CN106431031B - A method of utilizing ardealite sulphate aluminium cement co-producing sulfuric acid - Google Patents

A method of utilizing ardealite sulphate aluminium cement co-producing sulfuric acid Download PDF

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CN106431031B
CN106431031B CN201610842991.7A CN201610842991A CN106431031B CN 106431031 B CN106431031 B CN 106431031B CN 201610842991 A CN201610842991 A CN 201610842991A CN 106431031 B CN106431031 B CN 106431031B
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ardealite
sulphate aluminium
cement
aluminium cement
sulfuric acid
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CN106431031A (en
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李淑庆
胡兆平
刘阳
于南树
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KINGENTA NORSTERRA CHEMICAL Co Ltd
Kingenta Ecological Engineering Group Co Ltd
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KINGENTA NORSTERRA CHEMICAL Co Ltd
Kingenta Ecological Engineering Group Co Ltd
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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
    • C04B7/00—Hydraulic cements
    • C04B7/32—Aluminous cements
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The present invention relates to a kind of methods using ardealite sulphate aluminium cement co-producing sulfuric acid；Lime stone and the natural gypsum are replaced completely with ardealite, and after same bauxite, anthracite grinding homogenizing, at 1250~1300 DEG C, calcining prepares sulphate aluminium cement.The present invention can increase substantially ardealite utilization rate, and the SO 2 tail gas of high concentration can prepare sulfuric acid by absorption.Sulphoaluminate cement clinker setting rate prepared by the present invention is fast, and preceding later strength is high, and performance test shows that the mechanical strength of the sulphate aluminium cement prepared using the method for the present invention meets sulphate aluminium cement standard.

Description

A method of utilizing ardealite sulphate aluminium cement co-producing sulfuric acid
Technical field:
The invention belongs to the technical field of cement material, it is related to preparing sulphur using phosphorous chemical industry trade waste ardealite as raw material The method of aluminate cement.
Background technique:
It is also higher and higher to the technical requirements of special cement with the modernization of engineering technology.Including special engineering There is special requirement to the speed of rapid condensation and hardening and each phase hardness when construction, such as the connection construction of cement pipeline, The construction etc. of the Foundation Fieldbus field of Large-Scale Equipment.Although however using the continuous expansion with selling market, because product cost compared with It is high and be restricted, so that more users is unable to reach.On the other hand, as three big production of phosphate fertilizer states in the world it One, it is restricted by ardealite impurity index and application technology, it is difficult to realize large utilization, huge phosphate fertilizer industry leaves 300,000,000 Ton industrial by-product ardealite, about 70,000,000 tons of annual discharge amount, utilization is about 17,000,000 tons, and utilization rate is less than 30%, Bottleneck as phosphate & compound fertilizer industry sustainable development.How using by-product ardealite sulphate aluminium cement is prepared, had become One of the emphasis of domestic and international researcher research.
Chinese patent document CN1401604A discloses a kind of manufacture craft of quick hardening sulphoaluminate cement, this technique is with life Material proportion is dehydrated phosphogypsum 17-20%, lime stone 45-52%, alumina 31-35%, this technique successfully utilizes waste material phosphorus stone Cream can partially reduce the cost of sulphate aluminium cement, but ardealite in technique instead of the natural gypsum in raw-meal ingredient Usage amount only accounts for the 17-20% of raw-meal ingredient, it is also necessary to which effective use ardealite is not achieved in the lime stone of 45-52% Purpose, in addition the decomposition of ardealite can discharge sulfur dioxide in technique, it is improper conduct oneself well to comprehend cause environmental pollution.
Chinese patent document CN103304170A discloses a kind of method for producing sulphate aluminium cement, by lime stone, phosphorus Gypsum, low-grade bauxite and coke are configured to cement slurry by a certain percentage, calcine, forge at high temperature after grinding mixes By promoting ardealite decomposition as much as possible during burning, the calcium oxide for decomposing generation replaces part lime stone, sulfur dioxide Gas can be collected and prepare sulfuric acid, this processing compound is lime stone 30-60 parts, 25-55 parts of ardealite, low-grade bauxite 15-45 Part, the cost of cement can be suitably reduced successfully using waste material ardealite instead of the natural gypsum.But ardealite does not take completely Still there is up to 30-60 parts of lime stone for lime stone, in raw-meal ingredient, the carbon dioxide that decomposition of limestone generates can be significantly dilute The concentration of sulfur dioxide is released, so that the cost of preparing sulfuric acid by using sulfur dioxide and difficulty increase.
Chinese patent document CN101481222A discloses a kind of ardealite Partial Conversion sulphate aluminium cement by-product sulphur The method of sour ammonium, key step include ardealite conversion, conversion product be separated by filtration, the neutralization of conversion fluid, ammonium sulfate it is dense Contracting crystallizing and drying, the drying of filter cake and aluminium vanadine, raw meal proportioning and homogenizing, clinker burning and cooling, clinker be quenched, grinding and Change, calcine vent gas treatment etc..By to being not required to pretreated ardealite Partial Conversion and obtain meeting sulphate aluminium cement produce institute The mixture for needing dispensing requirements is not required to again additional lime stone, has expanded the application range of ardealite.But this technique needs first by phosphorus stone Cream is converted into calcium carbonate and then carries out raw-meal ingredient and calcining again, and required equipment and process flow are all complex, production cost It is high.
Summary of the invention:
The problem of for the preparation of current sulphate aluminium cement, the present invention, which provides one kind ardealite can be fully utilized, to be taken For the natural gypsum and lime stone, and can be by the aluminium sulfate production method of recycling tail gas co-producing sulfuric acid, and process route is simple, Production cost is low, has good economy and environmental benefit.
Summary of the invention
The present invention is using ardealite, bauxite, anthracite as raw material, and high-temperature calcination is made ripe after ingredient, grinding, homogenizing Material, gained clinker can add the natural gypsum or lime stone prepares different types of sulphate aluminium cement, can not also additional natural stone Cream directly obtains sulphate aluminium cement.
Detailed description of the invention
Technical scheme is as follows:
A method of using ardealite sulphate aluminium cement co-producing sulfuric acid, comprise the following steps that
A. the preparation of cement slurry:
Carry out ingredient according to following mass parts: ardealite is 65-80 parts, 20-32 parts of bauxite, 3-5 parts of anthracite；It will be each Component mixes, and obtains cement slurry after grinding homogenizing；
B. the preparation of clinker:
Cement slurry prepared by step a is calcined 30-40 minutes in 1250~1300 DEG C, obtains clinker, calcined The SO 2 tail gas generated in journey is sent into sulfuric acid preparation system after collecting, and prepares sulfuric acid；
C. the preparation of cement:
Clinker made from step b is regrind to get sulphate aluminium cement is arrived.
, according to the invention it is preferred to, fineness is 120-180 mesh after each component grinding in step a；
Preferably, Al in the bauxite2O3Mass fraction is 50-60%, further preferred 55%；
Preferably, the ardealite is half water ardealite.
, according to the invention it is preferred to, carry out ingredient according to following mass parts in step a: ardealite is 70-75 parts, aluminium alum It is 18-25 parts native, 3-4 parts of anthracite.
, according to the invention it is preferred to, calcining described in step b carries out in rotary kiln, shaft kiln or tunnel oven, further It is preferred that being carried out in rotary kiln.The process that SO 2 tail gas collection is prepared to sulfuric acid, by the prior art.
, according to the invention it is preferred to, it is 300~400m that clinker, which is ground to specific surface area, in step c2/ kg, further It is preferred that 350m2/kg。
According to the present invention, the clinker that step b is obtained can add the natural gypsum as requested, and different types of sulphur is made Aluminate cement.
The amount of allocating of the natural gypsum calculates as follows:
CG=0.13*M*AC/S
CG--- the mass fraction (ratio of the natural gypsum and clinker) of natural gypsum incorporation, if clinker is 1；
AC--- in clinkerMass fraction；
S --- SO in the natural gypsum3Mass fraction；
M --- natural gypsum coefficient, natural gypsum dosage is different in different sulphate aluminium cements, and M value is different, M value Range is between 0-4.
M value is as follows in different sulphate aluminium cements:
Early strong, high-strength sulphate aluminium cement M value: 0-1；Intumescent sulphate aluminium cement M value: 1-2；Seif-citing rate type Sulphate aluminium cement M value: 2-4；Low alkalinity type sulphate aluminium cement M value: 2.5-3.0.
The present invention substitutes the natural gypsum and lime stone by adjusting cement raw mix proportioning mode, with ardealite completely, passes through Calcium sulfate in ardealite is reduced into sulfur dioxide and calcium oxide by anthracite, sulfur dioxide through oxidative absorption Sulphuric acid product, Sulphate aluminium cement is made through high temperature sintering in calcium oxide, bauxite and the unreduced calcium sulfate of production.
Cement slurry of the present invention in high-temperature burning process, decompose under anthracite effect by most of ardealite, point Solution rate is 70-85%, wherein the calcium sulfate for participating in decomposition reaction, which decomposes generation calcium oxide, to be decomposed and generate all instead of lime stone Concentration of SO 2 gas be 7-9%, can be used for producing sulfuric acid；Remaining undecomposed ardealite is after high-temperature calcination, conversion For high temperature gypsum, the outer natural gypsum added needed for alternative clinker product.
Main chemical reactions of the present invention are as follows:
300 DEG C of raw material dehydrations of room temperature-, including mechanical water and the crystallization water；
300 DEG C -450 DEG C ardealites are changed into anhydrous gypsum；
450 DEG C -600 DEG C bauxites are decomposed to form α-Al2O3, there is α-SiO in material2And Fe2O3；
600℃—900℃ α-Al2O3、α-SiO2And Fe2O3It continues growing；
900 DEG C -1150 DEG C ardealite reduction generate CaO and SO2, 3CaO3Al2O3·CaSO4And 2CaOAl2O3· SiO2It is formed and is gradually accumulated；The absorptivity of free calcium oxide is up to 1/2, α-Al2O3、α-SiO2And CaSO4Content be reduced rapidly；
1150℃—1250℃ 3CaO·3Al2O3·CaSO4Continue to increase, free CaO and 2CaOAl2O3·SiO2Disappear It loses, 4CaO2SiOCaSO occurs at 1250 DEG C4Mineral, the mineral composition of sample is mainly 3CaO3Al at this time2O3· CaSO4、4CaO·2SiO·CaSO4、β-2CaO·SiO2, Free Ca SO4With a small amount of iron phase；
1250℃—1300℃ 4CaO·2SiO·CaSO4It disappears, resolves into α -2CaOSiO2With Free Ca SO4, this When clinker essential mineral 3CaO3Al2O3·CaSO4, 2CaOSiO2And calcium sulfate, there are also a small amount of iron phase, common aluminium sulfates Clinker is formed completely；
1300 DEG C -1400 DEG C clinkers are without significant change；
The solid slag that heretofore described ardealite generates when referring in phosphoric acid production with sulfuric acid treating phosphorite, it is different The ardealite that technique obtains is used equally for the present invention.
The present invention has the advantage that
1, compared to the method that other prepare sulphate aluminium cement using ardealite, ardealite can substitute stone completely in the present invention Lime stone and the natural gypsum carry out clinkersintering, greatly improve the utilization rate of ardealite, realize ardealite resource utilization, and Effectively reduce the cost of sulphate aluminium cement.
2, the decomposition reaction that anthracite promotes most of calcium sulfate in ardealite, undecomposed ardealite are added in raw material The sulphate component that a part is formed as calcium sulphoaluminate in cement clinker mineral, another part can be used to replace outside clinker The natural dihydrate gypsum component mixed, can directly produce sulphate aluminium cement.
3. due to not using lime stone in ingredient, so the concentration of SO 2 gas that decomposing ardealite generates is high, it can Meet requirement of the acid making system to sulfur dioxide concentration, efficiently use sulfur dioxide, avoids the pollution problem of sulfur dioxide.
4. the sulphoaluminate cement clinker that the present invention obtains can be applied to produce the differences such as fast hard, high-strength, expansion, low alkalinity The sulphate aluminium cement of type.
Specific embodiment:
The present invention is described in further detail With reference to embodiment, but not limited to this.
Ardealite is taken from big two water of Nuo Taier Chemical Co., Ltd., the half water law Wetting of Nintaus in following embodiment The semi-hydrated gypsum of phosphoric acid by-product, main component are shown in Table 1, and bauxite is derived from Guizhou, and main component is shown in Table 2.
Table 1: the main component and content of ardealite
Component CaO SO3 Fe2O3 Al2O3 SiO2
Content % 36.96 52.63 0.15 0.57 1.97
Table 2: the main composition and content of bauxite
Component CaO Fe2O3 SiO2 Al2O3 SO3
Content % 3.84 9.86 21.28 55.45 /
Embodiment 1:
According to following mass fraction progress ingredient: 65 parts of ardealite, 32 parts of bauxite, 3 parts of anthracite；Again by each component powder It is 120 mesh that mill, which is mixed to fineness, obtains cement slurry；The cement slurry prepared is placed in rotary kiln at 1300 DEG C and is calcined 30 minutes, clinker is obtained, the tail gas after calcining containing sulfur dioxide send sulfuric acid preparation system, prepares sulfuric acid；The cement of firing Clinker is regrind to 350m2After/Kg, sulphate aluminium cement product, the mechanical property of gained sulphate aluminium cement can be obtained It is shown in Table 3.
Embodiment 2:
According to following mass fraction progress ingredient: 68 parts of ardealite, 28 parts of bauxite, 4 parts of anthracite；Again by each component powder It is 150 mesh that mill, which is mixed to fineness, obtains cement slurry；The cement slurry prepared is placed in rotary kiln at 1300 DEG C and is calcined 40 minutes, clinker is obtained, the tail gas after calcining containing sulfur dioxide send sulfuric acid preparation system, prepares sulfuric acid；The cement of firing Clinker is regrind to 350m2After/Kg, sulphate aluminium cement product, the mechanical property of gained sulphate aluminium cement can be obtained It is shown in Table 3.
Embodiment 3:
According to following mass fraction progress ingredient: 73 parts of ardealite, 22 parts of bauxite, 5 parts of anthracite；Again by each component powder It is 180 mesh that mill, which is mixed to fineness, obtains cement slurry；The cement slurry prepared is placed in rotary kiln at 1300 DEG C and is calcined 30 minutes, clinker is obtained, the tail gas after calcining containing sulfur dioxide send sulfuric acid preparation system, prepares sulfuric acid；The cement of firing To 350m after clinker regrinding2Sulphate aluminium cement product, the mechanical property of gained sulphate aluminium cement can be obtained in/Kg It is shown in Table 3.
Embodiment 4:
According to following mass fraction progress ingredient: 80 parts of ardealite, 20 parts of bauxite, 5 parts of anthracite；Again by each component powder It is 180 mesh that mill, which is mixed to fineness, obtains cement slurry；The cement slurry prepared is placed in rotary kiln at 1250 DEG C and is calcined 40 minutes, clinker is obtained, the tail gas after calcining containing sulfur dioxide send sulfuric acid preparation system, prepares sulfuric acid；The cement of firing To 350m after clinker regrinding2Sulphate aluminium cement product, the mechanical property of gained sulphate aluminium cement can be obtained in/Kg It is shown in Table 3.
Embodiment 1-4 result:
The data from table 3 using the mechanical property of the sulphate aluminium cement of the method for the present invention sintering it is found that met The standard of sulphate aluminium cement in GB20472-2006.
Table 3: sulphate aluminium cement glue sand mechanical property

Claims (9)

1. a kind of method using ardealite sulphate aluminium cement co-producing sulfuric acid, comprises the following steps that
A. the preparation of cement slurry:
Carry out ingredient according to following mass parts: ardealite is 65-80 parts, 20-32 parts of bauxite, 3-5 parts of anthracite；By each component It mixes, obtains cement slurry after grinding homogenizing；
Al in the bauxite2O3Mass fraction is 50-60%；
B. the preparation of clinker:
Cement slurry prepared by step a is calcined 30-40 minutes in 1250-1300 DEG C, obtains clinker, in calcination process The SO 2 tail gas of generation is sent into sulfuric acid preparation system after collecting, and prepares sulfuric acid；
C. the preparation of cement:
Clinker made from step b is regrind to get sulphate aluminium cement is arrived.
2. the method according to claim 1 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that step Fineness is 120-180 mesh after each component grinding in rapid a.
3. the method according to claim 1 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that step Al in bauxite described in rapid a2O3Mass fraction is 55%.
4. the method according to claim 1 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that step Ardealite described in rapid a is half water ardealite.
5. the method according to claim 1 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that step Carry out ingredient according to following mass parts in rapid a: ardealite is 70-75 parts, 18-25 parts of bauxite, 3-4 parts of anthracite.
6. the method according to claim 1 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that step Calcining described in rapid b carries out in rotary kiln, shaft kiln or tunnel oven.
7. the method according to claim 1 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that step It is 300~400m that clinker, which is ground to specific surface area, in rapid c2/kg。
8. the method according to claim 1 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that step Different types of sulphate aluminium cement is made according to requiring amount of allocating to add the natural gypsum as follows in the clinker that rapid b is obtained；
The amount of allocating of the natural gypsum calculates as follows:
CG=0.13*M*AC/S
CG--- the mass fraction of natural gypsum incorporation, the ratio of the natural gypsum and clinker, if clinker is 1；
AC--- in clinkerMass fraction；
S --- SO in the natural gypsum3Mass fraction；
M --- natural gypsum coefficient, M value range is between 0-4.
9. the method according to claim 8 using ardealite sulphate aluminium cement co-producing sulfuric acid, which is characterized in that no It is as follows with M value in sulphate aluminium cement:
Early strong, high-strength sulphate aluminium cement M value: 0-1；Intumescent sulphate aluminium cement M value: 1-2；Seif-citing rate type sulphur aluminium Acid salt cement M value: 2-4；Low alkalinity type sulphate aluminium cement M value: 2.5-3.0.
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CN107056102B (en) * 2017-03-17 2020-01-24 山东卓联环保科技有限公司 System and method for producing sulphoaluminate cement and co-producing sulfur by utilizing desulfurized gypsum and aluminum ash
CN108485517A (en) * 2018-07-03 2018-09-04 贵州大学 A kind of technique of red mud and ardealite relieving haperacidity coproduction heat resistant powder coating
CN112358212A (en) * 2020-11-02 2021-02-12 荆州三迪建筑科技有限公司 Comprehensive utilization method of phosphogypsum
CN115010334A (en) * 2022-07-01 2022-09-06 武汉理工大学 Method for dealkalizing red mud by using phosphogypsum

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CN103304170B (en) * 2013-06-28 2014-08-20 重庆大学 Method for producing sulphate aluminum cement
CN105129744B (en) * 2015-07-21 2017-10-20 湖北湖大天沭新能源材料工业研究设计院有限公司 A kind of method that ardealite Sulphuric acid co-producing cement is thermally decomposed in advance

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