CN105060758A - Method for preparing alkali-slag cement retarder through jarosite slag - Google Patents

Method for preparing alkali-slag cement retarder through jarosite slag Download PDF

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Publication number
CN105060758A
CN105060758A CN201510532108.XA CN201510532108A CN105060758A CN 105060758 A CN105060758 A CN 105060758A CN 201510532108 A CN201510532108 A CN 201510532108A CN 105060758 A CN105060758 A CN 105060758A
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China
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slag
iron vitriol
alkali
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vitriol slag
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CN105060758B (en
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李玉香
谭宏斌
王进
王军霞
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Southwest University of Science and Technology
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Southwest University of Science and Technology
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Abstract

The invention discloses a method for preparing an alkali-slag cement retarder through jarosite slag. The method sequentially comprises the steps that a dispersing agent, the jarosite slag and an oxidizing agent are added into water and evenly stirred, lime is added, even stirring is carried out, and the mixture stands to achieve solid-liquid separation; solid phases obtained after solid-liquid separation are dried, and the alkali-slag cement retarder is obtained; an extraction agent is added into liquid phases obtained after solid-phase separation, valuable metal silver is recycled, and extraction liquid is recycled as water used in the first step. The method is simple and good in effect and has a significant benefit.

Description

The method of alkali-slag cement retardant is prepared with iron vitriol slag
Technical field
The present invention relates to a kind of Solid state fermentation, the iron vitriol slag that particularly a kind of zinc hydrometallurgy produces is that raw material is to prepare the method for alkali-slag cement retardant.
Background technology
Nineteen fifty-seven, Kiev School of Architecture & Civil Engineering of Ukraine ties up. and the people such as moral. Ge Luhuo Paderewski professor use rubble, boiler slag or blast-furnace slag levigate, or unslaked lime add blast-furnace slag and silicate cement (or not adding) mixing after, again with NaOH solution or the clean slurry of water glass solution modulation, obtain the gelling material of intensity up to 120MPa, good stability.To nineteen fifty-nine, they are the same with silicate cement by this cement of research proof further, can harden under standard and natural condition in water, also can harden under vapor cure treatment condition, this cement be present alkali-slag cement [Wu Qisheng. the research and development [J] of alkali slag cement. Chinese building material science and technology, 1999, (1): 1-4].
Alkali-slag cement has the excellent properties such as high-strength, low hydration heat, high impervious, high anti-freezing and high resistance to corrosion, and this method for production of cement is simple, save energy, cost are lower, can say that alkali-slag cement is a kind of environment-friendly type " green cement ".Although alkali-slag cement has excellent hydraulic properties, because alkali-slag cement exists the too fast shortcoming of condensation, be therefore greatly limited in application.When preparing high-strength concrete (> C80), the initial set process of alkali-slag cement completes usually in 10 ~ 30min.Obviously, the time of coagulation of alkali-slag cement is so short, is [the He Juan that at all cannot be applied in construction work, Yang Changhui, Kang Sufang. the progress [J] of alkali-slag cement slow setting problem. silicate is circulated a notice of, and 2010,29 (5): 1093-1097].
The people such as Zhang Shuo study discovery, several soluble zinc salt (zinc nitrate, zinc sulfate and zinc chloride) and the condensation of nitrate of baryta to alkali-slag cement have significant retarding action, and it is less to its strength development side effect, promoter action [Zhang Shuo is even had to strength of cement development during 0.5% volume, Pan Zhihua. chemical substance is on the impact [J] of alkali-slag cement time of coagulation and strength property. concrete, 2010, (9): 68-73].
Nearly ten years, the plumbous zinc metallurgy of China maintains the impetus increased fast, and 2010, plumbous zinc ultimate production reached 958.10 ten thousand tons.For the wet process Sheng electricity zinc factory of annual output 100000 tons, if zinc ore concentrate iron content is in 8%, then the iron vitriol slag (ammonium jarosite) of annual output is about 5.3 ten thousand tons, general slag field of building nearby is stored up, not only take valuable land resources, and the heavy metal in iron vitriol slag, as Zn, Cu, Cd, Pb, As and Sb etc., naturally the continuous stripping of meeting under condition is being stored up thus polluted underground water and soil [Chen Yongming, Tang Motang, 19th volume the 7th interim state non-ferrous metal journal Yang Sheng sea, decompose containing indium iron vitriol slag novel method [J] Deng .NaOH. China YouSe Acta Metallurgica Sinica, 2009, 19 (7): 1322-1331].The plumbous zinc metal production of China occupies the first in the world for years.While the develop rapidly of product production capacity, the process problem of the ammonium jarosite in production process progressively shows especially, is not only related to the comprehensive cyclic utilization of resource, and is more related to the impact on physical environment.
During with cement solidification process iron vitriol slag, the harmful element of curable iron vitriol slag [Hou little Qiang, Zheng Xutao, Guo Congsheng. admixture on impact [J] .2014 of cement solidification iron vitriol slag performance, 35 (3): 123-127].
General concrete tank can not be used for storing oils, and because oil product easily infiltrates open pore, well capillary penetration and goes out.If concrete is through special processing, can reaches and prevent oil product seepage loss.As add in hybrid junction soil some adulterants with filling concrete when hydration the microporosity that produces.Empirical evidence, admix in concrete colloidal iron hydroxide adulterant effect better [Beijing surveying and designing institute. mix ironic hydroxide oil-proof concrete tank [J]. refining of petroleum and chemical industry, 1958, (11): 36-38].
Summary of the invention
The iron vitriol slag that the object of the invention is to utilize zinc hydrometallurgy to produce, as raw material, provides a kind of alkali-slag cement retardant preparation method increasing the presetting period.
Technical scheme of the present invention is: a kind of iron vitriol slag prepares the method for alkali-slag cement retardant, comprise the steps: successively 1. in water, to add dispersion agent, iron vitriol slag and oxygenant, after stirring, then add lime, leave standstill after stirring, make solid-liquor separation; Wherein, iron vitriol slag add-on is 1/4 of the quality of water; Oxygenant add-on is the 1-5% of iron vitriol slag quality; Dispersion agent add-on is the 0.1-0.5% of iron vitriol slag quality; The add-on of lime is the 10-30% of iron vitriol slag quality; 2. gained solid phase after solid-liquor separation is dried, obtain alkali-slag cement retardant.
In aforesaid method, oxygenant is Na 2o 2, H 2o 2, KMnO 4in any one; Dispersion agent is any one in rosined soap, sodium alkyl benzene sulfonate, sodium lignosulfonate or oxidized paraffin wax soap.
In aforesaid method, add the extraction agent of iron vitriol slag quality 0.1-0.5% after solid-liquor separation in gained liquid phase, reclaim valuable metal silver, raffinate is as the water circulation use in step (1); Described extraction agent is any one in thioether, diethyl curing phosphoric acid, 2-(tertiary dodecyl sulfo-) pyridine.
The advantage of the inventive method adds dispersion agent, is conducive to the dispersion of iron vitriol slag; Add oxygenant, can by the ferrous oxidising one-tenth ferric iron in iron vitriol slag; The reaction of iron vitriol slag and lime, the solid phase obtained is the vitriol of calcium sulfate, ironic hydroxide and metal ion.Calcium sulfate can participate in the hydration reaction of cement, obtains sulplo-aluminate material.Ironic hydroxide can be filled in the Confucius of cement product, improves the compactness of Behavior of Hardened Cement Paste.The vitriol of metal ion hinders hydrated cementitious, plays delayed coagulation.
Decompose to iron vitriol slag the Ag released to reclaim, can further improve economic benefit.
Embodiment
Iron vitriol slag prepares a method for alkali-slag cement retardant, comprises the steps:
1. in water, add dispersion agent, and add iron vitriol slag and oxygenant, after stirring, add lime, leave standstill after stirring, make solid-liquor separation; 2. solid phase is dried, obtain retardant; 3. add extraction agent in the liquid phase, Footwall drift silver, raffinate can be used as the water circulation use in step (1).
Wherein, each component of water, dispersion agent, iron vitriol slag, oxygenant, lime, extraction agent and add-on reference table 1.Table 1 lists the formula composition of 12 embodiments being numbered 1-12.With retardant prepared by the inventive method, after joining alkali-slag cement, according to GB " cement normal consistency water consumption, time of coagulation, stability (GBT1346-2011) ", the presetting period recording this alkali-slag cement is all greater than 60 minutes.
Percentage ratio described in the present invention, if no special instructions be mass percent.

Claims (4)

1. prepare a method for alkali-slag cement retardant with iron vitriol slag, comprise the steps: successively in water, add dispersion agent, iron vitriol slag and oxygenant, after stirring, then add lime, leave standstill after stirring, make solid-liquor separation; Wherein, iron vitriol slag add-on is 1/4 of the quality of water; Oxygenant add-on is the 1-5% of iron vitriol slag quality; Dispersion agent add-on is the 0.1-0.5% of iron vitriol slag quality; The add-on of lime is the 10-30% of iron vitriol slag quality; gained solid phase after solid-liquor separation is dried, obtains alkali-slag cement retardant.
2. iron vitriol slag according to claim 1 prepares the method for alkali-slag cement retardant, it is characterized in that, described oxygenant is Na 2o 2, H 2o 2, KMnO 4in any one; Dispersion agent is any one in rosined soap, sodium alkyl benzene sulfonate, sodium lignosulfonate or oxidized paraffin wax soap.
3. iron vitriol slag according to claim 1 prepares the method for alkali-slag cement retardant, it is characterized in that, adds the extraction agent of iron vitriol slag quality 0.1-0.5% after solid-liquor separation in gained liquid phase, reclaims valuable metal silver; Raffinate is as step in water circulation use.
4. iron vitriol slag according to claim 3 prepares the method for alkali-slag cement retardant, it is characterized in that, described extraction agent is thioether, diethyl curing phosphoric acid, the tertiary dodecyl sulfo-of 2-() any one in pyridine.
CN201510532108.XA 2015-08-26 2015-08-26 Method for preparing alkali-slag cement retarder through jarosite slag Expired - Fee Related CN105060758B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105668604A (en) * 2016-01-04 2016-06-15 西南科技大学 Columnar gypsum prepared from pyrite cinder and filtrate treatment method
CN106734062A (en) * 2016-11-29 2017-05-31 金川集团股份有限公司 It is a kind of iron vitriol slag is solidified after for the method for filling mine

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1071401A (en) * 1991-10-09 1993-04-28 重庆建筑工程学院 Retardant for alkali slag cement
CN1094382A (en) * 1993-04-24 1994-11-02 湖南省建筑材料研究设计院 Slag alkali cement and manufacture method thereof
CN102249594A (en) * 2011-05-23 2011-11-23 江苏名和集团有限公司 Alkali-activated slag cement retarder and application method thereof
EP2467346B1 (en) * 2009-08-17 2014-05-21 Lafarge Additives for a hydraulic binder based on a belite-calcium-sulphoaluminate-ferrite clinker

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1071401A (en) * 1991-10-09 1993-04-28 重庆建筑工程学院 Retardant for alkali slag cement
CN1094382A (en) * 1993-04-24 1994-11-02 湖南省建筑材料研究设计院 Slag alkali cement and manufacture method thereof
EP2467346B1 (en) * 2009-08-17 2014-05-21 Lafarge Additives for a hydraulic binder based on a belite-calcium-sulphoaluminate-ferrite clinker
CN102249594A (en) * 2011-05-23 2011-11-23 江苏名和集团有限公司 Alkali-activated slag cement retarder and application method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张烁; 潘志华: "化学物质对碱-矿渣水泥凝结时间和强度性能的影响", 《混凝土》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105668604A (en) * 2016-01-04 2016-06-15 西南科技大学 Columnar gypsum prepared from pyrite cinder and filtrate treatment method
CN106734062A (en) * 2016-11-29 2017-05-31 金川集团股份有限公司 It is a kind of iron vitriol slag is solidified after for the method for filling mine

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