CN1330599C - Method for producing sulfuric acid associated with high Belite cement through anhydrite - Google Patents
Method for producing sulfuric acid associated with high Belite cement through anhydrite Download PDFInfo
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- CN1330599C CN1330599C CNB200510031351XA CN200510031351A CN1330599C CN 1330599 C CN1330599 C CN 1330599C CN B200510031351X A CNB200510031351X A CN B200510031351XA CN 200510031351 A CN200510031351 A CN 200510031351A CN 1330599 C CN1330599 C CN 1330599C
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Abstract
The present invention relates to a method for producing sulfuric acid associated with high Belite cement by anhydrite. Mineral compositions of a fired clinker comprises: 25 to 45% of C3S, 35 to 55% of C2S, 5 to 8% of C3A and 7 to 15% of C4AF. In addition, the content of SO3 is smaller than 2.5%, the content of CaS is smaller than 1.0% and the content of fCaO is smaller than 1.0%. When fired, CaSO4 is decomposed to generate SO2 whose concentration is 9 to 11%. Through acid washing, purification, double rotation and double suction, sulfuric acid of 93 % or 98% is prepared. The clinker is added with pulverized coal ash and dihydrate gypsum to produce low heat cement. The present invention is a new technology which has the advantages of wide ranges of raw materials, low price, simple production technology and easy production and operation. The sulfuric acid produced by the method for producing sulfuric acid associated with high Belite cement by anhydrite can reach the quality requirements of special type acid, and not only can be used for chemical fertilizer industry, but also can be used for food or medicine industry. Cement clinkers have the advantages of high Belite content and low hydration heat, which can be used for producing low-heat portland cement to realize the goals of low temperature calcination and energy saving, and added values of products can also be greatly enhanced.
Description
Technical field: patent of the present invention relates to a kind of method of utilizing anhydrite to produce producing sulfuric acid and jointly high belite cement of chemical technology field.
Background technology:
The invention relates to anhydrite and make sulfuric acid, produce the method for low-heat high belite cement simultaneously.Be to the improvement of existing gypsum system sulfuric acid method, be different from " a kind of by gypsum production vitriolic method " and " a kind of cement clinker and preparation technology thereof " fully, two kinds of products are all produced on a production line.
The present invention is for solving the shortage of China's sulphur resource, breaks away to rely on imported sulphur to produce sulfuric acid, and the price increase of containment sulfuric acid provides reliable production method, and the cement of the low hydration heat that simultaneously can also the production construction work needs improves concrete weather resistance.The abundant anhydrite of present application few resource is fully used.
The gypsum method was produced phosphogypsum or the natural dihydrate gypsum that sulfuric acid adopts in the past, all to pass through pre-treatment, they are dried to semi-hydrated gypsum (containing crystal water 4～6%) or dead burning becomes dehydrated gyp-, the former will consume 3000～3800kj/kg heat, and latter's thermal losses is bigger＞5000kj/kg.The construction cost of device is big, the production cost height, and production environment pollutes easily.Its production method has strict restriction to the composition of phosphogypsum, is difficult to reach requirement when the grade of Rock Phosphate (72Min BPL) is hanged down, so CaSO
4Rate of decomposition is low, the SO in the kiln gas
2Concentration is little, and vitriolic output can not get guaranteeing, and the undecomposed CaSO of a large amount of residues is arranged in the cement clinker
4, the grog label is defective.Even also can only produce ordinary portland cement clinker when the quality of gypsum reaches requirement.Also there is defective in sulfuric acid production process, and transformation efficiency and specific absorption are low, SO in the tail gas
2Concentration over-standard causes the pollution to environment.
Summary of the invention:
The objective of the invention is to overcome the defective of prior art, invent a kind of method of producing producing sulfuric acid and jointly high belite cement with anhydrite.That this invention is that a raw material is drawn materials is extensive, cheap, production technique simple, be easy to the novel process of production operation.The sulfuric acid of producing with method of the present invention can reach extraordinary sour specification of quality, not only can use in chemical fertilizer industry, also can be used for food or pharmaceutical industries.The high hydration heat of the special content of cement clinker Baily is low, can produce low-heat portland cement, and production method realizes the low temperature calcination save energy, significantly improves value-added content of product.
The present invention is realized by following embodiment:
1. natural lumpy anhydrite is crushed to＜25mm, the definite proportioning of specification of quality with coke and other subsidiary material are pressed sulfuric acid and cement after the automatic blending scale metering of machine control, feeds the raw mill grinding as calculated, and grinding becomes the raw material powder.The proportioning of main raw material is: (by mass percentage) anhydrite 78～88%
River sand 6～10%
Coke end 6～8%
Adulterant 0～5%.
2. the raw material fineness is controlled at 0.08mm and tails over 20～25%.The raw material rate value of preparation is:
Carbon and sulphur trioxide mole ratio C/SO
30.58～0.75
Lime saturation factor KH 0.90～1.08
Silica modulus SM2.20～3.00
Aluminium-oxygen modulus IM2.00～3.00
SO
3 ≥42％
3. the raw material that prepare are sent into calcining in the rotary kiln, and the grog firing temperature is 1300～1400 ℃, and the kiln internal control is made as weak oxide atmosphere when firing, the excess air coefficient of coal dust firing＜1.05, primary air flow＜15%, secondary air flow＞90%.Clinker mineral composition that burns till and rate value are at following scope: C
3S 25～45% C
2S 35～55%
C
3A 5～8％ C
4AF 7～15％
SO
3 ＜2.5％ CaS ＜1.0％
fCaOmm mm＜1.0％。
KH 0.75～0.82
SM 2.5～4.0
IM 1.3～2.1
Physicals through the check cement clinker is as follows:
| Numbering | Clinker mineral is formed % | # fineness % | Time of coagulation | Ultimate compression strength Mpa | Folding strength Mpa | ||||||||
| C 3S | C 2S | C 3A | C 4AF | Initial set | Final set | 3d | 7d | 28d | 3d | 7d | 28d | ||
| 1 | 33 | 36 | 8 | 7 | 7 | 2:20 | 5:50 | 27.8 | 43.5 | 66.7 | 5.8 | 6.7 | 9.8 |
| 2 | 20 | 47 | 5 | 7 | 8 | 2:46 | 9:05 | 18.2 | 36.6 | 55.6 | 3.1 | 4.6 | 7.5 |
| 3 | 28 | 42 | 6 | 11 | 7 | 1:30 | 5:45 | 17.4 | 30.6 | 60.6 | 3.9 | 5.6 | 8.0 |
| 4 | 27 | 41 | 5 | 7 | 7 | 1:33 | 6:43 | 19.4 | 32.3 | 58.2 | 3.8 | 6.2 | 7.6 |
# (0.08mm) tails over %
4. CaSO in the grog sintering procedure
4Under the effect of reductive agent coke, carry out following reaction:
Because formulating of recipe is reasonable, the rotary kiln thermal technology operating parameters of formulation is scientific and reasonable, can prevent the generation of side reaction, CaSO
4Rate of decomposition reach ≈ 96%, CaO that decomposites and SiO
2, Fe
2O
3, Al
2O
3Water generation reaction mud grog, and essential mineral is C
2S, firing temperature are at 1300～1400 ℃, so hear rate is low, and the exhausted air quantity of generation is little, the SO in the kiln gas
2Concentration reaches 9～11%.600 ℃ of kiln discharge gas temperature ≈ reclaim heat through waste heat boiler, and the by-product middle pressure steam is again through dust precipitator dedusting dust content＜10g/Nm
3Temperature＜350 ℃ as producing the vitriolic raw material, enter sulfuric acid apparatus.
5. the gas washing in SA production initiative adopts acid-scrubbing cleaning, double conversion and double absorption technology
Kiln gas enters the wet purification system, wet purification adopt tower, bubble,, electric acid-scrubbing cleaning flow process, kiln gas passes through washing tower (void tower), foam column, inter cooler, electrostatic precipitator successively, makes the further dedusting cooling of kiln gas.Enter drying tower after the demist and carry out drying, drying contains SO after foam-blocker removes the disacidify foam
2＞6%, oxygen sulphur is than (O
2/ SO
2) be 0.927 gas by special blower fan force feed, gas is heated to 410 ℃, enters convertor by the convertor top.Convertor is four sections twice convertors.Once heating system utilizes the reaction heat of the 3rd section and first section catalyst layer.SO
2Through the reaction of first, second and third section catalyst layer, transformation efficiency reaches about 94% for the first time in convertor, and reforming gas enters first absorption tower after heat exchange.After absorbing sulphur trioxide for the first time, gas passes through heat exchange again, is heated to 410 ℃ once more, enters the 4th section catalyst layer of convertor.The system of (being secondary) heating this time utilizes the reaction heat of the 4th section and second section catalyst layer.After the 4th section catalyst layer carried out transforming the second time, final transformation efficiency reached 99.5%.Reforming gas enters second absorption tower after heat exchange, carry out absorbing the second time.Sulphur trioxide is become the finished acid of 92.5% or 98.5% concentration by 98% sulfuric acid absorption.Specific absorption is generally more than 99.95%.
Product acid by analysis except that colourity other every indexs all reached " industrial sulphuric acid " (GB534-89) quality index of premium grads.
The result is as follows in the finished acid total analysis:
| Index name | Unit | Finished acid | The industrial sulphuric acid national standard | ||
| Acceptable end product | Premium grads | Extraordinary acid | |||
| Sulfuric acid (H 2SO 4) content | ％ | 98.88 | ≥98.0 | ≥98.0 | ≥98.0 |
| Ash content (spoon burns residue) | ％ | 0.018 | ≤0.03 | ≤0.03 | ≤0.02 |
| Iron (Fe) content | ％ | 0.0035 | ≤0.010 | ≤0.010 | ≤0.005 |
| (As) content | ％ | 1.7×10 -5 | ≤0.005 | ≤0.0001 | ≤8×10 -5 |
| Plumbous (pb) content | ％ | 1.9×10 -5 | -- | ≤0.01 | ≤0.001 |
| Amount of nitrogen oxides (in N) | ％ | 0.028 | -- | --- | ≤0.0001 |
| Potassium permanganate reducing substance content | ％ | 0.042 | -- | --- | ---- |
| Sulfurous gas so 2Content | ％ | 0.0026 | --- | --- | ≤0.01 |
| Transparency | Mm | 65 | ≥50 | ≥50 | ≥160 |
| Colourity | ml | ≈2.5 | ≤2.0 | ≤2.0 | ≤1.0 |
Description of drawings:
Accompanying drawing is produced the method process flow diagram of producing sulfuric acid and jointly high belite cement for the present invention utilizes anhydrite.
Embodiment describes in detail:
1. feature of the present invention is that to adopt the cheap anhydrite of aboundresources be that the gypsum reserves of main raw material China are very abundant, explored reserves have 1,000 hundred million tons approximately, 70% is anhydrite (main component is an anhydrous calciumsulphate), 23 provinces, cities and autonomous regions mineral products are arranged all, 1,000,000,000 tons of proven reserve has ten what provinces, cities and autonomous regions.The good CaSO of the grade of ore
4＞85%, do not contain free-water, crystal water＜2.0%, MgO content is higher in the ore of indivedual ore deposits, requires the＜2.5%, can reach.Other trace elements are to CaSO
4Decomposition and cement clinker burn till all do not have the influence.
The field conditions of ore is better, general depth of burial-200～-300m, (the Northwest is exploitation on the ground), productive expense is low, and comprising transport charge only has about 40 yuan/t.
Because the uncomfortable cooperation gelling material of the performance of anhydrite, can produce various plasterings such as Thistle board, gypsum block etc. with dihydrate gypsum, be used as retardant at cement industry, and anhydrite is not almost used, the owner of many industries is just seeking the approach used, so the present invention will be the development widening road of China's gypsum industry and sulfuric acid industry.
2. two of feature of the present invention be the prescription of design can satisfy produce sulfuric acid again can the coproduction cement clinker
If contain P in the raw material of preparation
2O
5, it and CaO generate eutectic when grog burns till, and CaO is by useless consumption, and the Calucium Silicate powder growing amount reduces, and influences cement intensity.CaSO
4Decomposition temperature is at 900～1200 ℃ under the reductive action of carbon, and traditional production technique is to adopt the prescription of the high silica modulus of high lime saturation ratio (KH) (SM), and purpose is to reduce fluxing mineral C
4AF content improves C
3The content of A when especially containing CaF in raw material, because it plays mineralization, has reduced the temperature that liquid phase forms, and influences CaSO
4Decomposition, but the C of this grog
4The little C of AF content
3A content is big, though that early strength increases is also little, hydration heat is big because the content of Calucium Silicate powder is few, and the present invention has avoided the influence of these objectionable constituent.
Compare with produce high belite cement with Wingdale, also need add gypsum and other composition during its preparation raw material, to stablize β C
2S generates and activation, and main raw material of the present invention is an anhydrite, CaSO
4The remaining a spot of SO of decomposition meeting
3, also having played above-mentioned effect, process procedure is simpler and more direct.
The prescription that the present invention adopts is based on by CaSO
4Decompose the amount of the CaO of back generation and determine lime saturation ratio (KH), and improve the gypsum consumption to greatest extent, produce high SO to reach
2The kiln gas of concentration is for making CaSO
4Fully decompose, avoiding low flux mineral to occur liquid phase too early influences CaSO
4Decompose, to C
4AF content and C
3The content of A has been done rational selection, owing to there are not objectionable constituent not play the influence of the composition of mineralization, therefore prescription of the present invention can satisfy and produces the cement clinker that sulfuric acid again can coproduction contains the Baily extra-high-speed.
3. significantly energy-saving and cost-reducing based on the invention described above, can produce high SO
2The kiln gas of concentration need not dehydrate in raw materials pretreatment, only get final product through crushing and grinding, compare with the phosphogypsum of 16～18% crystal water with the free-water that contains 28%, raw material per ton can be saved 0.18～0.22t coal, and the power consumption of crushing and grinding power consumption and drying process is suitable.
Aspect cement clinker burns till, because the raw material consumption of sulfuric acid per ton or cement clinker is reduced to 1.75～1.85t by 2.0～2.1t, do not contain crystal water in the gypsum, reduced the consumption of the dehydration fever of crystal water, the formation heat of grog is by 3225KJ/Kg, be reduced to 2980 KJ/Kg, owing to reduced to C in the grog
3Therefore the requirement of the content of S, grog firing temperature are 1300～1400 ℃, burn till hear rate 6900～7500KJ/Kg and (be generally 8000～8500KJ/Kg), so the exhausted air quantity that coal burning produces reduce, in addition CaSO
4Abundant decomposition make SO in the kiln gas
2Concentration improves, and reaches for 9～11% (the butt volume ratio contains the kiln tail and leaks out), for gas washing in SA production has been created favourable condition.
4. three of feature of the present invention is in the technical employing double conversion and double absorption technology of having initiated of gypsum relieving haperacidity
The application of double conversion and double absorption technology is the once leap of sulfuric acid industry technology, by increasing the intermediate absorption process, and under the effect of catalyzer, chemical reaction
Balance is to generating SO
3Direction move, thereby greatly improve SO
2Total conversion rate, total conversion rate from one change one inhale about 95% bring up to more than 99%.This Technology has been widely used in sulphur, sulfurous iron ore and the metallurgical off-gas acid-making industry, and gypsum relieving haperacidity adopts double conversion and double absorption technology that the report of application is not arranged as yet.This mainly is because due to the two big characteristics of phosphogypsum, dihydrate gypsum relieving haperacidity kiln gas: the one, and the SO of kiln gas
2Concentration is low, generally＜7%, is difficult to ensure the autothermal equilibrium of conversion system; The 2nd, the weak oxide atmosphere of gypsum calcination, oxygen sulphur ratio is O in the kiln gas
2/ SO
2Be worth lowly, be difficult to obtain 99.5% high conversion.One changes one inhales 95% transformation efficiency, makes SO in the discharge tail gas
2Concentration over-standard reclaims production sulfurous acid ammonia though be provided with ammonia process, does not also reach environmental requirement.At current strict control SO
2This technology is worthless under the situation of discharging.And double conversion and double absorption technology is owing to reach 99.5% high conversion, SO in the discharge tail gas
2Concentration fully can be up to standard.
The present invention (contains CaSO with the anhydrite that contains crystal water＜2%
4＞85%) makes raw material, by scientific and reasonable prescription and the advanced rotary kiln technology operating parameters of formulation, SO in the kiln gas
2Concentration reaches 9～11% (butts), thereby makes the into SO of convertor
2Concentration＞6% then can be realized self thermal equilibrium of gas washing in SA production.Oxygen sulphur compares O
2/ SO
2Value: once gas 1.0～1.1; Secondary gas 5.5～6.5, roughly the same with pyrite-based sulfuric acid production, so can reach 99.5% transformation efficiency, emptying end gas SO
2Concentration＜500ppm.
Adopt double conversion and double absorption technology in anhydrite relieving haperacidity, this is an important breakthrough to traditional gypsum (phosphogypsum, dihydrate gypsum) acid-making process, and it not only has good economic benefit, and very remarkable environmental benefit is more arranged.
The present invention has following outstanding feature in sum:
(1). main raw material(s)-anhydrite is drawn materials extensively cheap, has solved China's sulphur shortage of resources and has relied on imported sulphur to produce a vitriolic difficult problem.
(2), the production technique of the invention is compared with external dead burning technology with half water conservancy project skill, and technical process is simple and direct, and energy consumption reduces greatly.
(3), technical recipe can be produced the high belite Portland clinker, and has eliminated the influence of detrimental impurity, and quality product improves.The requirement of various industries with acid satisfied in the raising of vitriolic purity.
(4), environmental protection problem has obtained basic solution, and gas washing in SA production realizes double conversion and double absorption and Diluted Acid Washing enclosed purification, and all round process does not have obnoxious flavour and sewage discharge.
(5), has remarkable economic efficiency, contrast as following table with the material power consumption cost of sulphur and pyrite-based sulfuric acid production, by visible consuming cost with anhydrite system producing sulfuric acid and jointly cement clinker in the table is 37.9% of acid production with sulphur, it is 49.87% of pyrite-based sulfuric acid production, also near the expense of new dry process rotary kiln, the flyash of admixture 20～30% is produced low-heat portland cement to the consuming cost of cement clinker in grog, and manufacturing cost only is 156 yuan/ton.As seen economic benefit is very significant.
Sulphur, sulfurous iron ore and anhydrite relieving haperacidity jointly producing cement grog material and power consumption cost contrast table unit: unit/ton
| Sequence number | Title | Unit | Unit price unit | The sulphur norm quota of consumption | The sulphur iron norm quota of consumption | Remarks | Anhydrite relieving haperacidity jointly producing cement grog | Remarks | |||
| Quantity | The amount of money | Quantity | The amount of money | Quantity | The amount of money | ||||||
| 1 | Sulphur | T | 1200 | 0.331 | 397.2 | Byproduct steam 1t/t acid | |||||
| 2 | Sulfurous iron ore | T | 245 | 0.985 | 241.33 | Byproduct steam 0.8t/t acid | |||||
| 3 | Anhydrite | 1 | 40 | 1.55 | 62.0 | Raw material and fuel cost sulfuric acid and cement clinker were by 1: 1 pro rata distribution 210.6/2=105.3 | |||||
| 4 | River sand | T | 30 | 0.16 | 4.80 | ||||||
| 5 | Adulterant | T | 30 | 0.04 | 1.20 | ||||||
| 6 | Coke fines | T | 400 | 0.10 | 40.0 | ||||||
| 7 | Burn till and use coal | T | 380 | 0.27 | 102.6 | ||||||
| 8 | Electricity | Kwh | 0.50 | 70.0 | 35.0 | 120.0 | 60.00 | 120.0 | 60.0 | The sulfuric acid electricity consumption with share back grog electricity consumption sum | |
| 9 | Water | t | 1.50 | 1.25 | 1.87 | 16.0 | 24.00 | 2.78 | 4.14 | ||
| 10 | Catalyst | Kg | 20.0 | 0.10 | 2.00 | 0.10 | 2.00 | 0.07 | 1.40 | ||
| 11 | Lime | 100 | 0.06 | 6.00 | 0.005 | 0.50 | |||||
| 12 | Steam | t | 50 | 1.0 | -50.0 | 0.80 | -40.0 | 0.50 | -25.0 | Byproduct steam 0.5t/t acid | |
| 13 | |||||||||||
| 14 | Cost accounting | 386.04 | 293.33 | 146.34 | |||||||
Illustrate: 1. listed unit price is the recent market price, and 1040 yuan of/ton 2. anhydrite relieving haperacidity jointly producing cement grog output ratios of sulphur insurance and freight (CIF) are 1: 1,
3. the consuming cost of the material of grog and electric power is 123.3 yuan/ton
Claims (2)
1. method of utilizing anhydrite to produce producing sulfuric acid and jointly high belite cement is characterized in that:
(1) proportioning of anhydrite and coke fines and subsidiary material, determine that according to the specification of quality of producing sulfuric acid and cement clinker the proportioning of main raw material is:
Anhydrite 78～88%
Coke fines 6～8%
River sand 6～10%
Adulterant 0～5%
The composition of admixtion requires lime saturation factor KH 0.90～1.08
Silica modulus SM 2.20～3.00
Aluminium-oxygen modulus IM 2.00～3.00
Sulphur trioxide SO
3〉=42%
Carbon and sulphur trioxide mole ratio
C/SO
3 0.58～0.75；
(2) production method: the grog firing temperature is 1300～1400 ℃, the kiln internal control is made as weak oxide atmosphere, the excess air coefficient of coal dust firing＜1.05, primary air flow＜15%, secondary air flow＞90%, kiln gas reclaims heat through waste heat boiler, the by-product middle pressure steam, again through dust precipitator dedusting, dust content＜10g/Nm
3, temperature＜350 ℃ as producing the vitriolic raw material, enter sulfuric acid apparatus;
(3) make and contain sulfur dioxide flue gas concentration 9～11%, through acid-scrubbing cleaning, 92.5% or 98.5% sulfuric acid is made in twice absorption of twice conversion;
(4) the special C of the cement clinker Baily of the present invention's production
2S content height, its mineral composition and rate value are:
C
3S 25～45％ C
2S 35～55％
C
3A 5～8％ C
4AF 7～15％
SO
3 ＜2.5％ CaS ＜1.0％
fCaO ＜1.0％
KH 0.75～0.82
SM 2.5～4.0
IM 1.3～2.1。
2. as the right 1 described method of utilizing gypsum to produce producing sulfuric acid and jointly high belite cement, it is characterized in that its calcium sulfate of anhydrite CaSO
4Content＞85%, crystal water content＜2.0%.
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| CN1330599C true CN1330599C (en) | 2007-08-08 |
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| CN102838090B (en) * | 2012-10-16 | 2015-10-21 | 刘立文 | A kind of calcium sulfate produces technique and the equipment of sulfuric acid and calcium oxide |
| CN103253637A (en) * | 2013-06-04 | 2013-08-21 | 刘立文 | Method for producing sulfuric acid and calcium oxide by utilizing gypsum |
| CN104860556B (en) * | 2014-02-24 | 2018-07-13 | 唐山北极熊建材有限公司 | Quick setting and rapid hardening belite sulphoaluminate cement clinker, application and its production technology |
| CN106277864B (en) * | 2016-08-26 | 2018-04-13 | 中国建筑材料科学研究总院 | Extra large work low-heat portland cement clinker aggregate and preparation method thereof |
| CA3065488A1 (en) * | 2017-05-29 | 2018-12-06 | Ravi Kant AHALAWAT | Method for manufacturing cement |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6695910B2 (en) * | 2001-10-24 | 2004-02-24 | Ciments Francais | Sulfoaluminous clinker without iron and without free lime, its process of preparation and its use in white binders |
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2005
- 2005-03-23 CN CNB200510031351XA patent/CN1330599C/en not_active Ceased
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6695910B2 (en) * | 2001-10-24 | 2004-02-24 | Ciments Francais | Sulfoaluminous clinker without iron and without free lime, its process of preparation and its use in white binders |
Non-Patent Citations (1)
| Title |
|---|
| 硬石豪制硫酸联产水泥工艺的研究与设想 谢富康，化工时报，第10卷第6期 1996 * |
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