformity；
(2) according to solid-to-liquid ratio 1:3 and reaction acid concentration 50%, sulphuric acid is joined in the solidliquid mixture in (1), control
Reaction temperature is 140 DEG C, response time 1h；
(3) use centrifugal mode to carry out solid-liquid separation material after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, obtain the most transparent aluminum sulfate solution after filtration, steam
Aluminum sulfate solid is obtained after sending out crystallization.
Embodiment 5
The preparation method of a kind of aluminum sulfate, comprises the following steps:
(1) by 100g particle diameter, < the micro-spherical particle catalytic cracking spent catalyst of 200 μm and water carry out the 30min that pulls an oar, and are formed
The solidliquid mixture of uniformity；
(2) according to solid-to-liquid ratio 1:5 and reaction acid concentration 60%, sulphuric acid is joined in the solidliquid mixture in (1), control
Reaction temperature is 120 DEG C, response time 3h；
(3) use centrifugal mode to carry out solid-liquid separation material after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, obtain the most transparent aluminum sulfate solution after filtration, steam
Aluminum sulfate solid is obtained after sending out crystallization.
Embodiment 6
The preparation method of a kind of aluminum sulfate, comprises the following steps:
(1) by 100g particle diameter, < the micro-spherical particle catalytic cracking spent catalyst of 200 μm and water carry out the 30min that pulls an oar, and are formed
The solidliquid mixture of uniformity；
(2) according to solid-to-liquid ratio 1:3 and reaction acid concentration 50%, sulphuric acid is joined in the solidliquid mixture in (1), control
Reaction temperature is 120 DEG C, response time 3h；
(3) use centrifugal mode to carry out solid-liquid separation material after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, obtain the most transparent aluminum sulfate solution after filtration, steam
Aluminum sulfate solid is obtained after sending out crystallization.
According to the preparation method of the aluminum sulfate in above-described embodiment, Al in obtained Solid aluminum sulfate2O3>=15.8%,
PH ＞ 3.0, water-insoluble≤0.2%, Fe≤0.01%, meet National Industrial standard.Gained aluminum sulfate product in each embodiment
Mass analysis data as shown below:
| Analysis project | Al2O3/ % | pH | Water-insoluble/% | Fe/% |
| Embodiment 1 | 15.9 | 3.2 | 0.09 | 0.003 |
| Embodiment 2 | 16.3 | 3.1 | 0.08 | 0.004 |
| Embodiment 3 | 16.1 | 3.2 | 0.09 | 0.002 |
| Embodiment 4 | 15.9 | 3.1 | 0.1 | 0.004 |
| Embodiment 5 | 16.0 | 3.0 | 0.11 | 0.003 |
| Embodiment 6 | 15.8 | 3.1 | 0.09 | 0.005 |
Claims (3)
1. the preparation method of an aluminum sulfate, it is characterised in that: the raw material that the method is used is the particle diameter < microspheroidal of 200 μm
Catalytic cracking spent catalyst, the method mainly includes following step:
(1) catalytic cracking spent catalyst is pulled an oar with water, form the solidliquid mixture of uniformity；
(2) sulphuric acid is joined in the solidliquid mixture in (1) carry out dissolve reaction；
(3) use centrifugal mode to carry out solid-liquid separation whole products after reaction terminates, obtain the sulphuric acid containing foreign ion
The thick liquid of aluminum；
(4) the thick liquid of the aluminum sulfate in (3) adds Sodium Dimethyldithiocarbamate, after filtration, obtain the most transparent aluminum sulfate solution, evaporation knot
Aluminum sulfate solid is obtained after crystalline substance.
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, the condition dissolving reaction described in step (2) is: acid concentration 20～65%, instead
Answer temperature 90～150 DEG C, during reaction 1～6h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610601624.8A CN106277009A (en) | 2016-07-28 | 2016-07-28 | A kind of preparation method of aluminum sulfate |
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| CN201610601624.8A CN106277009A (en) | 2016-07-28 | 2016-07-28 | A kind of preparation method of aluminum sulfate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110386616A (en) * | 2019-08-14 | 2019-10-29 | 淄博汇成净水剂科技有限公司 | A method of processing FCC dead catalyst produces aluminum sulfate |
| CN115417438A (en) * | 2022-08-30 | 2022-12-02 | 青岛惠城环保科技集团股份有限公司 | Method for synthesizing hydrotalcite-like material by using waste catalyst as aluminum source |
Citations (5)
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|---|---|---|---|---|
| CN1657409A (en) * | 2005-02-21 | 2005-08-24 | 浙江大学 | Method for preparing high-purity ultrnfine silicone powder and aluminium sulphate using kadin as raw material |
| CN101746802A (en) * | 2010-01-24 | 2010-06-23 | 徐州浩通新材料科技股份有限公司 | Method for manufacturing aluminum sulfate |
| CN102101689A (en) * | 2010-12-23 | 2011-06-22 | 内蒙古昶泰资源循环再生利用科技开发有限责任公司 | Technological method for producing high-purity low-iron aluminum sulfate by using coal ash and comprehensively utilizing coal ash |
| CN102583479A (en) * | 2012-02-17 | 2012-07-18 | 昊青薪材（北京）技术有限公司 | Method for preparing industrial aluminum sulfate by using aluminum-silicon filter cakes left by extracting potassium from potassium feldspar |
| CN104773748A (en) * | 2015-03-10 | 2015-07-15 | 江苏永葆环保科技股份有限公司 | Method for preparing low-iron polyaluminium sulfate by using aluminiferous waste sulfuric acid mother liquor |
-
2016
- 2016-07-28 CN CN201610601624.8A patent/CN106277009A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657409A (en) * | 2005-02-21 | 2005-08-24 | 浙江大学 | Method for preparing high-purity ultrnfine silicone powder and aluminium sulphate using kadin as raw material |
| CN101746802A (en) * | 2010-01-24 | 2010-06-23 | 徐州浩通新材料科技股份有限公司 | Method for manufacturing aluminum sulfate |
| CN102101689A (en) * | 2010-12-23 | 2011-06-22 | 内蒙古昶泰资源循环再生利用科技开发有限责任公司 | Technological method for producing high-purity low-iron aluminum sulfate by using coal ash and comprehensively utilizing coal ash |
| CN102583479A (en) * | 2012-02-17 | 2012-07-18 | 昊青薪材（北京）技术有限公司 | Method for preparing industrial aluminum sulfate by using aluminum-silicon filter cakes left by extracting potassium from potassium feldspar |
| CN104773748A (en) * | 2015-03-10 | 2015-07-15 | 江苏永葆环保科技股份有限公司 | Method for preparing low-iron polyaluminium sulfate by using aluminiferous waste sulfuric acid mother liquor |
Non-Patent Citations (2)
| Title |
|---|
| 张雷: "废铝渣制备新型高分子絮凝剂的研究", 《中国优秀硕士学位论文全文数据库》 * |
| 王运正等: "《现代锰冶金》", 30 September 2015 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110386616A (en) * | 2019-08-14 | 2019-10-29 | 淄博汇成净水剂科技有限公司 | A method of processing FCC dead catalyst produces aluminum sulfate |
| CN115417438A (en) * | 2022-08-30 | 2022-12-02 | 青岛惠城环保科技集团股份有限公司 | Method for synthesizing hydrotalcite-like material by using waste catalyst as aluminum source |
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Application publication date: 20170104 |