CN108862206A - The technique that a kind of ardealite and red mud prepare aluminium coproduction humic acid complex fertilizer - Google Patents
The technique that a kind of ardealite and red mud prepare aluminium coproduction humic acid complex fertilizer Download PDFInfo
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- CN108862206A CN108862206A CN201810711214.8A CN201810711214A CN108862206A CN 108862206 A CN108862206 A CN 108862206A CN 201810711214 A CN201810711214 A CN 201810711214A CN 108862206 A CN108862206 A CN 108862206A
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- red mud
- humic acid
- ardealite
- complex fertilizer
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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
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
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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
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
Abstract
The present invention provides the techniques that a kind of ardealite and red mud prepare aluminium coproduction humic acid complex fertilizer, include the following steps：Ardealite, red mud, additive and modifying agent are mixed and ground, raw material are made, roasted, clinker is made；Clinker is dissolved out, and is separated by solid-liquid separation；Aluminium oxide is extracted to obtain in isolated solution；Isolated residue obtains sulfide through flotation；The concentrated sulfuric acid is produced into sulfide processing；The concentrated sulfuric acid is added in conversion reaction slot, humic acid, potassium chloride, ammonium chloride and phosphoric acid are added in conversion reaction slot, mixed acid slurry is stirred into；Mixed acid slurry is transferred in neutralization reactor, excessive ammonia reaction is passed through, obtains slurry, be sent into pelletizer, magnesium powder, calcium powder mixing is added, granulation forms material；By dry materials, cooling, screening, humic acid complex fertilizer is obtained.The present invention, which has, mentions aluminium and to prepare humic acid complex fertilizer at low cost, and waste residue utilization rate is high, and aluminium recovery is high, purity is high, the high feature of humic acid complex fertilizer quality.
Description
Technical field
The present invention relates to the techniques that a kind of ardealite and red mud prepare aluminium coproduction humic acid complex fertilizer, belong to chemical metallurgy neck
Domain.
Background technique
The solid slag that ardealite generates when referring in phosphoric acid production with sulfuric acid treating phosphorite, main component are sulfuric acid
Calcium（CaSO4）, content generally can reach 70-90% or so.In addition, ardealite also contains plurality of impurities：Undecomposed phosphorus ore,
Phosphoric acid, calcirm-fluoride, iron, aluminium compound, acid non-soluble substance, organic matter of non-washes clean etc..Ardealite is discharged every year about in China
20000000 tons, add up nearly hundred million tons of discharge capacity.For utilization rate of the ardealite in terms of building materials less than 5%, a large amount of gypsum stacks occupy soil
Ground seriously pollutes environment.
Red mud is to refine the waste generated in alumina process with bauxite.It is in crimson color muddy because it is rich in iron
And it gains the name.1 ton of aluminium oxide of every production about generates red mud 1.0-2.0 tons.The year yield of China's red mud is about 1.0 hundred million tons, is tired out
Counting volume of cargo in storage is about 500,000,000 tons.
Humic acid is the larger molecular organics matter being widely present in nature, be widely used in Agriculture, forestry And Animal Husbandry, petroleum, chemical industry,
The every field such as building materials, medical and health, environmental protection, across tens industries.There are many purposes for humic acid and its product.In agricultural side
Face, the manufactured humic acid fertilizer in conjunction with the elements such as nitrogen, phosphorus, potassium, have fertilizer synergistic, improvement soil, stimulation plant growth,
Improve the functions such as agricultural product quality.Humic acid complex fertilizer is prepared by low temperature conversion method, is first added in conversion reaction slot
The a large amount of concentrated sulfuric acid generates raw material with the compound of humic acid potassium copolymer in conversion reaction slot by metathesis reaction
Fertilizer, while the humic acid macromolecular dissociated during neutralization reaction polymerize generation ammonium humate with gas ammonia, substantially increases work
Effective combination of the humic acid and N P and K of property, solves and largely applies soil caused by inorganic fertilizer in agricultural production for a long time
The bottleneck problem that salination, getting fat do not increase income.In existing humic acid complex fertilizer preparation process, the concentrated sulfuric acid used is mostly
It is prepared by sulphur ore calcination, and the production technology of the concentrated sulfuric acid is complicated, causes the concentrated sulfuric acid at high cost, greatly increases corruption
The production cost of phytic acid compound fertilizer.
It is existing currently, seldom for the technology of the comprehensive utilization of ardealite and red mud, be substantially focused on building materials and pave the way etc. and is traditional
Field, causes the waste of a large amount of high value ingredients in ardealite and red mud, and added value is very low.Although existing current some benefits
Technique with red mud recycling aluminium is mature, still, is required to add considerable amount of reactive material progress instead in these processes
It answers, this considerably increases cost recovery.And ardealite and red mud comprehensive utilization are extracted to recycling aluminium, while coproduction humic acid is multiple
The technique in Hefei, has not been reported.
Goal of the invention
The object of the present invention is to provide the techniques that a kind of ardealite and red mud prepare aluminium coproduction humic acid complex fertilizer.The present invention
With aluminium is mentioned and to prepare humic acid complex fertilizer at low cost, waste residue utilization rate is high, and aluminium recovery is high, purity is high, humic acid complex fertilizer
The high feature of quality.
Technical solution of the present invention
A kind of ardealite and red mud prepare the technique of aluminium coproduction humic acid complex fertilizer, include the following steps：
A, ardealite, red mud, additive and modifying agent are mixed and is ground and raw material are made, be sent into roasting in kiln, clinker is made；
B, clinker made from step A is dissolved out, and is separated by solid-liquid separation；
C, CO is added into step B isolated solution2It is no longer generated to white precipitate, it is clear after then filtering out white precipitate
Drying and calcination are washed, aluminium oxide is obtained；
D, by step B isolated residue through flotation, sulfide is separated to obtain；
E, the step D sulfide isolated is placed under the oxygen-enriched environment of 30-50%, 3-5h is roasted at 800-1200 DEG C, roasted
The flue gas of generation is absorbed using the concentrated sulfuric acid after vanadic anhydride catalysis reaction, dilutes to obtain the concentrated sulfuric acid；
F, the concentrated sulfuric acid that step E is prepared is added in conversion reaction slot, preheats to the concentrated sulfuric acid in conversion reaction slot,
After the completion of preheating, humic acid, potassium chloride and ammonium chloride are even added to conversion reaction slot, phosphoric acid is then added, stirs evenly
Form mixed acid slurry；
G, mixed acid slurry made from step F is transferred in neutralization reactor, then passes to excessive ammonia and neutralization reaction occurs
About 10-20 minutes, slurry was sent into pelletizer by the slurry obtained after reaction, is added in pelletizer and is mixed by magnesium powder, calcium powder
Afterwards, pelletizer is granulated to form material；
H, after the dry materials for forming step G, through cooling, screening, humic acid complex fertilizer is obtained.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, and in step A, the red mud is
The red mud that alumina producing Bayer process generates；The additive is sodium carbonate or caustic soda；The modifying agent is anthracite, carbon or coal
Spoil.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, in step A, the raw material
In, ardealite and Bayer red mud are according to 1:The ratio of 0.8-2 weight ratio mixes, and additive adding proportion is by contained Na in raw material2O
And A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, the mixed proportion of modifying agent are the 10-25% of raw material total weight.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, and in step A, the kiln is industry
Rotary kiln, Industry Tunnel Kiln or industrial shaft kiln.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, are in temperature in step A
Calcining time 1-2h at 1000-1350 DEG C.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, in step B, clinker elder generation water
It is dissolved out after mill；It is 4-6 that liquid when dissolution, which consolidates volume ratio,:1.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, and in step C, calcination is in temperature
Calcination time 2-5h at 800-1200 DEG C.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, in step F, by weight,
The mixed acid slurry include concentrated sulfuric acid 250-300 parts, 80-120 parts of potassium chloride, 50-80 parts of phosphoric acid, 120-160 parts of humic acid,
10-15 parts of ammonium chloride；In step G, by weight, the magnesium powder of addition is 20-25 parts, and calcium powder is 20-25 parts.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, are converted in step F, after preheating anti-
The temperature for answering the concentrated sulfuric acid in slot is 80-90 DEG C.
Ardealite and red mud above-mentioned are prepared in the technique of aluminium coproduction humic acid complex fertilizer, it is characterised in that：In step H,
The drying temperature of the material is 100-120 DEG C.
The present invention is by making utility for ardealite and red mud reaction, recombination.The net reaction of principle is：
CaSO4（Ardealite）+ Na2O·SiO2·Al2O3（Red mud）→ Na2O·Al2O3 + CaO·SiO2↓+[sulphur]
From the reaction equation it is found that with the SiO in the CaO and red mud in ardealite2Generate calcium orthosilicate（ CaO·SiO2↓）Afterwards,
Obtain soluble fabulous sodium aluminate（Na2O·Al2O3）.[sulphur] in reaction equation refers to and adds modifying agent technique by raw material, raw
At metal sulfide, main component FeS；After leaching the sodium aluminate in clinker, obtained sediment flotation can be obtained
To FeS.
Beneficial effect
1, the present invention is by using ardealite and red mud as raw material, and is added after additive and modifying agent, in high-temperature roasting
Technique under obtain the clinker of main silicate-containing, aluminate and sulfide, and the main component of the aluminate is sodium aluminate, will
Sodium aluminate it is water-soluble go out after may be recovered aluminium, and after solid residue flotation, obtain sulfide, dense sulphur prepared using sulfide
Acid is first added a large amount of concentrated sulfuric acid in conversion reaction slot, generates raw material with corruption in conversion reaction slot by metathesis reaction
POTASSIUM PHYTATE is the compound fertilizer of copolymer, while the humic acid macromolecular dissociated during neutralization reaction polymerize generation corruption with gas ammonia
Phytic acid ammonium substantially increases effective combination of active humic acid and N P and K, due in entire technique mainly with ardealite and
Red mud is raw material, adds other a small amount of substances, therefore, greatly reduces recycling aluminium and prepares the cost of humic acid complex fertilizer
Investment.Meanwhile the utilization rate of ardealite and waste red mud residues is also greatly increased, to alleviate the pollution of ardealite and red mud to environment
With important contribution.
2, after the raw material that the present invention passes through is by roasting, obtained ingredient is clearly demarcated, and aluminium is mainly with the presence of aluminic acid na form, benefit
The characteristic of water is highly soluble in sodium aluminate, can be simple and quick be isolated and for extracting aluminium oxide, the rate of recovery is high, and pure
Degree is high.
3, sulfuric acid impurity produced by the present invention is few, at low cost, and a large amount of concentrated sulfuric acid first is added in conversion reaction slot, makes raw material
It is generated by metathesis reaction using humic acid potassium as the compound fertilizer of copolymer in conversion reaction slot, while in neutralization reaction process
In after the humic acid macromolecular dissociated polymerize generation ammonium humate with gas ammonia, and magnesium powder and calcium powder is added, is granulated and is prepared into rotten plant
Sour compound fertilizer's quality is high, and humic acid complex fertilizer is at low cost.
Further to prove effect of the invention, inventor has done following experiment.
1, aluminium recovery detects
To the ardealite and red mud in following five groups of embodiments, the content of ardealite and the aluminium in red mud is detected respectively, this is sent out
Residue and addition CO in bright technique, after detection is separated by solid-liquid separation after having extracted2The aluminium in solution filtered out afterwards contains
It measures, residue and addition CO after the rate of recovery=separation of solid and liquid2The content ÷ ardealite and red mud of the aluminium in solution filtered out afterwards
In aluminium content -1, the as rate of recovery of aluminium.Meanwhile with the baking mixed traditional handicraft for extracting aluminium oxide of red mud and calcium oxide
As a comparison case.Experimental data is as shown in table 1：
1 present invention process of table and the aluminium recovery of traditional handicraft compare
2, humic acid complex fertilizer Quality Detection
Humic acid complex fertilizer component content obtained in following five groups of embodiments is detected respectively, each point of humic acid complex fertilizer
Analysis project and analysis method are according to national compound fertilizer quality standard GB15063-2001.
From table 2 it can be seen that humic acid content height, total available nutrient (N+P in humic acid complex fertilizer of the invention2O5+
K2O) high, also contain magnesium, calcium microelement, balling ratio is high, the high feature of humic acid complex fertilizer quality, and humic acid of the present invention is multiple
Hefei component content meets containing humic acid water-soluble fertilizer（A great number of elements type）Solid product technical indicator (standard No. NY1106-
2006) standard.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1：A kind of ardealite and red mud prepare the technique of aluminium coproduction humic acid complex fertilizer, and steps are as follows：
A, ardealite, Bayer red mud, sodium carbonate and anthracite are mixed and is ground and raw material are made, be sent into industrial rotary kiln in temperature
Clinker is made in calcining time 2h at 1000 DEG C of degree；Wherein, ardealite and Bayer red mud are according to 1:The ratio of 0.8 weight ratio mixes,
Sodium carbonate adding proportion is by contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, anthracitic mixing ratio
Example is the 10% of raw material total weight；
B, clinker made from step A is consolidated into volume ratio with liquid as 4:1 carries out water mill dissolution, and is separated by solid-liquid separation；
C, CO is added in isolated solution2It is no longer generated to white precipitate, white precipitate is then filtered out into rear cleaning, drying
And the calcination time 5h at 800 DEG C of temperature, obtain aluminium oxide；
D, by step B isolated residue through flotation, sulfide is separated to obtain；
E, step D is isolated under the oxygen-enriched environment that sulfide is placed in 30%, roasts 5h at 800 DEG C, roast the flue gas warp of generation
After vanadic anhydride catalysis reaction, is absorbed using 98% concentrated sulfuric acid, dilute to obtain 94% concentrated sulfuric acid；
F, 94% concentrated sulfuric acid that step E is prepared is added in conversion reaction slot, carries out to the concentrated sulfuric acid in conversion reaction slot pre-
Heat, the temperature of the concentrated sulfuric acid is 80 DEG C in conversion reaction slot after preheating, and humic acid, potassium chloride and ammonium chloride are even added to conversion
Then phosphoric acid is added in reactive tank, stir evenly to form mixed acid slurry；
G, mixed acid slurry made from step F is transferred in neutralization reactor, then passes to excessive ammonia and neutralization reaction occurs
About 10 minutes, slurry was sent into pelletizer by the slurry obtained after reaction, was added in pelletizer after mixing by magnesium powder, calcium powder,
Pelletizer is granulated to form material；
H, by material that step G is formed be 100 DEG C in temperature at be dried after, through cooling, screening, obtain humic acid complex fertilizer.
In above-mentioned steps F, by weight, the mixed acid slurry includes 250 parts of the concentrated sulfuric acid, 80 parts of potassium chloride, phosphoric acid
50 parts, 120 parts of humic acid, 10 parts of ammonium chloride；In step G, by weight, the magnesium powder of addition is 20 parts, and calcium powder is 20 parts.
Embodiment 2：A kind of ardealite and red mud prepare the technique of aluminium coproduction humic acid complex fertilizer, and steps are as follows：
A, ardealite, Bayer red mud, caustic soda and carbon are mixed and is ground and raw material are made, be sent into industrial rotary kiln in temperature 1200
Clinker is made in calcining time 1.5h at DEG C；Wherein, ardealite and Bayer red mud are according to 1:The ratio of 1.2 weight ratios mixes, caustic soda
Adding proportion is by contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, the mixed proportion of carbon are that raw material are total
The 15% of weight；
B, clinker made from step A is consolidated into volume ratio with liquid as 5:1 carries out water mill dissolution, and is separated by solid-liquid separation；
C, CO is added in isolated solution2It is no longer generated to white precipitate, white precipitate is then filtered out into rear cleaning, drying
And the calcination time 4h at 1000 DEG C of temperature, obtain aluminium oxide；
D, by step B isolated residue through flotation, sulfide is separated to obtain；
E, step D is isolated under the oxygen-enriched environment that sulfide is placed in 35%, roasts 4h at 1000 DEG C, roast the flue gas of generation
After vanadic anhydride catalysis reaction, is absorbed using 97% concentrated sulfuric acid, dilute to obtain 93% concentrated sulfuric acid；
F, 93% concentrated sulfuric acid that step E is prepared is added in conversion reaction slot, carries out to the concentrated sulfuric acid in conversion reaction slot pre-
Heat, the temperature of the concentrated sulfuric acid is 85 DEG C in conversion reaction slot after preheating, and humic acid, potassium chloride and ammonium chloride are even added to conversion
Then phosphoric acid is added in reactive tank, stir evenly to form mixed acid slurry；
G, mixed acid slurry made from step F is transferred in neutralization reactor, then passes to excessive ammonia and neutralization reaction occurs
About 15 minutes, slurry was sent into pelletizer by the slurry obtained after reaction, was added in pelletizer after mixing by magnesium powder, calcium powder,
Pelletizer is granulated to form material；
H, by material that step G is formed be 110 DEG C in temperature at be dried after, through cooling, screening, obtain humic acid complex fertilizer.
In above-mentioned steps F, by weight, the mixed acid slurry includes 250 parts of the concentrated sulfuric acid, 120 parts of potassium chloride, phosphoric acid
80 parts, 120 parts of humic acid, 15 parts of ammonium chloride；In step G, by weight, the magnesium powder of addition is 20 parts, and calcium powder is 25 parts.
Embodiment 3：A kind of ardealite and red mud prepare the technique of aluminium coproduction humic acid complex fertilizer, and steps are as follows：
A, ardealite, Bayer red mud, sodium carbonate and gangue are mixed and is ground and raw material are made, be sent into industrial rotary kiln in temperature
Clinker is made in calcining time 1.5h at 1300 DEG C of degree；Wherein, ardealite and Bayer red mud are according to 1:The ratio of 1.5 weight ratios is mixed
It closes, sodium carbonate adding proportion is by contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, gangue mix
Composition and division in a proportion example is the 20% of raw material total weight；
B, clinker made from step A is consolidated into volume ratio with liquid as 6:1 carries out water mill dissolution, and is separated by solid-liquid separation；
C, CO is added in isolated solution2It is no longer generated to white precipitate, white precipitate is then filtered out into rear cleaning, drying
And the calcination time 3h at 1200 DEG C of temperature, obtain aluminium oxide；
D, by step B isolated residue through flotation, sulfide is separated to obtain；
E, step D is isolated under the oxygen-enriched environment that sulfide is placed in 40%, roasts 4h at 1100 DEG C, roast the flue gas of generation
After vanadic anhydride catalysis reaction, is absorbed using 98% concentrated sulfuric acid, dilute to obtain 92% concentrated sulfuric acid；
F, 92% concentrated sulfuric acid that step E is prepared is added in conversion reaction slot, carries out to the concentrated sulfuric acid in conversion reaction slot pre-
Heat, the temperature of the concentrated sulfuric acid is 90 DEG C in conversion reaction slot after preheating, and humic acid, potassium chloride and ammonium chloride are even added to conversion
Then phosphoric acid is added in reactive tank, stir evenly to form mixed acid slurry；
G, mixed acid slurry made from step F is transferred in neutralization reactor, then passes to excessive ammonia and neutralization reaction occurs
About 20 minutes, slurry was sent into pelletizer by the slurry obtained after reaction, was added in pelletizer after mixing by magnesium powder, calcium powder,
Pelletizer is granulated to form material；
H, by material that step G is formed be 120 DEG C in temperature at be dried after, through cooling, screening, obtain humic acid complex fertilizer.
In above-mentioned steps F, by weight, the mixed acid slurry includes 280 parts of the concentrated sulfuric acid, 100 parts of potassium chloride, phosphoric acid
70 parts, 140 parts of humic acid, 13 parts of ammonium chloride；In step G, by weight, the magnesium powder of addition is 22 parts, and calcium powder is 22 parts.
Embodiment 4：A kind of ardealite and red mud prepare the technique of aluminium coproduction humic acid complex fertilizer, and steps are as follows：
A, ardealite, Bayer red mud, caustic soda and gangue are mixed and is ground and raw material are made, be sent into industrial rotary kiln in temperature
Clinker is made in calcining time 1h at 1350 DEG C；Wherein, ardealite and Bayer red mud are according to 1:The ratio of 1.8 weight ratios mixes, and burns
Alkali adding proportion is by contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, the mixed proportion of gangue are
The 25% of raw material total weight；
B, clinker made from step A is consolidated into volume ratio with liquid as 5:1 carries out water mill dissolution, and is separated by solid-liquid separation；
C, CO is added in isolated solution2It is no longer generated to white precipitate, white precipitate is then filtered out into rear cleaning, drying
And the calcination time 4h at 1100 DEG C of temperature, obtain aluminium oxide；
D, by step B isolated residue through flotation, sulfide is separated to obtain；
E, step D is isolated under the oxygen-enriched environment that sulfide is placed in 45%, roasts 4h at 1200 DEG C, roast the flue gas of generation
After vanadic anhydride catalysis reaction, is absorbed using 97% concentrated sulfuric acid, dilute to obtain 91% concentrated sulfuric acid；
F, 91% concentrated sulfuric acid that step E is prepared is added in conversion reaction slot, carries out to the concentrated sulfuric acid in conversion reaction slot pre-
Heat, the temperature of the concentrated sulfuric acid is 85 DEG C in conversion reaction slot after preheating, and humic acid, potassium chloride and ammonium chloride are even added to conversion
Then phosphoric acid is added in reactive tank, stir evenly to form mixed acid slurry；
G, mixed acid slurry made from step F is transferred in neutralization reactor, then passes to excessive ammonia and neutralization reaction occurs
About 15 minutes, slurry was sent into pelletizer by the slurry obtained after reaction, was added in pelletizer after mixing by magnesium powder, calcium powder,
Pelletizer is granulated to form material；
H, by material that step G is formed be 100 DEG C in temperature at be dried after, through cooling, screening, obtain humic acid complex fertilizer.
In above-mentioned steps F, by weight, the mixed acid slurry includes 300 parts of the concentrated sulfuric acid, 80 parts of potassium chloride, phosphoric acid
80 parts, 160 parts of humic acid, 15 parts of ammonium chloride；In step G, by weight, the magnesium powder of addition is 20 parts, and calcium powder is 20 parts.
Embodiment 5：A kind of ardealite and red mud prepare the technique of aluminium coproduction humic acid complex fertilizer, and steps are as follows：
A, ardealite, Bayer red mud, caustic soda and anthracite are mixed and is ground and raw material are made, be sent into industrial rotary kiln in temperature
Clinker is made in calcining time 2h at 1200 DEG C；Wherein, ardealite and Bayer red mud are according to 1:The ratio of 2 weight ratios mixes, caustic soda
Adding proportion is by contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, anthracitic mixed proportion are made a living
Expect the 20% of total weight；
B, clinker made from step A is consolidated into volume ratio with liquid as 5:1 carries out water mill dissolution, and is separated by solid-liquid separation；
C, CO is added in isolated solution2It is no longer generated to white precipitate, white precipitate is then filtered out into rear cleaning, drying
And the calcination time 3h at 1100 DEG C of temperature, obtain aluminium oxide；
D, by step B isolated residue through flotation, sulfide is separated to obtain；
E, step D is isolated under the oxygen-enriched environment that sulfide is placed in 50%, roasts 5h at 1100 DEG C, roast the flue gas of generation
After vanadic anhydride catalysis reaction, is absorbed using 97% concentrated sulfuric acid, dilute to obtain 94% concentrated sulfuric acid；
F, 94% concentrated sulfuric acid that step E is prepared is added in conversion reaction slot, carries out to the concentrated sulfuric acid in conversion reaction slot pre-
Heat, the temperature of the concentrated sulfuric acid is 90 DEG C in conversion reaction slot after preheating, and humic acid, potassium chloride and ammonium chloride are even added to conversion
Then phosphoric acid is added in reactive tank, stir evenly to form mixed acid slurry；
G, mixed acid slurry made from step F is transferred in neutralization reactor, then passes to excessive ammonia and neutralization reaction occurs
About 20 minutes, slurry was sent into pelletizer by the slurry obtained after reaction, was added in pelletizer after mixing by magnesium powder, calcium powder,
Pelletizer is granulated to form material；
H, by material that step G is formed be 110 DEG C in temperature at be dried after, through cooling, screening, obtain humic acid complex fertilizer.
In above-mentioned steps F, by weight, the mixed acid slurry includes 280 parts of the concentrated sulfuric acid, 100 parts of potassium chloride, phosphoric acid
80 parts, 160 parts of humic acid, 15 parts of ammonium chloride；In step G, by weight, the magnesium powder of addition is 25 parts, and calcium powder is 25 parts.
Claims (10)
1. the technique that a kind of ardealite and red mud prepare aluminium coproduction humic acid complex fertilizer, which is characterized in that include the following steps：
A, ardealite, red mud, additive and modifying agent are mixed and is ground and raw material are made, be sent into roasting in kiln, clinker is made；
B, clinker made from step A is dissolved out, and is separated by solid-liquid separation；
C, CO is added into step B isolated solution2It is no longer generated to white precipitate, it is clear after then filtering out white precipitate
Drying and calcination are washed, aluminium oxide is obtained；
D, by step B isolated residue through flotation, sulfide is separated to obtain；
E, the step D sulfide isolated is placed under the oxygen-enriched environment of 30-50%, 3-5h is roasted at 800-1200 DEG C, roasted
The flue gas of generation is absorbed using the concentrated sulfuric acid after vanadic anhydride catalysis reaction, dilutes to obtain the concentrated sulfuric acid；
F, the concentrated sulfuric acid that step E is prepared is added in conversion reaction slot, preheats to the concentrated sulfuric acid in conversion reaction slot,
After the completion of preheating, humic acid, potassium chloride and ammonium chloride are even added to conversion reaction slot, phosphoric acid is then added, stirs evenly
Form mixed acid slurry；
G, mixed acid slurry made from step F is transferred in neutralization reactor, then passes to excessive ammonia and neutralization reaction occurs
About 10-20 minutes, slurry was sent into pelletizer by the slurry obtained after reaction, is added in pelletizer and is mixed by magnesium powder, calcium powder
Afterwards, pelletizer is granulated to form material；
H, after the dry materials for forming step G, through cooling, screening, humic acid complex fertilizer is obtained.
2. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
In step A, the red mud is the red mud that alumina producing Bayer process generates；The additive is sodium carbonate or caustic soda；It is described
Modifying agent is anthracite, carbon or gangue.
3. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
In step A, in the raw material, ardealite and Bayer red mud are according to 1:The ratio of 0.8-2 weight ratio mixes, and additive adds ratio
Example is by contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, the mixed proportion of modifying agent are raw material gross weight
The 10-25% of amount.
4. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
In step A, the kiln is industrial rotary kiln, Industry Tunnel Kiln or industrial shaft kiln.
5. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
It is the calcining time 1-2h at 1000-1350 DEG C of temperature in step A.
6. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
In step B, dissolved out after clinker elder generation water mill；It is 4-6 that liquid when dissolution, which consolidates volume ratio,:1.
7. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
In step C, calcination is the calcination time 2-5h at 800-1200 DEG C of temperature.
8. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
In step F, by weight, the mixed acid slurry includes concentrated sulfuric acid 250-300 parts, 80-120 parts of potassium chloride, phosphoric acid 50-80
Part, 120-160 parts of humic acid, 10-15 parts of ammonium chloride；In step G, by weight, the magnesium powder of addition is 20-25 parts, calcium powder
It is 20-25 parts.
9. the technique that ardealite according to claim 1 and red mud prepare aluminium coproduction humic acid complex fertilizer, it is characterised in that：
In step F, the temperature of the concentrated sulfuric acid is 80-90 DEG C in conversion reaction slot after preheating.
10. ardealite according to claim 1 and red mud prepare the technique of aluminium coproduction humic acid complex fertilizer, feature exists
In：In step H, the drying temperature of the material is 100-120 DEG C.
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