CN107434255B - A method of utilizing waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum series product - Google Patents
A method of utilizing waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum series product Download PDFInfo
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- CN107434255B CN107434255B CN201610930742.3A CN201610930742A CN107434255B CN 107434255 B CN107434255 B CN 107434255B CN 201610930742 A CN201610930742 A CN 201610930742A CN 107434255 B CN107434255 B CN 107434255B
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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
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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
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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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
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/466—Conversion of one form of calcium sulfate to another
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Abstract
The present invention provides a kind of methods using waste hydrochloric acid containing aluminium, aluminium-containing sludge production aluminium polychloride and gypsum series product.The method first uses waste hydrochloric acid containing aluminium invade mentioning to aluminium-containing sludge as solvent, aluminium ion therein is sufficiently invaded and is mentioned to once invading in extract, solid after separation is containing a small amount of aluminum ions calcium sulphate dihydrate, diluted acid containing aluminium is further used, as solvent two is carried out without aluminium dilute hydrochloric acid, invades mention three times, after being finally 6.5-7.5 with clear water and regulator adjustment PH, it filters out solid drying and dewatering and produces anhydrous plaster powder, and produce the building material series products such as light gypsum board in turn.Once invade extract with two, the aluminium hydroxide invading in extract and obtains three times carries out polymerization reaction generation liquid aluminium polychloride under the cooperation of regulator, be finally concentrated and be spray-dried and produce 30% solid polyaluminium chloride.The harmless treatment of electrode platinum industry waste hydrochloric acid, useless aluminium-containing sludge had both may be implemented in the present invention, can also realize resource utilization.
Description
Technical field
The invention belongs to chemical waste harmless treatments and resource utilization field, are related to a kind of generation of electrode platinum enterprise
The harmless treatment of waste hydrochloric acid containing aluminium and aluminium-containing sludge and the technology of resource utilization.
Background technique
A large amount of waste hydrochloric acid containing aluminium, Waste Sulfuric Acid containing aluminium, acid waste water containing aluminium can be generated in electrode platinum production process, these acid
Property liquid waste belong to dangerous waste, it is necessary to be first neutralized with alkali, in sodium hydroxide and neutralize cost it is very high, enterprise is difficult to
It bears, although cheap with lime neutralization, but a large amount of aluminium-containing sludge can be generated.It is reported that only Nantong Area just have it is tens of
Electrode platinum enterprise, family, the various spent acid hundreds of thousands tons generated every year, the whole country are even more to have million tons of acid waste waters, these
If dangerous waste cannot get effective and reasonable disposition, it will cause serious influence to the normal production run of environment and enterprise.
The traditional treatment method of enterprise is first to carry out film process to highly concentrated spent acid at present, extracts the sour reuse work of a part
Skill, remaining diluted acid are neutralized with lime again.Discharged wastewater met the national standard after neutralization, the sludge of generation try to fill again.Due to generating
Sludge be also defined as dangerous waste at present, and due in sludge can the sliming due to variation of moisture content containing aluminium flocculating agent.
To above situation, enterprise has a headache very much, additional these resource itself are wasting, therefore, at the recycling of these wastes
Reason causes the attention of relevant enterprise and scientific research institution, and various processing methods continue to bring out.
Probably there are following methods in the country to the method for electrode platinum waste hydrochloric acid, Waste Sulfuric Acid, aluminium-containing sludge recycling treatment at present:
Direct making aluminium polychloride.It is directly added into calcium aluminate powder in the aluminium containing salt acid of 16-18%, produces polyaluminium
Aluminium.This method is feasible, but since the variety variations of waste hydrochloric acid containing aluminium are big, a considerable number of, not only needs a large amount of calcium aluminate
Powder, and yield is big, cost reduction is simultaneously few, therefore, it is difficult to guarantee that sale is smooth, scale performance difficulty.
Vacuum distillation crystallisation.Waste hydrochloric acid is pumped into circulating evaporator, waste hydrochloric acid starts to evaporate at 102 DEG C, into rectifying
Water and hydrochloric acid are separated in device, concentrate low temperature crystallization after evaporation, centrifugal dehydration, product is the crystalline hydrate of alchlor, is steamed
The hydrochloric acid issued applies electrode platinum production technology.Waste Sulfuric Acid can also be by this process.The technology to equipment anticorrosion performance
It is required that tight, investment is big, and operating cost is high, and is difficult to handle to diluted acid and sludge.
Exchange resin method.This method swaps spent acid by more than half aluminium ion by resins exchange by resin.Exchange
Spent acid afterwards continues to apply technique after adding concentration, and the aluminium in resin produces alchlor water purification agent after being stripped with diluted acid.The party
Method equally exist processing medium it is single, treating capacity is limited, equipment is huge, it is difficult to scale operation defect.
To sum up, it is domestic at present it is a kind of for electrode platinum enterprise spent acid, sewage sludge harmlessness, recycling, effective, energy
The process route of large scale processing.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention is provided a kind of produced using waste hydrochloric acid containing aluminium and aluminium-containing sludge and polymerize
Electrode platinum industry waste hydrochloric acid containing aluminium had both may be implemented, the innoxious of aluminium-containing sludge of giving up in the method for aluminium chloride and gypsum series product
Processing, can also realize the purpose of its resource utilization.
To solve the above problems, the present invention adopts the following technical scheme:
A method of aluminium polychloride and gypsum series product being produced using waste hydrochloric acid containing aluminium and aluminium-containing sludge,
It uses 16-18% waste hydrochloric acid containing aluminium invade mentioning to aluminium-containing sludge as solvent, aluminium ion therein is sufficiently invaded and is mentioned
To once invading in extract, the solid after separation is containing a small amount of aluminum ions calcium sulphate dihydrate；Further with diluted acid containing aluminium, without aluminium
Dilute hydrochloric acid is invaded separation solid above again respectively as solvent and is mentioned, and is finally 6.5- with clear water and regulator adjustment system PH
After 7.5, filters out solid and drying and dewatering produces anhydrous plaster powder, and produce gypsum series product in turn；
It once invades extract and carries out polymerization reaction life under the cooperation of regulator with the aluminium hydroxide in extract and obtained is invaded again
At liquid aluminium polychloride, finally it is concentrated and carries out spray drying 30% solid polyaluminium chloride of production.
Preferably, the diluted acid containing aluminium is respectively the dilute hydrochloric acid containing aluminium or sulfuric acid of 2-8%, and the aluminium diluted acid that is free of is to concentration
It does not require, is mainly 1.5-2 as foundation using the PH of dilute acid soln.
Preferably, in the method the following steps are included:
(1) 16-18% waste hydrochloric acid and aluminium-containing sludge is stirred mixing according to the quality proportioning of 1.5-3:1, and passes through
Homogenizer is transferred to stir and heat up and in the special reactor of included filter device；
(2) heating special reactor keeps the temperature 160-200 minutes and sufficiently carries out once invading mentioning to 50-85 degree；
(3) what is filtered out once invades extract for making aluminium polychloride, and the solid after separation stays in kettle；
(4) 1-1.3 times of amount of solid of water is added into kettle, and adjusts acidity with diluted acid containing aluminium, stirring evenly rear system PH is
1.5-2 then heats to 50-60 degree range and keeps the temperature extraction 100-120 minutes, and the liquid filtered out invades extract to be secondary, Gu
Body material is stayed in further to invade in kettle and be mentioned；
(5) enter clear water or draining up to standard into kettle, adjusting PH with lime or liquid alkaline after stirring evenly at normal temperature is 6.5-
7.5, it is then separated by filtration with filter press, separation liquid can be used as the raw water invaded mention again and use, and solid is used to produce anhydrous
Gypsum；
(6) it once invades extract and the aluminium hydroxide from production carries out polymerization reaction under the assistance of regulator and makes in liquid
Aluminum oxide content reach or approach 10%, be then 3-4 with regulator adjustment PH, basicity be greater than 40% terminate it is anti-
It answers, appropriate evaporation is so that aluminum oxide concentration reaches 13-14% in liquid, finally by steaming dry in atomizing drying tower
Hair, produces the solid polyaluminium chloride that aluminum oxide content reaches 30%.
It preferably, further include that clear water or draining up to standard are added into kettle after step (4), with without aluminium diluted acid after stirring evenly
Adjustment PH is 1.5-2, is extracted 60-90 minutes in the heat preservation of 40-50 degree, the liquid filtered out is to invade extract three times, and solid material stays in
Cleaning is further neutralized in kettle.
Preferably, after step (6) further include:
Solid after cleaning under the heated-air drying of 150-180 degree, obtains anhydrous plaster powder by rotary kiln drying oven, and
Gypsum material series building product is produced by forming machine；
Two, dilute three times to invade extract merging, it is 5-6 with 30% sodium hydroxide, soda ash, sodium bicarbonate or lime adjustment PH, adds
Enter stratification after polyacrylamide flocculation sedimentation, lower part solid is press-filtered out aluminium hydroxide, and top clear water applies technique, and periodically
Qualified discharge.
Preferably, the sludge is the aluminium-containing sludge in electrode platinum enterprise's spent acid or waste water and generated, and ingredient is mainly
The aluminum oxide of 6-8% and the calcium sulfate of 12-22%, the moisture of 70-80%；Hydrochloric acid mass concentration in the waste hydrochloric acid containing aluminium
For 5-18%, aluminium mass concentration is 0.1-2%.
Preferably, the regulator is lime, liquid alkaline, soda ash or hydrochloric acid.
Preferably, described be 31% technical hydrochloric acid and water without aluminium diluted acid according to dilute acid soln PH is that 1.5-2 is blent.
The beneficial effects of the present invention are:
(1) treated, and solid residue obtains harmless treatment, and the land plaster produced is pure white, with high purity, and subsequent building materials produce
Quality is secure；
(2) the biggest factor for influencing aluminium polychloride sale is cost and quality, and cost the biggest factor is aluminum oxide,
And this technique silicon source all is from waste, thus it is at low cost, for additional electrodes platinum spent acid containing aluminium in addition to aluminium and acid, other impurity are few,
Product quality is easily guaranteed that；
(3) this technique by the pollutants such as useless concentrated hydrochloric acid, useless dilute hydrochloric acid, useless dilute sulfuric acid, aluminium-containing sludge innoxious together, resource
Neutralizing is determined, and it is not high to equipment requirement, investment is small, processing cost is small and can produce profit, mass production amplify scale be easy；
(4) waste water after producing product fully achieves the discharge standard of national tertiary effluent, technique production without secondary pollution
It is raw；
(5) waste hydrochloric acid containing aluminium, the harmlessness disposing of aluminium-containing sludge and the target of resource utilization are realized simultaneously.
Detailed description of the invention
By the way that embodiment is described in conjunction with following accompanying drawings, features described above of the invention and technological merit will become
More understands and be readily appreciated that.
Fig. 1 is process flow chart of the embodiment of the present invention.
Specific embodiment
The embodiment of the present invention described below with reference to the accompanying drawings.Those skilled in the art will recognize, not
Deviate the spirit and scope of the present invention in the case where, can with a variety of different modes or combinations thereof to described embodiment into
Row amendment.Therefore, attached drawing and description are regarded as illustrative in nature, and are not intended to limit the scope of the claims.This
Outside, in the present specification, attached drawing is drawn not in scale, and identical appended drawing reference indicates identical part.
The present embodiment is described in detail below with reference to Fig. 1.
A method of using waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum series product, with containing aluminium
Waste hydrochloric acid invade mentioning as solvent to aluminium-containing sludge, and aluminium ion therein is sufficiently invaded and is mentioned to once invading in extract, after separation
Solid be containing a small amount of aluminum ions calcium sulphate dihydrate, further use diluted acid containing aluminium, be free of aluminium dilute hydrochloric acid as solvent progress two,
It invades and mentions three times, after being finally 6.5-7.5 with water and regulator adjustment system PH, filter out solid and drying and dewatering produces anhydrous stone
Cream powder, and the building material series products such as light gypsum board are produced in turn；
It once invades extract and invades the aluminium hydroxide in extract and obtained with two, three times and carry out polymerizeing instead under the cooperation of regulator
Liquid aluminium polychloride should be generated, be finally concentrated and carries out spray drying 30% solid polyaluminium chloride of production.It is wherein described to invade
It mentions and refers to impregnating method of the solid sample to extract wherein solute with liquid solvent.
Wherein aluminium-containing sludge of electrode platinum enterprise, including all aluminium containing salts acid, sulfuric acid, nitric acid, phosphoric acid, waste acid water etc. are through stone
The sludge generated after grey neutralization reaction, calcium chloride and calcium nitrate are dissolved in water, can filter out, so solid to be processed is dirty containing aluminium
Mud main component is Al (OH)3And CaSO4.Aluminium-containing sludge in the present embodiment is in electrode platinum enterprise's spent acid or waste water and to generate
Aluminium-containing sludge, ingredient is mainly the aluminum oxide of 6-8% and the calcium sulfate of 12-22%, the moisture of 70-80%；It is described
Hydrochloric acid mass concentration is 5-18% in waste hydrochloric acid containing aluminium, and aluminium mass concentration is 0.1-2%.
The hydrochloric acid of (1) 3 kilogram 16% (containing aluminum oxide 2.5%) is added in 5L glass reaction kettle, is added 1 kilogram containing solid
The aluminium-containing sludge of amount 22%, stirring evenly rear liquid PH is 0.2, and being transferred the material by Homogenizing pump can heat up and with filter screen
In special glass reaction kettle；
(2) to 80 degree or so, heat preservation sufficiently carries out extracting to invade mentioning temperature reaction device for 180 minutes；
(3) then one side pneumatics, filters on one side and liquid is transferred in polymerization reaction kettle, obtains once invades extract 3.3 altogether
Kilogram, the aluminum oxide content in liquid is 4.6%；
(4) into the solid material stayed in a kettle be added 1.5 kilograms of content of hydrochloric acid 5.5%, aluminium content 1% containing aluminium it is dilute
Acid, and the liquid level of clear water to 80% is supplemented, stirring evenly rear PH with lime adjustment system is 1.5-2, is warming up to 50 degree or so heat preservations and mentions
It takes 120 minutes, then one side pneumatics, filters on one side and secondary extract of invading is transferred in the neutralization reaction slot of about 10L；
(5) to the liquid level that clear water to 80% is added is stayed in the solid material in kettle, the PH after system stirs evenly is adjusted with hydrochloric acid
It for 1.5-2, is warming up to 40 degree or so heat preservations and extracts 60 minutes, then one side pneumatics again, extract will be invaded on one side three times by, which filtering, turns
It moves in the neutralization reaction slot of 10L；
(6) clear water is added into kettle to 80% liquid level, adjusting PH with regulator after stirring evenly at normal temperature is 6.5-7.5, so
It blowing and is separated by filtration afterwards with filter press, filters out about 0.6 kilogram of gypsum of moisture content 30%, separation water is as next time two, three
The secondary raw water for invading extract；
(7) by about 6 kilogram two, three times it is dilute invade extract merge, with liquid alkaline adjustment PH be 5-6, be added polyacrylamide after it is quiet
Layering is set, lower part solid is press-filtered out the aluminium hydroxide 90g of moisture content about 20%, and top clear water applies technique；
(8) it is dried 4 hours under 180 degree in an oven after the gypsum cleaning that (6) step obtains more than, obtains anhydrous gypsum
0.4 kilogram of powder, color is as white as polished jade, and solidification effect is good, can be used as production of construction materials.
(9) 3.3 kilograms of extracting solutions are added the aluminium hydroxide 340g from production, are warming up to 80 degree or so insulation reactions 2
A hour is 3.4 with lime adjustment PH, obtains 3.5 kilograms of aluminium polychloride of 10.2%, basicity 65%.Concentration and evaporation
The aluminum oxide 2780g of concentration 12.9% is obtained afterwards, and the solid that 150 degree of drying obtain 31.1% aluminum oxide for 8 hours is poly-
Close aluminium chloride 1200g.
Relative theory and reaction equation of the present invention are as follows:
It is mentioned 1. the aluminium hydroxide in sludge is invaded by acid solution, reaction equation are as follows:
3HCl (hydrochloric acid)+Al (OH)3(aluminium hydroxide)=AlCl3(alchlor)+3H2O (water)
Aluminium-containing sludge is mainly made of aluminium hydroxide and calcium sulfate, is invaded by acid and is proposed technique for the aluminium hydroxide quilt in sludge
Acid dissolution is into acid solution, and calcium sulfate does not dissolve in acidic liquid under Low acid, so the two is separated.
2. polymerization reaction:
Hydrochloric acid and aluminium hydroxide in aluminium containing salt acid carry out polymerization reaction under mildly acidic conditions, generate aluminium polychloride,
Reaction equation is as follows:
2Al(OH)3+ n HCl=Al2Cln(OH)6-n
3. basicity adjusts:
Basicity in aluminium polychloride requires to be greater than 40%, and basicity refers to working as OH and AL ion in aluminium polychloride
Measure percentage.So after polymerization reactor control aluminum oxide content determines AL (aluminium) ion concentration, by with lime or hydrogen
Sodium oxide molybdena is up to standard to adjust basicity to supplement OH concentration.
The present invention produces aluminium polychloride and plasterboard using the waste hydrochloric acid containing aluminium and aluminium-containing sludge of electrode platinum enterprise, and often
The aluminium polychloride and gypsum board manufacture technique of rule are compared, without purchasing hydrochloric acid, sulfuric acid, alumina powder, and will be at waste material
Utilization is set, by the CaSO in aluminium-containing sludge4Invade mention separation after obtain pure land plaster, by aluminium containing salt acid in chlorination
Al (OH) in aluminium, aluminium-containing sludge3It proposes polymerization by invading and obtains aluminium polychloride, significantly reduce production cost.
In addition a small amount of Waste Sulfuric Acid containing aluminium can be adulterated in the waste hydrochloric acid containing aluminium that electrode platinum enterprise generates, is produced through the invention
Technique can generate polyaluminium sulfate, due to polyaluminium sulfate and water treatment agent, so will not influence the water of product of the present invention
Treatment effect.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of method using waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum series product, feature exist
In: it the described method comprises the following steps:
(1) 16-18% waste hydrochloric acid containing aluminium and aluminium-containing sludge is stirred mixing according to the quality proportioning of 1.5-3:1, and passes through
Homogenizer is transferred to stir and heat up and in the special reactor of included filter device；
(2) heating special reactor keeps the temperature 160-200 minutes and sufficiently carries out once invading mentioning to 50-85 degree；
(3) what is filtered out once invades extract for making aluminium polychloride, and the solid after separation stays in kettle；
(4) 1-1.3 times of amount of solid of water is added into kettle, and adjusts acidity with diluted acid containing aluminium, stirring evenly rear system pH is 1.5-2,
It then heats to 50-60 degree range and keeps the temperature extraction 100-120 minutes, the liquid filtered out invades extract to be secondary, and solid material is stayed
It further invades and mentions in kettle；
(5) clear water is added into kettle, adjusting pH with regulator after stirring evenly at normal temperature is 6.5-7.5, is then filtered with filter press
Separation, separation liquid are used as the raw water mentioned is invaded again, and solid is used to produce anhydrous gypsum；
(6) once invade extract with from production aluminium hydroxide carried out under the assistance of regulator polymerization reaction make in liquid three
Al 2 O content reaches 10%, is then 3-4 with regulator adjustment pH, basicity is greater than 40%, and reaction was completed, appropriate to evaporate
So that aluminum oxide concentration reaches 13-14% in liquid, is evaporated finally by dry in atomizing drying tower, produce three oxygen
Change the solid polyaluminium chloride that two aluminium contents reach 30%.
2. according to claim 1 a kind of serial using waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum
The method of product, which is characterized in that
It further include that clear water is added into kettle after step (4), with being 1.5-2 without aluminium diluted acid adjustment pH after stirring evenly, in 40-50
Degree heat preservation is extracted 60-90 minutes, and the liquid filtered out is to invade extract three times, and solid material, which stays in, further neutralizes cleaning in kettle；
The diluted acid containing aluminium is the dilute hydrochloric acid containing aluminium or sulfuric acid of 2-8%.
3. according to claim 2 a kind of serial using waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum
The method of product, which is characterized in that
After step (6) further include:
Solid after cleaning under the heated-air drying of 150-180 degree, obtains anhydrous plaster powder, and pass through by rotary kiln drying oven
Forming machine produces gypsum material series building product；
Two, extract merging is invaded three times, is 5-6 with 30% sodium hydroxide, soda ash, sodium bicarbonate or lime adjustment pH, is added poly- third
Stratification after acrylamide flocculation sedimentation, lower part solid are press-filtered out aluminium hydroxide, and top clear water applies technique, and periodically row up to standard
It puts.
4. according to claim 1 a kind of serial using waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum
The method of product, which is characterized in that the aluminium-containing sludge is the aluminium-containing sludge in electrode platinum enterprise's spent acid or waste water and generated,
Ingredient is the aluminum oxide of 6-8% and the calcium sulfate of 12-22%, the moisture of 70-80%；Hydrochloric acid matter in the waste hydrochloric acid containing aluminium
Amount concentration is 5-18%, and aluminium mass concentration is 0.1-2%.
5. according to claim 1 a kind of serial using waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum
The method of product, which is characterized in that
The regulator is lime, liquid alkaline, soda ash or hydrochloric acid.
6. according to claim 2 a kind of serial using waste hydrochloric acid containing aluminium and aluminium-containing sludge production aluminium polychloride and gypsum
The method of product, which is characterized in that
Described be 31% technical hydrochloric acid and water without aluminium diluted acid according to dilute acid soln pH is that 1.5-2 is blent.
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| CN1948156A (en) * | 2006-10-31 | 2007-04-18 | 童益 | Method of producing aluminium polychloride using aluminium hydroxide mud |
| CN101549879B (en) * | 2009-05-12 | 2010-12-01 | 苏州市亨文环保水业有限公司 | Production method of polyaluminium chloride |
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