CN106673041B - A kind of production technology of efficiently highly concentrated polyaluminium chloride - Google Patents
A kind of production technology of efficiently highly concentrated polyaluminium chloride Download PDFInfo
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- CN106673041B CN106673041B CN201611225293.9A CN201611225293A CN106673041B CN 106673041 B CN106673041 B CN 106673041B CN 201611225293 A CN201611225293 A CN 201611225293A CN 106673041 B CN106673041 B CN 106673041B
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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
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
Abstract
The invention discloses a kind of production technology of efficiently highly concentrated polyaluminium chloride, in the case where not increasing a large amount of process equipments and other raw material, using the Aluminiferous waste slag after aluminium ingot, aluminium strip surface acid-washing waste liquid neutralisation treatment as raw material, efficient height is produced by negative pressure synergy concentration technology to thick liquid polyaluminium chloride, to substitute Conventional solid product.The technique is simple to operation, and Productive statistics are low, is adapted to industrialized production, obtained efficiently high concentrated liquid polyaluminium chloride and Conventional solid product purifying water effect are about 1:1, while Aluminiferous waste slag is utilized, the production cost of polyaluminium chloride is greatly lowered, " turning waste into wealth ", meets energy-saving and emission-reduction, the environmental protection concept of recycling economy.
Description
Technical field
The invention belongs to polyaluminium chloride production technical field, and in particular to a kind of production work of efficiently highly concentrated polyaluminium chloride
Skill.
Background technology
Polyaluminium chloride is a kind of efficient inorganic high-molecular coagulant adopting, have the advantages that efficiently, it is low consumption, inexpensive, convenient, it
Purifying water effect is considerably beyond other water purification agents such as ferric trichloride, aluminum sulfate.
At present, polyaluminium chloride mainly has liquid (alumina content >=10%) and solid (alumina content >=29%) two
Kind.Solid product is on the basis of fluid product, and fluid product is converted into solid product by techniques such as drying, drying,
This process adds the costs such as substantial amounts of artificial, fuel, equipment, packaging, carrying.The advantage of solid product is to transport at a distance
It is defeated cost-effective.But using preceding and solid product must be diluted preparation, solid product is added water by a certain percentage
Come into operation after coming back to liquid condition.And during fluid product changes into solid product, limited by technique,
General is difficult that 100% effective ingredient is completely converted into solid.Simultaneously in high-temperature drying procedures, the degree of polymerization of product by
Destroy.Therefore, the viscosity of fluid product can be than the viscosity of the fluid product after the solid of high temperature drying dilutes again, purity more
It is high.But because the active ingredient of polyaluminium chloride solid product is still high compared with fluid product, cause water treatment efficiency solid product with
Fluid product is about 1:2.7, therefore the cost performance of solid product long distance transportation is higher, fluid product market cannot still have
The popularization of effect.If efficiently highly concentrated fluid product can be selected, the water process effect as solid product is reached in water process
Fruit, then can solve caused various problems in drying process, while home or overseas can also be reached and found a good sale in, solid product it is excellent
It will definitely not exist, can more realize economic benefit.Therefore, produce the efficient height polyaluminium chloride that thicks liquid and directly substitute solid product
It is the revolutionary technical barrier for being currently badly in need of capturing.
The content of the invention
It is an object of the invention in place of overcome the deficiencies in the prior art, there is provided a kind of life of efficiently highly concentrated polyaluminium chloride
Production. art, in the case where not increasing a large amount of process equipments and other raw material, neutralized using aluminium ingot, aluminium strip surface acid-washing waste liquid
Aluminiferous waste slag after processing produces efficient height as raw material, by negative pressure synergy concentration technology and thicked liquid polyaluminium chloride, with for
For Conventional solid product.The technique is simple to operation, and Productive statistics are low, is adapted to industrialized production.Obtained efficiently high concentrated liquid
Polyaluminium chloride and Conventional solid product purifying water effect are about 1:1, while Aluminiferous waste slag is utilized, it is greatly lowered the production of polyaluminium chloride
Cost, " turning waste into wealth ", meet energy-saving and emission-reduction, the environmental protection concept of recycling economy.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of production technology of polyaluminium chloride, including：
Step 1：The hydrochloric acid of suitable quantity of water and 163~217 parts of total acidities 30~32% is configured to HCl volumes under agitation
Concentration is 22.5~24.5% hydrochloric acid solution；116~164 parts of aluminum oxide are added under normal pressure and temperature into the hydrochloric acid solution to contain
Measure the Aluminiferous waste slag for 15~20%, stirring to dissolving；Then it is persistently overheating to temperature of reaction system control at 100~125 DEG C,
3~4.5h is reacted under normal pressure；
Step 2：The feed liquid that step 1 is obtained supplements suitable quantity of water under agitation, adds 31~65 parts of calcium aluminate powder, adds
After water use regulation feed liquid density >=1.23g/ml, then add 5~8 parts of synergist tertiary sodium phosphate, be warming up to reaction system
Temperature control reacts 3.5~4.5h at 105~115 DEG C under normal pressure；
Step 3：The feed liquid that step 2 is obtained carries out separation of solid and liquid, obtains mother liquor；
Step 4：It is 1.40~1.45g/ml by the mother liquor concentrations that step 3 obtains to density, then cures 3~5 days, produces
Efficient high concentrated liquid polyaluminium chloride, its relative density are 1.40~1.45g/ml, alumina weight percentage composition >=20%, alkali
Spend ＞ 80.0%, pH value 3.5~5.0, water insoluble matter content ＜ 0.1%.
In one embodiment：The Aluminiferous waste slag is the Aluminiferous waste slag after aluminium ingot, aluminium strip surface acid-washing waste liquid neutralisation treatment, its
Alumina content is 15~20%, and moisture is 75~85%, impurity content ＜ 5%.
In one embodiment：In the calcium aluminate powder, acid-soluble aluminum content 48~54%, calcium oxide content 26~34%.
In one embodiment：In the step 3, separation of solid and liquid uses plate compression device.
In one embodiment：In the step 4, concentrated using negative pressure synergy enrichment facility.
Among the present invention, unless otherwise stated, according to the mass fraction, content is mass fraction to number.
The present invention is on the basis of using existing process equipment and raw material, is not increasing a large amount of process equipments and other
In the case of raw material, innovation and creation are carried out, product economy benefit is higher, while overcomes following production technology problem：
1. in the technique of the present invention, two not good liquors after calcium aluminate powder and synergist polymerisation are passed through into plate compression device
Press filtration, mother liquor is obtained, on the one hand ensures the purity of mother liquor, despumation is to polymerization effect in mother liquor negative pressure synergy concentration process
Influence, on the other hand, the impurity that can avoid containing in mother liquor impurity blocking device, damage in negative pressure synergy enrichment facility are set
It is standby, cause synergy concentration process not realize smoothly.And in existing production technology, in order to exclude waste residue impurity to existing process
The influence of former synergist calcium oxide or calcium hydroxide enhanced reaction of modification, it is that plate compression point must be carried out before calcium aluminate powder is added
Separate out mother liquor.Efficient high concentrated liquid polyaluminium chloride if the present invention according to the traditional handicraft, can not be obtained.
2. in order to realize the production of efficient highly concentrated polyaluminium chloride, invention introduces new synergist tertiary sodium phosphate, new synergy
Agent tertiary sodium phosphate can be engaged with follow-up negative pressure synergy enrichment facility and maturing process, promote and reach the increasing of polyaluminium chloride
Effect polymerization enrichment purification, has been significantly greatly increased hydroxyl overseas Chinese federation and has improved the product degree of polymerization, made alumina content, the molecule charge of product
The product quality indicators such as amount, coagulability, bin stability and basicity improve level.If using other synergist,
The efficient high concentrated liquid polyaluminium chloride of the present invention can not be obtained.
3. efficiently highly concentrated polyaluminium chloride technique is all linked with one another for whole production, indispensable, this is that present invention applicant passes through
Largely, prolonged development test, the final technology for summarizing invention.Added by the specific response parameter of modulation process, each raw material
Parts by weight and each raw material order of adding, these are all the key factors of the efficient highly concentrated polyaluminium chloride of present invention production.If each original
Material adds that ratio of weight and number is improper, each raw material order of adding is incorrect, each specific response parameter of technique does not regulate and control, then can not
Smoothly complete the production of efficient highly concentrated polyaluminium chloride.
The efficient high concentrated liquid polyaluminium chloride that the present invention obtains, the relative density at 20 DEG C are 1.40~1.45g/ml,
Alumina weight percentage composition >=20%, basicity ＞ 80.0%, pH value 3.5~5.0, water insoluble matter content ＜ 0.1%, meet
GB15892-2009 standards.And it is >=1.15g/ according to relative density of the liquid polyaluminium chloride of existing process production at 20 DEG C
Ml, alumina weight percentage composition >=10%, basicity ＞ 75.0%, pH value 3.5~5.0, water insoluble matter content ＜ 0.1%.
There is larger gap in the two, the efficient height for illustrating that the present invention can not be produced according to existing process thicks liquid polyaluminium chloride production
Product.
By it is produced by the present invention efficiently high concentrated liquid polyaluminium chloride product with certain using conventional material production product and
GB15892-2009 quality index contrast such as following table：
As can be seen from the above table, efficiently high its alumina content of concentrated liquid polyaluminium chloride, basicity, water produced by the present invention
Insolubles content is superior to the product of conventional raw materials production.
Secondly, by efficient highly concentrated polyaluminium chloride (liquid) 1#, conventional polyaluminium chloride (solid) 2# of the invention prepared and often
Polyaluminium chloride (liquid) 3# is advised, water factory (takes each medicament optimal by six stirring instruments progress coagulation contrast test in Quanzhou
Dosage detects effluent quality), as a result such as following table：
As can be seen from the above table, existing process fluid product water treatment efficiency and Conventional solid product are about 2.7:1.And this
Each comprehensive physical and chemical index of invention product is superior to conventional liq polyaluminium chloride product, the water process with Conventional solid polyaluminium chloride
Effect is about 1:1, this is that existing process can not be realized.
Compared with background technology, it has the following advantages that the technical program：
1. the Aluminiferous waste slag of the invention using after aluminium ingot, aluminium strip surface acid-washing waste liquid neutralisation treatment is as raw material, by negative
Pressure synergy concentration technology produces efficient height and thicked liquid polyaluminium chloride product.Not only each cost of material is relatively low but also technical matters
It is relatively simple, while Aluminiferous waste slag is utilized, reduce environmental pollution to greatest extent, " turning waste into wealth ", " treatment of wastes with processes of wastes against one another ", to reach
Energy-saving and emission-reduction, the environmental protection concept of recycling economy.
2. adding synergist in process of production, while by negative pressure synergy concentration technology, hydroxyl overseas Chinese federation is significantly greatly increased
The product degree of polymerization is improved, produces alumina content, molecule charge amount, coagulability, bin stability and basicity of product etc.
Quality figureofmerit improves level.
3. in the case where not increasing a large amount of process equipments and other raw material, using aluminium ingot, aluminium strip surface acid-washing waste liquid
Aluminiferous waste slag after neutralisation treatment produces the efficient height polyaluminium chloride that thicks liquid as raw material, by negative pressure synergy concentration technology and produced
Product.Parts by weight and each raw material order of adding are added by the specific response parameter of modulation process, each raw material, these are all the present invention
The key factor of the efficient highly concentrated polyaluminium chloride of production.This is that present invention applicant passes through a large amount of, prolonged development test, finally
Summarize the technology of invention.If each raw material adds, ratio of weight and number is improper, each raw material order of adding is incorrect, each technique is specifically anti-
Answer parameter not regulate and control, then can not smoothly complete the production of efficient highly concentrated polyaluminium chloride.
4. it is produced by the present invention efficiently high concentrated liquid polyaluminium chloride product alumina content >=20%, purifying water effect with often
It is about 1 to advise solid product:1, complete alternative solid product.Fluid product is effectively saved by techniques such as dry, drying to turn
Change solid product, the cost such as caused substantial amounts of artificial, fuel, equipment, packaging, carrying into, while avoid and done in high temperature
During dry, the loss of polyaluminium chloride product active ingredient and the destruction of the product degree of polymerization, solve solid product and using
The wasting of resources that occurs in journey, dust, the caking that makes moist, employee's occupational disease, labor intensity are big, packaging waste processing, environment are dirty
The problems such as dye.Efficient highly concentrated polyaluminium chloride facilitates long distance transportation, and suitable home or overseas is found a good sale in, and is greatly enlarged liquid polychlorostyrene
Change the market of aluminium, make it possible that fluid product substitutes solid product.
5. efficiently high concentrated liquid polyaluminium chloride properties of product produced by the present invention are suitable with Conventional solid polyaluminium chloride, and water
Insolubles content is relatively low so that the application of product is more wide.
Brief description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the technological process of production schematic diagram of the efficient highly concentrated polyaluminium chloride of the present invention.
Embodiment
Present disclosure is illustrated below by embodiment：
Embodiment 1
Step 1：, using in steam-heated acidproof primary first-order equation kettle, added while stirring appropriate with agitating device
Water and 175 parts of technical hydrochloric acids, it is configured to the hydrochloric acid solution that volumetric concentration is 22.8%；Under normal pressure and temperature into the hydrochloric acid solution
Add 138 parts of Aluminiferous waste slags, stirring to dissolving；Then it is persistently overheating to temperature of reaction system control at 100~125 DEG C, normal pressure
Lower reaction 3h；Sampling detection；
Step 2：The feed liquid that step 1 obtains is steam-heated acidproof to being utilized with agitating device by pumping
It polymerize in secondary response kettle, starts stirring, supplements suitable quantity of water, start to add 46 parts of calcium aluminate powder, water use regulation after adding
Feed liquid density 1.24g/ml, 6 parts of synergist tertiary sodium phosphate is then added, be warming up to temperature of reaction system control 105~115
DEG C, react 3.5h under normal pressure；Sampling detection；
Step 3：The secondary feed liquid that step 2 obtains is subjected to separation of solid and liquid by plate and frame filter press press filtration, obtains mother
446 parts of liquid；Sampling detection；
Step 4：The mother liquor that step 3 obtains is entered into negative pressure synergy enrichment facility by pumping and carries out synergy concentration, concentration
It is 1.41g/ml to density, then pumps it to aerobic fermentation tank, aeration curing 4 days under normal temperature and pressure, produces efficient high concentrated liquid polychlorostyrene
Change 238 parts of aluminium product, detection storage.Finished product meets GB15892-2009 standards.
Wherein, the technical hydrochloric acid is that (for total acidity in terms of HCl, i.e., 31%) HCl mass fraction is to total acidity 31%
Technical hydrochloric acid.The Aluminiferous waste slag is aluminium ingot, the Aluminiferous waste slag after aluminium strip surface acid-washing waste liquid neutralisation treatment, its alumina content
For 15~20%, moisture 80% or so, impurity ＜ 5%.In the calcium aluminate powder, acid-soluble aluminum content 50%, calcium oxide contains
Amount 28~31%.
Embodiment 2
Step 1：, using in steam-heated acidproof primary first-order equation kettle, added while stirring appropriate with agitating device
Water and 209 parts of technical hydrochloric acids, it is configured to the hydrochloric acid solution that volumetric concentration is 24%；Add under normal pressure and temperature into the hydrochloric acid solution
Enter 157 parts of Aluminiferous waste slags, stirring to dissolving；Then it is persistently overheating to temperature of reaction system control at 100~125 DEG C, under normal pressure
React 4.5h；Sampling detection；
Step 2：The feed liquid that step 1 obtains is steam-heated acidproof to being utilized with agitating device by pumping
It polymerize in secondary response kettle, starts stirring, supplements suitable quantity of water, start to add 61 parts of calcium aluminate powder, water use regulation after adding
Feed liquid density 1.26g/ml, 8 parts of synergist tertiary sodium phosphate is then added, be warming up to temperature of reaction system control 105~115
DEG C, react 4h under normal pressure；Sampling detection；
Step 3：The secondary feed liquid that step 2 obtains is subjected to separation of solid and liquid by plate and frame filter press press filtration, obtains mother
521 parts of liquid；Sampling detection；
Step 4：The mother liquor that step 3 obtains is entered into negative pressure synergy enrichment facility by pumping and carries out synergy concentration, concentration
It is 1.44g/ml to density, then pumps it to aerobic fermentation tank, aeration curing 5 days under normal temperature and pressure, produces efficient high concentrated liquid polychlorostyrene
Change 275 parts of aluminium product, detection storage.Finished product meets GB15892-2009 standards.
Wherein, the technical hydrochloric acid is that (for total acidity in terms of HCl, i.e., HCl contents are Nacl 31%) to total acidity 31%
Acid.The Aluminiferous waste slag is aluminium ingot, the Aluminiferous waste slag after aluminium strip surface acid-washing waste liquid neutralisation treatment, its alumina content is 15~
20%, moisture 80% or so, impurity ＜ 5%.In the calcium aluminate powder, acid-soluble aluminum content 50%, calcium oxide content 28~
31%.
Embodiment 3
Step 1：, using in steam-heated acidproof primary first-order equation kettle, added while stirring appropriate with agitating device
Water and 188 parts of technical hydrochloric acids, it is configured to the hydrochloric acid solution that volumetric concentration is 23.5%；Under normal pressure and temperature into the hydrochloric acid solution
Add 149 parts of Aluminiferous waste slags, stirring to dissolving；Then it is persistently overheating to temperature of reaction system control at 100~125 DEG C, normal pressure
Lower reaction 4h；Sampling detection；
Step 2：The feed liquid that step 1 obtains is steam-heated acidproof to being utilized with agitating device by pumping
It polymerize in secondary response kettle, starts stirring, supplements suitable quantity of water, start to add 54 parts of calcium aluminate powder, water use regulation after adding
Feed liquid density 1.25g/ml, 7 parts of synergist tertiary sodium phosphate is then added, be warming up to temperature of reaction system control 105~115
DEG C, react 4.5h under normal pressure；Sampling detection；
Step 3：The secondary feed liquid that step 2 obtains is subjected to separation of solid and liquid by plate and frame filter press press filtration, obtains mother
477 parts of liquid；Sampling detection；
Step 4：The mother liquor that step 3 obtains is entered into negative pressure synergy enrichment facility by pumping and carries out synergy concentration, concentration
It is 1.43g/ml to density, then pumps it to aerobic fermentation tank, aeration curing 3 days under normal temperature and pressure, produces efficient high concentrated liquid polychlorostyrene
Change 246 parts of aluminium product, detection storage.Finished product meets GB15892-2009 standards.
Wherein, the technical hydrochloric acid is that (for total acidity in terms of HCl, i.e., HCl contents are Nacl 31%) to total acidity 31%
Acid.The Aluminiferous waste slag is aluminium ingot, the Aluminiferous waste slag after aluminium strip surface acid-washing waste liquid neutralisation treatment, its alumina content is 15~
20%, moisture 80% or so, impurity ＜ 5%.In the calcium aluminate powder, acid-soluble aluminum content 50%, calcium oxide content 28~
31%.
It is described above, only present pre-ferred embodiments, therefore the scope that the present invention is implemented can not be limited according to this, i.e., according to
The equivalent changes and modifications that the scope of the claims of the present invention and description are made, all should still it belong in the range of the present invention covers.
Claims (5)
- A kind of 1. production technology of polyaluminium chloride, it is characterised in that：Including：Step 1：The hydrochloric acid of suitable quantity of water and 163~217 parts of total acidities 30~32% is configured to HCl volumetric concentrations under agitation For 22.5~24.5% hydrochloric acid solution；Adding 116~164 parts of alumina contents into the hydrochloric acid solution under normal pressure and temperature is 15~20% Aluminiferous waste slag, stirring to dissolving；Then it is persistently overheating to temperature of reaction system control at 100~125 DEG C, normal pressure 3~4.5h of lower reaction；Step 2：The feed liquid that step 1 is obtained supplements suitable quantity of water under agitation, adds 31~65 parts of calcium aluminate powder, adds and finish Water use regulation feed liquid density >=1.23g/mL afterwards, 5~8 parts of synergist tertiary sodium phosphate is then added, is warming up to temperature of reaction system Control reacts 3.5~4.5h at 105~115 DEG C under normal pressure；Step 3：The feed liquid that step 2 is obtained carries out separation of solid and liquid, obtains mother liquor；Step 4：It is 1.40~1.45g/mL by the mother liquor concentrations that step 3 obtains to density, then cures 3~5 days, produces liquid Body polyaluminium chloride, its relative density are 1.40~1.45g/mL, alumina weight percentage composition >=20%, basicity ＞ 80.0%, pH value 3.5~5.0, water insoluble matter content ＜ 0.1%；Wherein, unless otherwise stated, according to the mass fraction, content is mass fraction to number.
- 2. the production technology of polyaluminium chloride according to claim 1, it is characterised in that：The Aluminiferous waste slag is aluminium ingot, aluminium Aluminiferous waste slag after belt surface pickle liquor neutralisation treatment, its alumina content are 15~20%, and moisture is 75~85%, Impurity content ＜ 5%.
- 3. the production technology of polyaluminium chloride according to claim 1, it is characterised in that：In the calcium aluminate powder, dissolved aluminum Content 48~54%, calcium oxide content 26~34%.
- 4. the production technology of polyaluminium chloride according to claim 1, it is characterised in that：In the step 3, separation of solid and liquid Using plate compression device.
- 5. the production technology of polyaluminium chloride according to claim 1, it is characterised in that：In the step 4, using negative pressure Synergy enrichment facility is concentrated.
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| CN114084895A (en) * | 2021-04-08 | 2022-02-25 | 内蒙古蒙泰集团有限公司 | Preparation method of polyaluminum chloride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5904856A (en) * | 1995-01-24 | 1999-05-18 | Kemira Kemi Aktiebolag | Process for the preparation of aluminum salt solutions |
| CN101531389A (en) * | 2009-03-26 | 2009-09-16 | 嘉善海峡净水灵化工有限公司 | Method for producing polyaluminium chloride |
| CN102070170A (en) * | 2009-11-19 | 2011-05-25 | 蓝保(厦门)水处理科技有限公司 | Method for producing polyaluminium chloride |
| CN104477959A (en) * | 2014-12-18 | 2015-04-01 | 嘉善海峡净水灵化工有限公司 | Production process of high-concentration polyaluminium chloride |
-
2016
- 2016-12-27 CN CN201611225293.9A patent/CN106673041B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5904856A (en) * | 1995-01-24 | 1999-05-18 | Kemira Kemi Aktiebolag | Process for the preparation of aluminum salt solutions |
| CN101531389A (en) * | 2009-03-26 | 2009-09-16 | 嘉善海峡净水灵化工有限公司 | Method for producing polyaluminium chloride |
| CN102070170A (en) * | 2009-11-19 | 2011-05-25 | 蓝保(厦门)水处理科技有限公司 | Method for producing polyaluminium chloride |
| CN104477959A (en) * | 2014-12-18 | 2015-04-01 | 嘉善海峡净水灵化工有限公司 | Production process of high-concentration polyaluminium chloride |
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