CN103922626B - The treatment process of lithium by-product lithium slag, concrete alkali aggregate reaction inhibitor and application thereof are proposed in a kind of salt lake - Google Patents
The treatment process of lithium by-product lithium slag, concrete alkali aggregate reaction inhibitor and application thereof are proposed in a kind of salt lake Download PDFInfo
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- CN103922626B CN103922626B CN201410150737.1A CN201410150737A CN103922626B CN 103922626 B CN103922626 B CN 103922626B CN 201410150737 A CN201410150737 A CN 201410150737A CN 103922626 B CN103922626 B CN 103922626B
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- lithium
- salt lake
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- slag
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 66
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000002893 slag Substances 0.000 title claims abstract description 35
- 239000006227 byproduct Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000008569 process Effects 0.000 title claims abstract description 7
- 239000003513 alkali Substances 0.000 title abstract description 28
- 239000002683 reaction inhibitor Substances 0.000 title description 5
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract 2
- 238000000227 grinding Methods 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 239000000470 constituent Substances 0.000 abstract description 3
- 206010013786 Dry skin Diseases 0.000 abstract description 2
- 238000000498 ball milling Methods 0.000 abstract description 2
- 230000005764 inhibitory process Effects 0.000 abstract description 2
- 230000002787 reinforcement Effects 0.000 abstract description 2
- 239000004568 cement Substances 0.000 description 19
- 239000000203 mixture Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000011734 sodium Substances 0.000 description 7
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000011398 Portland cement Substances 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000012267 brine Substances 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 241001131796 Botaurus stellaris Species 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- -1 admixture Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001418 larval effect Effects 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses the treatment process that lithium by-product lithium slag is carried in a kind of salt lake, comprise the steps: 1) salt lake is carried after lithium by-product lithium slag grinds and sieving; 2) product after sieving, through washing, precipitation, filtration, collects solid also dry.The invention also discloses the inhibitor utilizing the method to prepare.The present invention is by operations such as suitable ball milling, washing, precipitation, filtration, dryings, reduce the ratio of the objectionable constituent sodium-chlor in lithium slag, can obtain functional, the inhibitor of cheap concrete alkali aggregate reaction, this inhibitor avoids the aggravation of sodium-chlor to concrete reinforcement corrosion and concrete alkali aggregate reaction, has the advantages that volume is few, inhibition is good.
Description
Technical field
The invention belongs to Salt Lake Chemistry field, be specifically related to a kind of salt lake and propose the treatment process of lithium by-product lithium slag, concrete alkali aggregate reaction inhibitor and application thereof.
Background technology
Concrete alkali-aggregate reaction (Alkali-AggregateReaction is called for short AAR) is the Free alkali metal ion (Na in concrete
+, K
+deng) and reactive aggregate between a kind of swelling property of occurring react, be the major cause causing concrete durability to decline, once occur, be difficult to stop, more not easily administer, be called as concrete " cancer ", AAR reaction has become in concrete structure the second largest disease being only second to steel bar corrosion.
At present, prevent the major measure of concrete alkali-aggregate reaction (AAR) from having following measure:
(1) inert aggregate is used.Inert aggregate is used to be prevent concrete generation alkali to gather materials the most safe and reliable measure of expanding.But China's reactive aggregate particularly siliceous reactive aggregate is more extensive relative to inert aggregate distribution, and aggregate resources is non-renewable, aggregate resources constantly consumes and the factor such as construction costs limits the selection of aggregate.In addition, at present to evaluation aggregate basic active, particularly the potential basic active of expansion aggregate there is no cocksure method slowly.Therefore, the use of inert aggregate can be subject to the restriction of region and economic aspect.
(2) concrete alkali content is controlled.AAR is a chemical reaction, and when higher alkali content is lower than certain value, AAR reaction is difficult to generation or level of response is comparatively light, is not enough to concrete cracking is destroyed.Restriction concrete alkalinity, generally sets about from reduction cement, admixture, mineral admixture alkali content.China's standard specify alkalinity lower than 0.6% cement be low alkali cement.The U.S., Britain, Japan, New Zealand etc. once also adopted identical standard to reduce alkali content in concrete, and this alleviates AAR problem to a certain extent.But in recent years, widely use containing alkali admixture, and contained alkali is mostly effective alkali, this makes restriction higher alkali content further difficult.
(3) controlling moisture.There are some researches show, reduce relative humidity, AAR can be reduced and expand.But the humidity condition residing for concrete works is uppity, and the factor such as drying and watering cycle can also cause alkali in concrete migration and in Local enrichment, thus aggravation AAR.It is generally acknowledged when relative humidity lower than 80% time, AAR will occur.But the U.S. is shown by on-the-spot test, even if highway pavement and other highway structureses are under desert climate condition, enough moistures are also had to cause AAR.Research shows that the moisture of residual water-content in concrete and outside is enough to AAR is proceeded.Therefore, only fundamentally AAR can not be stoped by waterproof measure.
(4) mineral admixture or chemical admixture is used.Use the mineral admixture replacing section cement such as flyash, silicon ash and slag, can delay or suppress AAR to expand.But just effectively may suppress AAR because mineral admixture needs quite high volume, this brings disadvantageous effect often to other performance of concrete.Large quantity research shows, the salt of the alkali metal containing lithium that admixture is a small amount of has certain restraining effect to AAR.The explanation more consistent for lithium salts suppression AAR ratio of expansion is: with Na
+(K
+) compare, Li
+there is less ionic radius, higher electric density, cause L-S to have stronger ionic bond power compared with N-S and K-S thus, cause Li
+replace Na+ (K
+) preferentially defining the reaction product L-S-H of non-expansibility, these finer and close products are wrapped in and gather materials around, prevent Na
+(K
+) to the further erosion of gathering materials.With mix compared with mineral admixture, use chemical admixture need not change concrete execution conditions, operation is simple and feasible, and addition content is few, and be easily accepted in the widely used contemporary engineering of admixture.But the salt cost of alkali metal lithium is very high, mainly at theoretical side, going back seldom of practical application.And corresponding be that a large amount of lithium slags produced in the performance history of domestic salt lake cannot be fully used.Since the industrialized production of lithium is proposed in domestic employing salt lake, the lithium slag of its by-product, because foreign matter content is high and magazins' layout difficult, does not all find new utilization ways always, is difficult to be made full use of, cause the wasting of resources in Salt Lake Area, have impact on the normal production that salt lake brine proposes lithium industry.
Therefore, in concrete works technical field, in order to improve concrete weather resistance, improve concrete construction quality, and extend its work-ing life and reduce maintenance cost, the admixture of concrete alkali aggregate reaction can be suppressed in the urgent need to a kind of low price.
Summary of the invention
The object of the present invention is to provide the preparation method that a kind of cost is low, volume is few, preparation method simply, does not affect mechanical performance of concrete, can effectively suppress the inhibitor of concrete expansion, the inhibitor prepared and application thereof.
Preparation method of the present invention comprises: a kind of preparation method of concrete alkali aggregate reaction inhibitor, comprises the steps:
1) sieve after salt lake being proposed the grinding of lithium by-product lithium slag;
2) product after sieving, through washing, precipitation, filtration and drying, obtains the inhibitor of concrete alkali aggregate reaction.
The by-product powdered material of lithium by-product lithium slag for producing in salt lake brine extraction Quilonum Retard technological process is carried in described salt lake, composition mainly comprises Quilonum Retard, magnesium hydroxide, calcium carbonate, sodium-chlor etc., its concrete composition changes to some extent according to the technique adopted, but its bulk composition is similar.Such as Chinese patent open file CN102976367A discloses a kind of method utilizing salt lake brine to produce battery-level lithium carbonate, the method uses selective membrane separating technology separated salt lake bittern water, finally obtains the lithium slag containing Quilonum Retard, magnesium hydroxide, calcium carbonate, sodium-chlor etc.Objectionable constituent mainly sodium-chlor in described lithium slag, because of the reinforcing bar in chlorion meeting corrosion concrete, and sodium ion can increase the alkali content in concrete, thus causes the generation that Concrete AR reacts.
Preferably, step 1) in sieve salt lake proposed the grinding of lithium by-product lithium slag after cross 100 ~ 180 mesh sieves.
Preferably, step 2) described in washing temperature be 80 DEG C ~ 120 DEG C, preferably 100 DEG C, till the sodium-chlor in lithium slag is all cleaned.
Preferably, step 2) described in drying temperature be 80 ~ 110 DEG C, preferably 100 DEG C.
Preferably, step 2) described in time of drying be 10 ~ 24h, preferred 24h.
Preferably, step 2) described sedimentation time is 1h ~ 3h, preferred 1.5h.Precipitation not only can allow the sodium-chlor in lithium slag have time enough to dissolve, and other composition water-fast in lithium slag can be made by standing separation, to be conducive to filtration, separating impurity sodium-chlor.
As stated above, can prepare a kind of concrete alkali aggregate reaction inhibitor, this inhibitor may be used at concrete works field replacing partial cement or adds as additive, prevents or suppress the generation that Concrete AR expands.
The present invention is by operations such as suitable ball milling, washing, precipitation, filtration, dryings, reduce the ratio of the objectionable constituent sodium-chlor in lithium slag, the inhibitor of functional, cheap concrete alkali aggregate reaction can be obtained, this inhibitor avoids the aggravation of sodium-chlor to concrete reinforcement corrosion and alkali, has the advantages that volume is few, inhibition is good.The present invention not only solves the lithium resource carried in lithium process in salt lake and wastes problem, the inhibitor also for suppressing concrete alkali to provide a kind of low cost.
Accompanying drawing explanation
Fig. 1, salt lake brine put forward the XRD figure of lithium by-product lithium slag.
Fig. 2, mix the rate of expansion figure carrying lithium by-product lithium dreg concrete different larval instar.
Embodiment
Comparative example 1 ordinary Portland cement C42.5, adopts quick mortar bars method, and the mass ratio of its cement and sand is 1:2.25, and water cement ratio 0.47, in control temperature (40 ± 2) DEG C, tests its rate of expansion under the condition of relative humidity 95%.
Lithium by-product lithium slag is carried from Qinghai Li Ye company limited in embodiment 1 raw material salt lake, and chemical composition is: Mg
2+containing 33.82%, Li
+containing 2.70%, Ca
2+containing 1.54%, Na
+containing 0.52%, Cl
-containing 1.85%, SO
4 2-containing 0.002%, K
+containing 0.14.
Raw material salt lake is carried lithium by-product lithium slag and be milled to 100 orders, then after the water washing using 100 DEG C, precipitation 1.5h, then 24h is calcined at 80 DEG C, obtain the inhibitor of concrete alkali aggregate reaction.
Ordinary Portland cement C42.5, adopts quick mortar bars method, adopts the salt lake Quilonum Retard by-product lithium slag of 30% to replace part of cement consumption, the mass ratio of its cement and sand is 1:2.25, water cement ratio 0.47, in control temperature (40 ± 2) DEG C, tests its rate of expansion under the condition of relative humidity 95%.As can be seen from table 1 and Fig. 2, compare in comparative example 1, the rate of expansion of embodiment 1 obviously obtains suppression.
The rate of expansion of the concrete mortar rod of salt lake lithium slag mixed by table 1
Lithium by-product lithium slag is carried from Qinghai Li Ye company limited in embodiment 2 raw material salt lake, and chemical composition is: Mg
2+containing 33.82%, Li
+containing 2.70%, Ca
2+containing 1.54%, Na
+containing 0.52%, Cl
-containing 1.85%, SO
4 2-containing 0.002%, K
+containing 0.14.
Raw material salt lake is carried lithium by-product lithium slag and be milled to 180 orders, then after the water washing using 100 DEG C, precipitation 1.5h, then 18h is calcined at 80 DEG C, obtain the inhibitor of concrete alkali aggregate reaction.
Ordinary Portland cement C42.5, adopts quick mortar bars method, adopts the salt lake Quilonum Retard by-product lithium slag of 5% to replace part of cement consumption, the mass ratio of its cement and sand is 1:2.25, water cement ratio 0.47, in control temperature (40 ± 2) DEG C, tests its rate of expansion under the condition of relative humidity 95%.
Lithium by-product lithium slag is carried from Qinghai Li Ye company limited in embodiment 3 raw material salt lake, and chemical composition is: Mg
2+containing 33.82%, Li
+containing 2.70%, Ca
2+containing 1.54%, Na
+containing 0.52%, Cl
-containing 1.85%, SO
4 2-containing 0.002%, K
+containing 0.14.
Raw material salt lake is carried lithium by-product lithium slag and be milled to 120 orders, then after the water washing using 120 DEG C, precipitation 1h, then 10h is calcined at 80 DEG C, obtain the inhibitor of concrete alkali aggregate reaction.
Ordinary Portland cement C42.5, adopts quick mortar bars method, adopts the salt lake Quilonum Retard by-product lithium slag of 10% to replace part of cement consumption, the mass ratio of its cement and sand is 1:2.25, water cement ratio 0.47, in control temperature (40 ± 2) DEG C, tests its rate of expansion under the condition of relative humidity 95%.
Lithium by-product lithium slag is carried from Qinghai Li Ye company limited in embodiment 4 raw material salt lake, and chemical composition is: Mg
2+containing 33.82%, Li
+containing 2.70%, Ca
2+containing 1.54%, Na
+containing 0.52%, Cl
-containing 1.85%, SO
4 2-containing 0.002%, K
+containing 0.14.
Raw material salt lake is carried lithium by-product lithium slag and be milled to 180 orders, then after the water washing using 80 DEG C, precipitation 1h, then 24h is calcined at 110 DEG C, obtain the inhibitor of concrete alkali aggregate reaction.
Ordinary Portland cement C42.5, adopts quick mortar bars method, adopts the salt lake Quilonum Retard by-product lithium slag of 50% to replace part of cement consumption, the mass ratio of its cement and sand is 1:2.25, water cement ratio 0.47, in control temperature (40 ± 2) DEG C, tests its rate of expansion under the condition of relative humidity 95%.
The data such as the rate of expansion of above-described embodiment are see table 1 and Fig. 2.
Claims (3)
1. a treatment process for lithium by-product lithium slag is put forward in salt lake, comprises the steps:
1) sieve after salt lake being proposed the grinding of lithium by-product lithium slag;
2) product after sieving, through washing, precipitation, filtration, collects solid also dry;
Step 2) described in washing temperature be 80 DEG C ~ 120 DEG C;
Step 1) in salt lake proposed the grinding of lithium by-product lithium slag after cross 100 ~ 180 mesh sieves;
Step 2) described in drying temperature be 80 ~ 110 DEG C;
Step 2) described in time of drying be 10 ~ 24h;
Step 2) described sedimentation time is 1h ~ 3h.
2. the inhibitor obtained by method according to claim 1.
3. the application of inhibitor described in claim 2 in concrete works technical field.
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|---|---|---|---|
| CN201410150737.1A CN103922626B (en) | 2014-04-15 | 2014-04-15 | The treatment process of lithium by-product lithium slag, concrete alkali aggregate reaction inhibitor and application thereof are proposed in a kind of salt lake |
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| CN201410150737.1A CN103922626B (en) | 2014-04-15 | 2014-04-15 | The treatment process of lithium by-product lithium slag, concrete alkali aggregate reaction inhibitor and application thereof are proposed in a kind of salt lake |
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| CN108273826B (en) * | 2018-01-17 | 2018-12-11 | 成都绿锂环保科技有限公司 | A kind of complete mutually high-valued recoverying and utilizing method of lithium slag |
| CN108516706A (en) * | 2018-04-25 | 2018-09-11 | 中国科学院青海盐湖研究所 | A kind of special cement and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594173A (en) * | 2004-07-05 | 2005-03-16 | 南京师范大学 | Alkali resistant aggregate reaction cement added with composite industrial residue and its firing method |
| CN203382518U (en) * | 2013-07-17 | 2014-01-08 | 西藏金睿资产管理有限公司 | System for differentially extracting lithium carbonate, NaCl and KCl in salt lake brine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594173A (en) * | 2004-07-05 | 2005-03-16 | 南京师范大学 | Alkali resistant aggregate reaction cement added with composite industrial residue and its firing method |
| CN203382518U (en) * | 2013-07-17 | 2014-01-08 | 西藏金睿资产管理有限公司 | System for differentially extracting lithium carbonate, NaCl and KCl in salt lake brine |
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