CN101717837B - Chemical activation liquid of converter slag and application method thereof - Google Patents
Chemical activation liquid of converter slag and application method thereof Download PDFInfo
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- CN101717837B CN101717837B CN200910227881XA CN200910227881A CN101717837B CN 101717837 B CN101717837 B CN 101717837B CN 200910227881X A CN200910227881X A CN 200910227881XA CN 200910227881 A CN200910227881 A CN 200910227881A CN 101717837 B CN101717837 B CN 101717837B
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Abstract
The invention relates to a chemical activation liquid of converter slag and an application method thereof. The chemical activation liquid of the converter slag is an acidic aqueous solution prepared by water-soluble acidic substances except hydrochloric acid and hydrofluoric acid and has an acidic concentration of 0.1-1.0 mol/l measured by [H+]; and an osmotic agent accounting for 0.01-0.05% relative to the mass concentration of the solution is added to the acidic aqueous solution. The application method comprises the following steps of: fully stirring and uniformly mixing the converter slag and the chemical activation liquid after water quenching or hot stuffing and iron separation processing by adding 0.5-1.0m3 of the chemical activation liquid to each ton of dry converter slag; soaking and activating for 1-24 h while keeping a moist state; and baking or drying to obtain the converter slag processed by the chemical activation liquid. The converter slag processed by the chemical activation liquid is used as a composite material and ground into cement or used as a concrete additive, and has greatly improved activity than that of unprocessed converter slag. The invention can remarkably improve the early performance of the cement and the concrete.
Description
Technical field
The present invention relates to a kind of chemical activation liquid, relate in particular to a kind of chemical activation liquid that is used to handle bessemer furnace slag.The bessemer furnace slag of handling through chemical activation liquid of the present invention can be used for the mixing material that Grinding Process in Cement Plants is made cement in material of construction production and Application Areas, and as the raw material of the steel-making slag powder of commerical ready-mixed concrete stirring station.The invention still further relates to the using method of this bessemer furnace slag chemical activation liquid.
Background technology
Slag is the by product that produces in order to remove impurity in the steel in steelmaking process, and according to the difference of method for making steel, slag can be divided into bessemer furnace slag, electric furnace slag and open hearth slag.Converter steelmaking is the main method of modern steel-making, and bessemer furnace slag also is the main waste residue of China's Steel industry discharging.Bessemer furnace slag is based on crystalline mineral, and itself just has hydraulically active, and promptly independent just the mixing with water of bessemer furnace slag, dissolution phenomena and hydration reaction can take place, and just hydration reaction is slow.
Produce one ton of converter steel and will discharge 130～240 kilograms of slags.China is Iron and Steel Production and consumption big country, and the slag of annual discharging reaches tens million of tons, and the slag that accumulates for many years reaches several hundred million tons, often is attended by rather grand uniqueness " view "---a slag mountain near each large-scale iron and steel enterprise.The big steel slag of the annual discharging of iron and steel enterprise is not only stored up and the huge heavy economic burden of enterprise that becomes of maintenance cost because of constantly buying to plough, and the slag of storing up causes serious pollution also for the air and the underground water of periphery, therefore, the resource utilization exploitation of Multipurpose Utilization of Steel Slag or slag becomes the major issue of " contributes to contemporary times and brings benefits for future centuries ".
In American-European countries, Multipurpose Utilization of Steel Slag early, mainly at the blast furnace aspect that utilizes and build the road etc., U.S.'s utilization ratio reaches 98%, Germany also reaches 77%.The slag comprehensive utilization of China originates in the end of the fifties in last century, researched and developed out at present the method that multiple slag is handled and utilized, it is the most general with other metal wherein to reclaim iron and steel from slag, but after reclaiming 7～10% iron and steel, remaining waste residue still exists secondary emission and pollution problem.The application of slag in cement concrete because of have utilization big, utilize approach many, utilize thoroughly and characteristics such as non-secondary pollution, processing cost be relatively low, and become unique approach of China's slag comprehensive utilization, specifically approach has:
1) as the raw material of calcination of cement clinker.Utilize slag chemical ingredients and cement clinker more approaching, and the characteristics that iron level is higher, slag is substituted traditional sulfate slag (iron powder) and part Wingdale preparation raw material as ferro-controlling raw material, " crystal seed " and the mineralization of this raw material invar slag in calcining, can improve calciner grog output, reduce the clinker burning hear rate, reduce CO
2Discharging, but the utilization of slag is lower, generally only accounts for about 10% of raw material.Also have when slag is discharged to add " modification agent " that slag is formed is consistent with cement clinker, become cement clinker behind the quenching, but " modification agent " of this method adding kind is many, quantity is also very big, will certainly have influence on normally carrying out of process for making.
2) as the blended material or the concrete admixture of cement grinding.Utilize slag similar with mineral composition to the chemical constitution of cement clinker, and characteristics with certain hydraulically active, cement clinker, slag, slag or flyash, the common grinding of gypsum are become cement, China has also successively issued corresponding national standards GB13693-1992 (dross slag cement) and GB13590-2006 (slag silicate cement) twice for this reason, and has stipulated that the addition content of slag in the cement must be more than 30%.In addition, also can be with the independent grinding of slag to 400m
2The above fineness of/kg becomes a kind of mineral admixture, can be mixed into general cement or the alternative part cement form with mineral additive when concrete mixes and stirs with chamotte powder and add, corresponding national standards is GB/T20491-2006 (steel-making slag powder that is used for cement and concrete).Utilizing slag to produce building material mades such as steel slag brick, building block, ground and roadbed also all is the hydraulically active that has utilized slag, i.e. gelling characteristic institute deutero-related products or application.
With slag as the blended material of cement grinding or mineral admixture when fully utilizing slag significantly, can also reduce the cement clinker consumption that consumes the ample resources and the energy, reduce the Cement Production cost, can realize the combination of economic benefit and environmental benefit.
But slag is used two technology " bottleneck " that but exist as the blended material or the mineral admixture of cement grinding:
1, slag cools off insufficient in discharge process, and iron level is higher, compact structure, so though it is close with the cement clinker mineral composition, but because of its hydration rate slow, cause the cement and the concrete early stage performance of admixture slag to reduce: early strength is low, condense slowly, when particularly addition content is big this effect more obvious, this has just limited the extensive application of slag in cement and concrete.
2, f-CaO content height in the slag, compact structure, hydration reaction is slow, and volume easily causes soundness of cement bad when big.
At above-mentioned restraining factors, the technician has also carried out a large amount of research and has put into practice work.Taked following measure:
1) the physically activated or mechanical activation method of slag.Comprising process for treating steel slag such as water quenching, hot application method, hot vexed pot process, mainly is by increasing the steel-making slag powder fineness to improve cement and concrete early stage performance.These methods can both effectively reduce the lumpiness and the f-CaO content of slag, and slag is carried out repeatedly the broken and grinding fineness with the raising steel-making slag powder, also can slow down in the slag f-CaO to the influence of soundness of cement, also can improve simultaneously the hydration rate of steel-making slag powder, cement and concrete early stage performance are made moderate progress.But the raising of steel-making slag powder fineness can cause being multiplied of grinding pow consumption, the remarkable reduction of mill output.
2) the chemical activation method of slag.Cement and the concrete early stage performance of one or more chemical additives of admixture in the process of cement grinding to improve the admixture slag.This class additive is also referred to as exciting agent, and its principle is mainly derived from the extension that the fifties in last century, USSR (Union of Soviet Socialist Republics) was studied " alkali-slag cement ".The exciting agent of steel slag cement mainly contains several classes such as potassium sodium compound that contain potassium sodium compound (as sodium sulfate, soda ash, water glass etc.), halide (as fluorite, calcium chloride etc.), vitriol (as calcined gypsum or alunite), silicate or aluminate.These additives can improve the early stage performance of the cement concrete of admixture slag, and neither be too high for the higher regrind mill of cost.But the side effect to cement concrete is but very big, is not suitable for the requirement of modern cement concrete: the potassium sodium ion is introduced concrete can cause the concrete alkali, influence concrete weather resistance and work-ing life; Muriate also can aggravate the corrosion of inside concrete reinforcing bar, influences mechanical properties of concrete; The stimulation effect of calcined gypsum or alunite is less, and easily has influence on the adaptability of concrete to water reducer.
Summary of the invention
Purpose of the present invention is intended to overcome the defective that above-mentioned prior art exists; provide a kind of bessemer furnace slag early activation effect in cement and concrete utilization that can make remarkable; utilization ratio significantly improves; without any side effects, thus the bessemer furnace slag chemical activation liquid that other industrial discharge spent acid is protected environment also can be disposed simultaneously.
Another object of the present invention provides a kind of using method of simple bessemer furnace slag chemical activation liquid.
Bessemer furnace slag chemical activation liquid of the present invention is a kind of acidic aqueous solution that is mixed with by the water-soluble acid material beyond demineralizing acid and the hydrofluoric acid, acid concentration is counted 0.1～1.0mol/l with [H+] in the solution, and adds the permeate agent that accounts for solution quality concentration 0.01～0.05% in this acidic aqueous solution.
In the described acidic aqueous solution, the kind of acid can be selected a kind of in sulfuric acid, sulfurous acid, nitric acid, phosphoric acid, phosphoric acid dihydro amine, formic acid, the acetic acid etc., perhaps several arbitrary proportion mixing acid, also can use the industrial waste acid of objectionable constituent such as not containing Cl, F, K, Na, but must not use hydrochloric acid and hydrofluoric acid.
The permeate agent of described interpolation is negatively charged ion or nonionogenic tenside, and it mainly plays acceleration and promotes the effect of H+ to the steel slag particle internal penetration.Permeate agent can be selected naphthalenesulfonate formaldehyde condensation compound, condensate of melamine and formaldehyde, sulfamate formaldehyde condensation products, high-efficiency water-reducing agent of poly-carboxylic acid, alkylphenol polyoxyethylene etc.
Further, described chemical activation liquid can also comprise the hardening accelerator that accounts for solution quality concentration 0～0.5%.
Described hardening accelerator is organic amine compound, plays the effect of further refinforced cement and early age strength of concrete.Can have by hardening accelerator for you to choose: trolamine, tri-isopropanolamine, urea, quadrol, hexamethylenetetramine, azanol etc.
The concrete using method of bessemer furnace slag chemical activation liquid of the present invention is:
According to adding 0.5～1.0m in the dry bessemer furnace slag per ton
3The ratio of chemical activation liquid, with fully stirring through shrend or heat bessemer furnace slag and chemical activation liquid vexed and that select iron to handle in advance, mix, keeping soaking activation 1～24 hour under the moisture state, oven dry or dry after, promptly get the bessemer furnace slag of handling through chemical activation liquid.
Wherein, described hardening accelerator can add in the bessemer furnace slag with chemical activation liquid, also can adding separately after the chemical activation liquid activation that bessemer furnace slag mixes via acidic aqueous solution and permeate agent, before the grinding.If it is fashionable that hardening accelerator adds before the bessemer furnace slag grinding, add-on is 0.05～0.5% of a bessemer furnace slag weight.
The present invention is directed to the character and the characteristics of bessemer furnace slag itself, active aquation of bessemer furnace slag water hardening and sclerosis behavior are paid attention to respectively, will be through shrend or heat vexed and select bessemer furnace slag particle that iron handled with containing certain H
+The chemical activation liquid that the acidic aqueous solution of concentration and permeate agent mix soaks activation, make bessemer furnace slag accelerate dissolution and aquation under the effect of H+, also can impel clearing up of f-CaO in the slag, also can make the bessemer furnace slag particle become loose porous simultaneously, be easy to further aquation.Wherein, the permeate agent in the chemical activation liquid can play and quicken and promotion H
+Effect to the infiltration of bessemer furnace slag granule interior.The bessemer furnace slag of handling through such chemical activation is as blended material and the cement that grinding is made or use as concrete admixture, and the more untreated bessemer furnace slag of activity greatly improves, and cement and concrete early stage performance can significantly improve, its former because:
1, the admixture prehydration is handled the cement or the concrete of bessemer furnace slag, the extent of hydration of slag wants high a lot of when identical hydration age, a large amount of hydrated products that form provide prerequisite for the formation of hardening of cement body structure, the early strength of cement thereby be increased.
2, the hydrated product of the bessemer furnace slag formation of process prehydration processing itself can promote the further formation of hydrate in cement or the concrete system, can play " crystal seed " effect of hydration reaction.
3, owing to H in the prehydration process
+Strong dissolving and " erosion " effect to slag can make fine and close slag loose porous, are easy to further improve its hydration rate.
4, H in the prehydration process
+To the effect of clearing up of f-CaO, can weaken the influence of f-CaO to cement performance, help the raising of cement performance.
Further, make or during the steelslag powder as additive grinding, admixture can promote the hardening accelerator of cement or concrete hardening again at cement grinding, cement and concrete early stage performance will be better, and the utilization of bessemer furnace slag also can correspondingly further improve.
Bessemer furnace slag chemical activation liquid of the present invention has following beneficial effect:
1, the early activation effect is remarkable, and the utilization ratio of slag in cement and concrete increased substantially;
2, activation solution is without any side effects to cement and concrete, and workability of concrete energy, mechanical property and weather resistance are not had any disadvantageous effect;
3, the implementing process method is simple, and raw material sources are extensive, cheap, and certain grinding-aid effect is arranged, and is suitable for industrial applications;
4, can in the comprehensive utilization bessemer furnace slag, dispose the industrial waste acid of other industrial discharge.
Below by the bessemer furnace slag before and after the pre-treatment of chemical activation liquid is carried out sem analysis, further understand superiority through the pretreated bessemer furnace slag of chemical activation liquid:
From Fig. 1～Fig. 6 as can be seen, two obvious characteristics are arranged through pretreated bessemer furnace slag: the one, the surface of pre-treatment slag is obviously loose porous, and it is much fine and close that then want on untreated slag surface; The 2nd, the surface of pre-treatment slag has formed uneven needle-like and bar-shaped hydrated product, the generation of hydrated product is obviously inhomogeneous, may be that the preferential hydration forms on the higher point of some activation energy, hydrated product may be ettringite (AFt), some also has the characteristics of I type CSH gel, and this also is the proof of activated steel slag surface prehydration.
For analyzing the type of pre-treatment slag surface resultant, some points among the SEM figure of Fig. 5, Fig. 6 have been carried out the EPMA analysis, as Fig. 7～Fig. 8.Micro-area composition before and after the contrast activation contains minor N and S in the activated steel slag hydrated product, and in conjunction with the result of preceding surface analysis, hydrated product can preliminary judgement be ettringite (AFt).
Description of drawings
Fig. 1 is the SEM picture of slag of being untreated under magnification 2000X;
Fig. 2 is the SEM picture of pre-treatment slag under magnification 2000X;
Fig. 3 is the SEM picture of slag of being untreated under magnification 5000X;
Fig. 4 is the SEM picture of pre-treatment slag under magnification 5000X;
Fig. 5 is the SEM picture of slag of being untreated under magnification 10000X;
Fig. 6 is the SEM picture of pre-treatment slag under magnification 10000X;
Fig. 7 is the surface composition analysis chart of slag of being untreated;
Fig. 8 is the surface composition analysis chart of pre-treatment slag.
Embodiment
Embodiment 1
Preparation is used for the high reactivity steel-making slag powder of cement and concrete
1) will adopt slag two-stage crushing that hot vexed pot process handled to 8mm, select metal after, the bessemer furnace slag particle that obtains is less, water ratio is 4%, density is 3.31g/cm
3, its chemical ingredients sees Table 1:
Table 1 slag chemical composition analysis
Cement clinker adopts the dry-process rotory kiln cement mill to produce, and spherical for the black densification, granularity is bigger than normal, density 3.18g/cm
3, its chemical ingredients and essential mineral composition see Table 2 respectively, and gypsum is a natural dihydrate gypsum.
Table 2 cement clinker chemical composition analysis
2) add chemical activation liquid such as the table 3 that OP-10 permeate agent and trolamine hardening accelerator are mixed with different proportionings with dilute sulfuric acid aqueous solution, oven dry above-mentioned bessemer furnace slag activated 24 hours in the different chemical activation solution of table 3 after, the activation solution consumption is the dried slag of 850 ± 50ml/ kilogram, grinding to 410 ± 20m then
2/ kg.
The composition proportioning of the several chemical activation liquid of table 3
3) according to the standard of GB/T 20491-2006, be under 3: 7 the condition at the mass ratio of steel-making slag powder and 42.5 silicate cements, measure the strength of cement of above-mentioned admixture steel-making slag powder, calculate the activity index specific tenacity of 42.5 silicate cements (promptly with) in the different length of times, and with the steel-making slag powder (0 of activation treatment not
#) compare.As seen from Table 4, still can not satisfy the requirement of secondary steel-making slag powder among the GB/T 20491-2006 without the steel-making slag powder of activation treatment, but after present method activation treatment, activity index is far above the requirement of GB/T 20491-2006 one-level steel-making slag powder regulation, and seven days activity indexs even be 2 times of standard-required illustrate that this activation method has significant morning of strong promoter action to bessemer furnace slag.
The activation effect of the different proportioning activation solutions of table 4
The high reactivity steel-making slag powder of this activation method of process preparation can be used to prepare cement and use as concrete admixture, as 1～4
#Every index of sample has all reached the technical requirements of 42.5R class g cement.
In addition, other index also can satisfy the corresponding requirements of GB/T 20491-2006.
Table 5 is to replace the C that the different cement of measuring are designed and prepare with activated steel slag powder
30And C
60Concrete 3d intensity experiment result, the concrete 3d intensity under different grades and the different replacement amounts, the reinforced effects of activated steel slag powder all is better than non-activated steel-making slag powder.
The C of the different cement replacement of table 5 amount
30And C
60Concrete 3d ultimate compression strength comparing result/MPa
Embodiment 2
Be used to produce the slag silicate cement
1) will adopt slag crushing that water quenching handled and wet grinding to 5mm, and obtain the wet slag of converter after selecting metal, water ratio is about 8% after outdoor airing, and the chemical ingredients of slag and other raw material sees Table 6.
Certain cement production enterprise experiment of table 6 chemical composition analysis of raw material
2) with produce nitro-cotton byproduct---nitre sulphur mixing spent acid is a main component, water is to being diluted to mass concentration about 8% (with [H
+] meter), add naphthalene water reducer and be mixed with activation solution, proportioning such as table 7 as permeate agent and trolamine hardening accelerator.By the activation solution consumption of the dried slag of 1000 ± 50ml/ kilogram, dry the bessemer furnace slag powder activate 12 hours in activation solution after.
The dried slag of proportioning/kg of table 7 chemical activation liquid
3) slag, slag, grog and gypsum are carried out combined grinding according to following table 8 metering and adding standard test mill, the control fineness is at 350 ± 10m
2/ kg goes out mill and is the slag silicate cement; Perhaps slag and slag are distinguished grinding to 450 ± 20m on the standard test mill
2Behind/the kg, be mixed into the slag silicate cement with silicate cement by a certain percentage again.
Proportioning/the wt% of several slag silicate cements of table 8
Combined grinding and the fundamental property of the slag silicate cement that makes of grinding is as shown in table 9 respectively:
The performance of several slag silicate cements of table 9
As seen from Table 9,6
*With 8 standards that reached 32.5 grades of slag silicate cements, and 7
*With 9 standards that reached 42.5 grades of slag silicate cements, can be used for general industrial and covil construction, road engineering and other engineering.
Embodiment 3
Be used to produce masonry cement
Raw material and slag activation method respectively will be through bessemer furnace slag and slag difference grinding to 450 ± 20m on the standard test mill of activation treatment with embodiment 2
2Behind/the kg,, can be mixed into the special-purpose masonry cement that meets the GB/T3183-2003 requirement again by steel-making slag powder 40%, slag powders 40%, chamotte powder 15%, terra alba 5% (grog and gypsum combined grinding).Mainly by steel-making slag powder and the composite masonry cement performance of slag powders and as shown in table 10 with the contrast of standard:
Table 10 slag masonry cement performance reaches the comparison with standard
As seen from Table 10, reach in the waste residue total amount under 80% the situation, mainly still can reach the requirement of 22.5 grade standards, belong to typical cement with little clinker kind by the masonry cement of steel-making slag powder and slag powders preparation.
The activation effect contrast of different acidic substance
Adopt the raw material identical, at chamotte powder 26% (320 ± 10m with embodiment 2
2/ kg), steel-making slag powder 30% (400 ± 20m
2/ kg), slag powders 40% (450 ± 20m
2/ kg), be mixed with the slag silicate cement under the proportioning of terra alba 4% (with the grog grinding).Slag adopts different types of acid activation, is 0.3～0.4mol/l in the activation solution acid concentration of [H+], does not add permeate agent and hardening accelerator.Measure the intensity of each slag silicate cement respectively, and compare with the cement of the preparation of activated steel slag powder not, the result is as shown in table 11:
The multi-form acid of table 11 is to the influence of dross slag cement intensity
As can be seen from the above table, multi-form mineral acid or organic acid all have in various degree promoter action, wherein H to the early strength of slag silicate cement
2SO
4Effect the most remarkable, secondly be H
3PO
4, HNO
3And HAc, later strength also generally is higher than the not cement of activated steel slag preparation.But increasing degree is littler.
The 3d intensity of activated steel slag too low (11#) does not reach the national standard requirement of 32.5 grades of slag silicate cements, and remaining has all reached the national standard requirement of 32.5 grades of slag silicate cements, and certain surplus strength is arranged.
The method that hot vexed pot process described in the foregoing description, water quenching are handled slag all is prior aries, and dawn is known to those skilled in the art.
Claims (6)
1. bessemer furnace slag chemical activation liquid, it is characterized in that described activation solution is a kind of acidic aqueous solution that is mixed with by the water-soluble acid material beyond demineralizing acid and the hydrofluoric acid, acid concentration in the solution is counted 0.1～1.0mol/l with H+ concentration, and in this acidic aqueous solution, adding the permeate agent account for final solution mass concentration 0.01～0.05%, described permeate agent is a kind of in naphthalenesulfonate formaldehyde condensation compound, condensate of melamine and formaldehyde, sulfamate formaldehyde condensation products, high-efficiency water-reducing agent of poly-carboxylic acid or the alkylphenol polyoxyethylene.
2. bessemer furnace slag chemical activation liquid according to claim 1, it is characterized in that described activation solution also comprises accounts for the final solution mass concentration greater than 0 smaller or equal to 0.5% hardening accelerator, and described hardening accelerator is a kind of in trolamine, tri-isopropanolamine, urea, quadrol, hexamethylenetetramine or the azanol.
3. bessemer furnace slag chemical activation liquid according to claim 1 is characterized in that described water-soluble acid material is a kind of, the perhaps several arbitrary proportion mixing acid in sulfuric acid, sulfurous acid, nitric acid, phosphoric acid, phosphoric acid dihydro amine, formic acid or the acetic acid.
4. bessemer furnace slag chemical activation liquid according to claim 1 is characterized in that described water-soluble acid material is the industrial waste acid that does not contain Cl, F, K and Na objectionable constituent.
5. the using method of the described bessemer furnace slag chemical activation of claim 1 liquid is characterized in that according to adding 0.5～1.0m in the dry bessemer furnace slag per ton
3The ratio of chemical activation liquid will be vexed through shrend or heat in advance, and the bessemer furnace slag and the chemical activation liquid that select iron to handle fully stir, mix, keeping soaking activation 1～24 hour under the moisture state, after drying or drying, promptly getting the bessemer furnace slag of handling through chemical activation liquid.
6. the using method of the described bessemer furnace slag chemical activation of claim 2 liquid is characterized in that according to adding 0.5～1.0m in the dry bessemer furnace slag per ton
3The ratio of chemical activation liquid, will be vexed through shrend or heat in advance, and the bessemer furnace slag and the chemical activation liquid that select iron to handle fully stir, mix, keeping soaking activation 1～24 hour under the moisture state, after drying or drying, promptly getting the bessemer furnace slag of handling through chemical activation liquid, wherein, described hardening accelerator adds in the bessemer furnace slag with the acidic aqueous solution of the chemical activation liquid mixed solution with permeate agent.
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| CN115679023A (en) * | 2022-10-20 | 2023-02-03 | 江西联达白源冶金有限公司 | Steel slag activity excitant and preparation method thereof |
| CN115872651A (en) * | 2023-01-10 | 2023-03-31 | 河北通华公路材料有限公司 | Modification method of steel slag powder for concrete and application of steel slag powder |
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