CN108545983A - A kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent - Google Patents
A kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent Download PDFInfo
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- CN108545983A CN108545983A CN201810711207.8A CN201810711207A CN108545983A CN 108545983 A CN108545983 A CN 108545983A CN 201810711207 A CN201810711207 A CN 201810711207A CN 108545983 A CN108545983 A CN 108545983A
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- iron
- red mud
- ardealite
- liquid
- accelerating agent
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Sludge (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of methods that ardealite and iron red mud carry iron coproduction liquid accelerating agent, include the following steps：1）Ardealite, iron red mud, additive and modifying agent are mixed and ground, raw material are made, is sent into roasting in kiln, clinker is made；2）By step 1）After clinker obtained grinding plus it is water-soluble go out, and be separated by solid-liquid separation, respectively liquid and residue；3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is roasted into obtain iron oxide；4）By step 2）Isolated liquid stands 12 days under the protection of nitrogen, then takes supernatant, is stirred evenly to get liquid accelerating agent after polyacrylic acid and ethylene glycol is added in clear liquid then up.The present invention has ardealite and iron red mud processing cost low, and added value is high, and sodium aluminate solution purity is high, and accelerator performance is good, feature at low cost.
Description
Technical field
The present invention relates to a kind of methods that ardealite and iron red mud carry iron coproduction liquid accelerating agent, belong to chemical metallurgy neck
Domain.
Background technology
Ardealite refer in phosphoric acid production with sulfuric acid treating phosphorite when the solid slag that generates, main component is 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 generally in powdery, appearance one
As be the colors such as greyish white, sallow, light green, contain：Organophosphor, sulphur fluoride compound venomous injurant, unit weight 0.733-0.88g/cm3,
Particle diameter is generally 5~15um, pH 1.5~3.0.About 20,000,000 tons of ardealite is discharged in China every year, adds up discharge capacity nearly hundred million
Ton.For utilization rate of the ardealite in terms of building materials less than 5%, a large amount of gypsum stack land occupations seriously pollute environment.
Iron red mud is one kind in red mud type, is gained the name because iron content is very high, iron content can reach
30% or so, it is the very high iron red mud of iron content such as the red mud in Guangxi and Yunnan Province.Meanwhile generally existing in red mud
A large amount of silicon and aluminium.The main component of Bayer iron red mud is：Sodium aluminosilicate：1.7Na2O·SiO2·Al2O3And bloodstone
Fe2O3；Basicity is very high：PH value 12 or so, and have certain radioactivity, directly result in utilization difficulty of the red mud in terms of building materials
It is very big.Currently, red mud comprehensive utilization ratio is less than 4%.Processing for red mud, domestic and international alumina producer is mostly by red mud in heap
Field is stacked, wet method of building a dam stockpiling.Red mud per ton annual stockpiling maintenance cost in China's is up to 35 yuan.From 1 day January in 2018, state
Family will also levy 25 yuan/ton of environmentally friendly tax, therefore, considerably increase the processing cost of red mud.
Liquid accelerating agent is one kind in cement hardener, in liquid.Usually matched for primary raw material by sodium aluminate solution
Make, still, sodium aluminate solution needed for now current liquid accelerating agent generally by aluminum oxide clinker add it is water-soluble go out after
Go out, and usually contain other impurities in these aluminum oxide clinkers, purity is not high, and accelerator performance obtained is poor；And if selected
The sodium aluminate of purification is configured to solution to prepare accelerator, then can greatly increase the manufacturing cost of accelerator.
It is now currently, seldom for the technology of the comprehensive utilization of ardealite and iron red mud, it is substantially focused on building materials and paving
The traditional fields such as road, and this has resulted in a large amount of high value ingredients in ardealite and red mud and has been wasted, added value is very low.And lead to
It crosses ardealite and iron red mud synthesis puies forward the technique of iron co-production liquid accelerating agent, have not been reported.
Goal of the invention
The object of the present invention is to provide a kind of methods that ardealite and iron red mud carry iron coproduction liquid accelerating agent.The present invention
Low with ardealite and iron red mud processing cost, added value is high, and sodium aluminate solution purity is high, and accelerator performance is good, at low cost
The characteristics of.
Technical scheme of the present invention
A kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent, includes the following steps：
1）Ardealite, iron red mud, additive and modifying agent are mixed and ground, raw material are made, is sent into roasting in kiln, be made ripe
Material；
2）By step 1）After clinker obtained grinding plus it is water-soluble go out, and be separated by solid-liquid separation, respectively liquid and residue；
3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is roasted into obtain iron oxide；
4）By step 2）Isolated liquid stands 1-2 days under the protection of nitrogen, then takes supernatant, then up clear liquid
It is stirred evenly to get liquid accelerating agent after middle addition polyacrylic acid and ethylene glycol.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, the step 1）Raw material in, phosphorus
Gypsum and iron red mud are according to 1：The ratio of 0.7-1.5 weight ratios mixes.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, the step 1）Raw material in, add
Add agent adding proportion by contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, the mixed proportion of modifying agent
For the 10-25% of raw material total weight.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, step 1）In, the high ferro is red
Mud is the red mud that alumina producing Bayer process generates, wherein Fe2O3Content be higher than 20%.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, step 1）In, the additive is
Sodium sulphate, sodium carbonate or caustic soda；The modifying agent is anthracite, carbon or gangue.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, step 1）In, the kiln is industry
Rotary kiln, Industry Tunnel Kiln or industrial shaft kiln；Calcination temperature is 1000-1350 DEG C, and roasting time is 0.5-2 hours.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, step 2）In, when the dissolution
It is 4-6 that liquid, which consolidates volume ratio,:1.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, step 3）In, the iron sulfide is
It is placed under the oxygen-enriched environment of 35-50%, is roasted 1-5 hours at 800-1000 DEG C.
The method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, step 4）In, the polyacrylic acid
Addition be supernatant gross mass 0.005-0.02%；The addition of the ethylene glycol is the 0.008- of supernatant gross mass
0.015%。
The addition of the method that ardealite above-mentioned and iron red mud carry iron coproduction liquid accelerating agent, the polyacrylic acid is
The 0.015% of supernatant gross mass；The addition of the ethylene glycol is the 0.01% of supernatant gross mass.
The present invention is by by ardealite and red mud reaction, recombination, making utility.The net reaction of principle is：
CaSO4（Ardealite）+ Na2O·SiO2·Al2O3（Iron 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（ 2CaO·SiO2↓）Afterwards,
Obtain soluble fabulous sodium aluminate（Na2O·Al2O3）.[sulphur] in reaction equation refers to adding 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.
Advantageous effect
1, two kinds of pollution waste residues of the ardealite of long-standing problem people all the time and iron red mud by being used as mainly by the present invention
Raw material is reacted, by being roasted at high temperature after adding additive and modifying agent, compared to tradition individually with ardealite
Or iron red mud is reacted as raw material to extract the technique of recycling valuable material, treatment process of the invention is more simple
Single, cost is more cheap.Meanwhile the stockpiling problem of ardealite and iron red mud is also further solved, increase ardealite
With the application of iron red mud, it is of great significance to alleviating environmental pollution.
2, the present invention using ardealite and iron red mud as raw material by being reacted, according to reaction principle of the present invention,
It can be obtained with silicate, sulfide after roasting（Predominantly iron sulfide）With the substance based on sodium aluminate, and by simply floating
Choosing and water dissolving-out process can detach the ingredients such as iron, sulphur and aluminium, successfully be extracted in ardealite and iron red mud
Valuable constituent, substantially increase the added value of ardealite and iron red mud.
3, the present invention handled by roasting technique, after clinker is by water-soluble leaching, the solute in solution based on sodium aluminate,
And other inorganic impurities are practically insoluble in water, while organic impurities is free of, therefore, the purity of sodium aluminate may be up in leachate
99% or more, have the advantages that purity is high.
4, the present invention can greatly improve speed by using high-purity sodium aluminate solution of dissolution as raw material, preparing accelerator
The performance of solidifying agent, meanwhile, reduce the production cost of accelerator.
Further to prove that beneficial effects of the present invention, inventor have done following experiment：
According to China building material industry standard JC477-2005《Gunite concrete accelerator》In requirement, to liquid of the present invention speed
The performance of solidifying agent is tested.
A, cement paste is prepared for detecting setting time.Accelerator made from 1-5 of the embodiment of the present invention is taken to prepare 5 respectively
Group cement paste, cement 1000g, water 350g, accelerator 80g in every group of cement paste；Then record 5 groups of cement pastes just
Solidifying time and final setting time.
B, mortar is prepared for detecting compression strength.Accelerator made from 1-5 of the embodiment of the present invention is taken to prepare 5 groups of sand respectively
It starches, cement 900g, water 450g, sandstone 1350g, accelerator 80g in every group of mortar；Then 1 day pressure resistance of 5 groups of mortars is recorded
Degree and 28 days compressive strength rates.It the results are shown in Table 1
By the test result of upper table as it can be seen that the liquid accelerating agent prepared using the present invention, performance indicator can reach professional standard
The requirement of JC477-2005.
Specific implementation mode
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 method that ardealite and iron red mud carry iron coproduction liquid accelerating agent, steps are as follows：
1）By ardealite and iron red mud according to 1：The ratio of 0.7 weight ratio mixes, and sodium sulphate and anthracite mixing is then added
And grind and raw material are made, sodium sulphate adding proportion presses contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 adds
Add, anthracitic mixed proportion is the 10% of raw material total weight；Raw material are sent into industrial rotary kiln and are roasted 2 hours at 1000 DEG C,
Clinker is made；
2）By step 1）It is 4 to add water to consolidate volume ratio by liquid after clinker grinding obtained:1 dissolution, and be separated by solid-liquid separation, respectively
Liquid and residue；
3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is placed in 35% oxygen-enriched ring
Under border, iron oxide is roasted 5 hours to obtain at 800 DEG C；
4）By step 2）Isolated liquid stands 1 day under the protection of nitrogen, then takes supernatant, then up in clear liquid
It is stirred evenly to get liquid accelerating agent after the polyacrylic acid of 0.005wt% and the ethylene glycol of 0.008wt% is added.
Embodiment 2：A kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent, steps are as follows：
1）By ardealite and iron red mud according to 1：The ratio of 0.9 weight ratio mixes, and sodium carbonate then is added and carbon is mixed and ground
Raw material are milled into, sodium carbonate adding proportion presses contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, carbon
Mixed proportion be raw material total weight 14%；Raw material are sent into Industry Tunnel Kiln and are roasted 1.6 hours at 1000 DEG C, are made ripe
Material；
2）By step 1）It is 4.5 to add water to consolidate volume ratio by liquid after clinker grinding obtained:1 dissolution, and be separated by solid-liquid separation, respectively
Obtain liquid and residue；
3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is placed in 38% oxygen-enriched ring
Under border, iron oxide is roasted 4 hours to obtain at 850 DEG C；
4）By step 2）Isolated liquid stands 1 day under the protection of nitrogen, then takes supernatant, then up in clear liquid
It is stirred evenly to get liquid accelerating agent after the polyacrylic acid of 0.009wt% and the ethylene glycol of 0.01wt% is added.
Embodiment 3：A kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent, steps are as follows：
1）By ardealite and iron red mud according to 1：The ratio of 1.1 weight ratios mixes, and caustic soda and gangue mixing is then added simultaneously
Raw material are made in grinding, and caustic soda adding proportion presses contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, coal
The mixed proportion of spoil is the 18% of raw material total weight；Raw material are sent into industrial rotary kiln, Industry Tunnel Kiln or industrial shaft kiln
1200 DEG C roast 1.2 hours, and clinker is made；
2）By step 1）It is 5 to add water to consolidate volume ratio by liquid after clinker grinding obtained:1 dissolution, and be separated by solid-liquid separation, respectively
Liquid and residue；
3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is placed in 42% oxygen-enriched ring
Under border, iron oxide is roasted 3 hours to obtain at 900 DEG C；
4）By step 2）Isolated liquid stands 2 days under the protection of nitrogen, then takes supernatant, then up in clear liquid
It is stirred evenly to get liquid accelerating agent after the polyacrylic acid of 0.012wt% and the ethylene glycol of 0.011wt% is added.
Embodiment 4：A kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent, steps are as follows：
1）By ardealite and iron red mud according to 1：The ratio of 1.3 weight ratios mixes, and sodium sulphate and gangue mixing is then added
And grind and raw material are made, sodium sulphate adding proportion presses contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 adds
Add, the mixed proportion of gangue is the 22% of raw material total weight；By at 1280 DEG C, roasting 0.8 is small in raw material feeding industrial rotary kiln
When, clinker is made；
2）By step 1）It is 5.5 to add water to consolidate volume ratio by liquid after clinker grinding obtained:1 dissolution, and be separated by solid-liquid separation, respectively
Obtain liquid and residue；
3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is placed in 46% oxygen-enriched ring
Under border, iron oxide is roasted 2 hours to obtain at 950 DEG C；
4）By step 2）Isolated liquid stands 1 day under the protection of nitrogen, then takes supernatant, then up in clear liquid
It is stirred evenly to get liquid accelerating agent after the polyacrylic acid of 0.015wt% and the ethylene glycol of 0.013wt% is added.
Embodiment 5：A kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent, steps are as follows：
1）By ardealite and iron red mud according to 1：The ratio of 1.5 weight ratios mixes, and caustic soda and anthracite mixing is then added simultaneously
Raw material are made in grinding, and caustic soda adding proportion presses contained Na in raw material2O and A12O3+Fe2O3The molecular proportion of summation is 1:1 addition, nothing
The mixed proportion of bituminous coal is the 25% of raw material total weight；Raw material are sent into industrial shaft kiln and are roasted 0.5 hour at 1350 DEG C, are made
Clinker；
2）By step 1）It is 6 to add water to consolidate volume ratio by liquid after clinker grinding obtained:1 dissolution, and be separated by solid-liquid separation, respectively
Liquid and residue；
3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is placed in 50% oxygen-enriched ring
Under border, iron oxide is roasted 1 hour to obtain at 1000 DEG C；
4）By step 2）Isolated liquid stands 2 days under the protection of nitrogen, then takes supernatant, then up in clear liquid
It is stirred evenly to get liquid accelerating agent after the polyacrylic acid of 0.02wt% and the ethylene glycol of 0.015wt% is added.
Claims (10)
1. a kind of method that ardealite and iron red mud carry iron coproduction liquid accelerating agent, which is characterized in that include the following steps：
1）Ardealite, iron red mud, additive and modifying agent are mixed and ground, raw material are made, is sent into roasting in kiln, be made ripe
Material；
2）By step 1）After clinker obtained grinding plus it is water-soluble go out, and be separated by solid-liquid separation, respectively liquid and residue；
3）To step 2）Flotation agent is added in isolated residue, floatingly selects iron sulfide, iron sulfide is roasted into obtain iron oxide；
4）By step 2）Isolated liquid stands 1-2 days under the protection of nitrogen, then takes supernatant, then up clear liquid
It is stirred evenly to get liquid accelerating agent after middle addition polyacrylic acid and ethylene glycol.
2. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
The step 1）Raw material in, ardealite and iron red mud are according to 1：The ratio of 0.7-1.5 weight ratios mixes.
3. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
The step 1）Raw material in, additive adding proportion press raw material in contained Na2O 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.
4. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
Step 1）In, the iron red mud is the red mud that alumina producing Bayer process generates, wherein Fe2O3Content be higher than 20%.
5. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
Step 1）In, the additive is sodium sulphate, sodium carbonate or caustic soda；The modifying agent is anthracite, carbon or gangue.
6. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
Step 1）In, the kiln is industrial rotary kiln, Industry Tunnel Kiln or industrial shaft kiln；Calcination temperature is 1000-1350 DEG C, when roasting
Between be 0.5-2 hours.
7. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
Step 2）In, it is 4-6 that the liquid when dissolution, which consolidates volume ratio,:1.
8. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
Step 3）In, the iron sulfide is placed under the oxygen-enriched environment of 35-50%, is roasted 1-5 hours at 800-1000 DEG C.
9. the method that ardealite according to claim 1 and iron red mud carry iron coproduction liquid accelerating agent, it is characterised in that：
Step 4）In, the addition of the polyacrylic acid is the 0.005-0.02% of supernatant gross mass；The addition of the ethylene glycol is
The 0.008-0.015% of supernatant gross mass.
10. the method that ardealite according to claim 9 and iron red mud carry iron coproduction liquid accelerating agent, feature exist
In：The addition of the polyacrylic acid is the 0.015% of supernatant gross mass；The addition of the ethylene glycol is the total matter of supernatant
The 0.01% of amount.
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Citations (3)
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|---|---|---|---|---|
| US20060144797A1 (en) * | 2002-07-04 | 2006-07-06 | Mcconchie David | Processes for the treatment of a waste material having a high ph and/or alkalinity |
| CN101434403A (en) * | 2008-12-16 | 2009-05-20 | 重庆市博赛矿业（集团）有限公司 | Novel method for processing calx sodica sintered alumina by dry method |
| CN102815881A (en) * | 2012-09-04 | 2012-12-12 | 焦作市新筑王材料科技有限公司 | Production method for preparing liquid setting accelerator from alumina clinker |
-
2018
- 2018-07-03 CN CN201810711207.8A patent/CN108545983A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060144797A1 (en) * | 2002-07-04 | 2006-07-06 | Mcconchie David | Processes for the treatment of a waste material having a high ph and/or alkalinity |
| CN101434403A (en) * | 2008-12-16 | 2009-05-20 | 重庆市博赛矿业（集团）有限公司 | Novel method for processing calx sodica sintered alumina by dry method |
| CN102815881A (en) * | 2012-09-04 | 2012-12-12 | 焦作市新筑王材料科技有限公司 | Production method for preparing liquid setting accelerator from alumina clinker |
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| Title |
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