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Effects of Lixiviant (H2SO4 and C6H8O7) and Reductant (H2O2) with an Application of Acid Leaching in Production of High Quality Quartz

Authors:
  • SDU/Beijing University of Chemical Technology/Satbayev University/Nazarbayev University

Abstract

Purification of quartz with chemical processes is extremely important for many industries including optical quality glass, electronic and advanced technological products. Iron as the most significant impurity present in quartz ores can be substantially removed by aqueous chemical processes using organic and inorganic acids. In this study to investigate the removal of iron as impurity from quartz ores, sulfuric acid and citric acid leaching tests with hydrogen peroxide were conducted. Chemical leaching tests were performed to evaluate the performances of different acids and effects of the parameters including pulp density, temperature, leaching duration and reagent concentration on Fe2O3 removal using full factorial design method. The results were evaluated by ANOVA (analysis of variance) method and empirical regression models were established. Under optimum condition (5% pulp ratio, 3M sulfuric acid concentration, 1M hydrogen peroxide concentration, 90°C temperature and 120 minutes of leaching (reaction) time), a Fe2O3 removal of 98,9% and 1 ppm Fe2O3 content high quality quartz product were obtained when sulphuric acid leaching in the presence of hydrogen peroxide was tested.
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Effects of Lixiviant (H2SO4 and C6H8O7) and Reductant (H2O2) with an
Application of Acid Leaching in Production of High Quality Quartz
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\HULQL GHPLU LOH NRPSOHNV ROXúWXUDUDN GHPLULQ
o|NHOPHVLQLHQJHOOH\HQ YH JHQLúS+ DUDOÕ÷ÕQGD
OLo LúOHPLQLQ JHUoHNOHúPHVLQL VD÷OD\DQ RUJDQLN
DVLWOHUDOPDNWDGÕU3DQLDVYG$PELNDGH-
YLYH/DOLWKDPELND$NFLOYH7XQFXN
$NFLOYG
%LUoRNDUDúWÕUPDFÕNXYDUVYHVLOLNDNXPXQGDVDI-
VÕ]OÕN RODUDN EXOXQDQ )H223¶LQ X]DNODúWÕUÕOPDVÕ
DPDFÕ\OD |]HOOLNOH VOIULN DVLW 7RUR YG 
9HJOLR YG  %DQ]D YG  7XQFXN YH
$NFLOYHRNVDOLNDVLW%RQQH\8EDO-
GLQLYG7D[LDUFKRXYG9HJOLRYG
9HJOLRYG$UVODQ YH%D\DW
'XYGUHDNWLÀHULLOHIDUNOÕoDOÕúPDNRúXOOD-
UÕQGDOLoLúOHPOHULJHUoHNOHúWLUPLúWLU
&HYKHUGHNL )H223 JLEL VDIVÕ]OÕNODUÕQ X]DNODú-
WÕUÕOPDVÕ LoLQ KHU ]DPDQ DVLW OLoL WHN EDúÕQD \H-
WHUOL JHOPHPHNWHGLU )H+2¶QLQ o|]QUO÷QQ
)H+3¶WHQ GDKD \NVHN ROGX÷X GúQOHUHN DVLW
OLoL LúOHPOHULQGH RNVDOLN DVLW VLWULN DVLW JOLNR]
KLGURMHQ SHURNVLW JLEL IDUNOÕ LQGLUJH\LFL UHDNWLÀHU
NXOODQÕODELOLU2NVDODWVLWUDWJLELRUJDQLNDQ\RQODU
\]H\H WXWXQDUDN )H+3 ± 2 ED÷ÕQÕ ]D\ÕÀDWPDN-
WD YH E|\OHFH LQGLUJH\LFL o|]QPH DUWPDNWDGÕU
6FKZHUWPDQQ
+LGURMHQSHURNVLW+222KHP\NVHOWJH\LFLKHP
GH LQGLUJH\LFL UHDNWLI RODUDN NXOODQÕOPDNWDGÕU
H222 JoO ELU \NVHOWJHQ YH oHYUHVHO DoÕGDQ
JYHQOLELUUHDNWLIWLU+LGURMHQSHURNVLWDVLGLNo|-
11
]HOWLOHUGH%D÷ÕQWÕ¶HJ|UHLQGLUJHQLU
H222 + 2H+Ɲĺ+22(0 9 
+LGURMHQ SHURNVLW D\QÕ ]DPDQGD %D÷ÕQWÕ ¶GHNL
\NVHOWJHQPHWHSNLPHVLQHJ|UHLQGLUJH\LFLUHDN-
WLIRODUDNGDYUDQPDNWDGÕU
H222ĺ22 + 2H+Ɲ 
7RSODPWHSNLPHLVH%D÷ÕQWÕ¶WHYHULOPHNWHGLU
2H222ĺ22 + 2H22 
+LGURMHQSHURNVLWLQER]XQPDVÕLOHo|]HOWLGHJHU-
oHNOHúHQ HOHNWURQ WUDQVIHUL YDVÕWDVÕ\OD RNVLMHQ
PLQHUDO \]H\LQGHQ DGVRUSODQPDNWDGÕU  9
SRWDQVL\HOGH÷HULPHWDOVO¿WOHUL RNVLWOH\HELOPH-
VL LoLQ \HWHUOLGLU $\GR÷DQ  $\GR÷DQ YG
 $\QÕ ]DPDQGD KLGURMHQ SHURNVLW DVLGLN
o|]HOWLOHUGHNL ELUoRN PHWDO RNVLW ELOHúL÷LQH NDU-
úÕ GD LQGLUJH\LFL UHDNWLI RODUDN GDYUDQPDNWDGÕU
(O+D]HNYG/LYG%D÷ÕQWÕYH
¶WHNL\NVHOWJHQPHYHLQGLUJHQPHWHSNLPHOHULQH
J|UHQHWWHSNLPH\DQL)H223¶LQLQGLUJH\LFLUHDN-
WLIRODUDN+222¶LQNXOODQÕOGÕ÷ÕDVLGLNo|]HOWLOHUGHNL
NLP\DVDOo|]QPHVL%D÷ÕQWÕ¶WHYHULOPHNWHGLU
)H223++Ɲĺ)H+2 + 3H22 
)H223 + H222 + 4H+ĺ)H+2 + 3H2222 
%X oDOÕúPD NDSVDPÕQGD VDÀDúWÕUÕOPÕú NXYDUV
UQHOGHVLLoLQNXYDUVÕQLQGLUJH\LFLUHDNWLIKLG-
URMHQSHURNVLWYDUOÕ÷ÕQGDLQRUJDQLNVOIULNDVLW
YH RUJDQLN VLWULN DVLW DVLWOHU LOH ELU OLo \|QWHPL
JHOLúWLULOPHVL DPDoODQPÕúWÕU )DUNOÕ IDNW|UOHULQ
NDWÕVÕYÕ RUDQÕ UHDNWLI GHULúLPL VÕFDNOÕN OLo V-
UHVLOLoSHUIRUPDQVÕ]HULQHHWNLOHULEHOLUOHQHUHN
HWNLOHU$129$9DU\DQV$QDOL]L\|QWHPL LOH GH-
÷HUOHQGLULOPLúWLU
2. 'ENEYSEL ÇAL,ù0ALAR
2.1. KXYDUV NXPXQHVL
.XYDUVQXPXQHVL.DOWXQ0DGHQFLOLN6DQYH7LF
$ù dLQH $\GÕQ¶GHQ %DUPDF NÕUÕFÕ oÕNÕúÕ 
FP RODUDN WHPLQ HGLOPLúWLU .XYDUV FHYKHUL |Q-
FHOLNOHoHQHOLNÕUÕFÕ)ULWVFKPDUNDLOHNDGHPHOL
RODUDN PP ER\XWXQD NÕUÕOPÕúDUGÕQGDQPHU-
GDQHOL NÕUÕFÕ ODERUDWXDU WLS hQDO 0KHQGLVOLN
NXOODQÕODUDNQXPXQHQLQWDPDPÕPPER\XWXQD
NÕUÕOPÕúWÕU'DKDVRQUDNXYDUVQXPXQHVLP
ER\XWXQGD DOPLQD ELO\HOL GH÷LUPHQGH |÷WO-
PúYHOLoWHVWOHULQHX\JXQKDOHJHWLULOPLúWLU
.XYDUV FHYKHULQLQ PLQHUDORMLN \DSÕVÕQÕ EHOLU-
OHPHN DPDFÕ\OD RSWLNFHYKHU PLNURVNREX LOH
PDNURVNRELN YH PLNURVNRELN LQFHOHPHOHU \DSÕO-
PÕúWÕU$\UÕFD07$YH ùLúHFDP$U*HODERUDWX-
DUODUÕQGDQDOÕQDQPLQHUDORMLNDQDOL] UDSRUODUÕ LOH
NDUúÕODúWÕUÕODUDNNXYDUVEQ\HVLQGHEXOXQDQVDI-
VÕ]OÕNODUÕLoHUHQPLQHUDOOHUEHOLUOHQPLúWLU
<DSÕODQPDNURVNRELN YH PLNURVNRELN LQFHOHPH-
OHUGH÷HUOHQGLULOGL÷LQGHNXYDUV|UQH÷LQGH)H223
WDúÕ\ÕFÕ PLQHUDOOHU RODUDN KHPDWLW NXYDUVODUÕQ
]HULQGH VÕYDPDODU YH NXYDUV oDWODNODUÕQÕQ
DUDVÕQÕGROGXUPXúúHNLOGHYHPLNDQÕQoR÷XQ-
OXNODPXVNRYLWEL\RWLWYHD]PLNWDUGDIORJRSLW
PLQHUDOL RODUDN EXOXQGX÷X EHOLUOHQPLúWLU ùHNLO
dLIWQLNROLQFHNHVLW|UQH÷LJ|UQWVQGHoLIW
RSWLNHNVHQOLPLQHUDORODQPLNDJ|]OHQLUNHQWHN
QLNROLQFHNHVLW|UQH÷LJ|UQWVQGHLVHRSDNPL-
QHUDORODQKHPDWLWYHWHNRSWLNHNVHQOLPLQHUDOOHU
VLOLVPLQHUDOOHULJ|]OHQPLúWLU
.XYDUV FHYKHULQLQ NLP\DVDO NDUDNWHUL]DV\R-
QXQGD ;ÕúÕQÕ ÀRUHVDQV ;5) 6SHFWUR ;H-
SRV \|QWHPL NXOODQÕOPÕú YH DQDOL]OHU .DOWXQ
0DGHQFLOLN 6DQ YH 7LF $ù¶\H DLW DNUHGLWH RO-
PXú ,62  VHUWL¿NDOÕ $U*H YH .DOL-
WH .RQWURO /DERUDWXDUODUÕQGD \DSÕOPÕúWÕU ;5)
DQDOL]OHULQGH )H223 LoHUL÷L  KDVVDVL\HWOH
RNXQPDNWDGÕU 1XPXQHOHULQ LoHUL÷LQGHNL WP
PHWDORNVLWOHULQGD÷ÕOÕPÕ WDPNLP\DVDODQDOL]LOH
HOGHHGLOPLúYHVRQXoODUÕdL]HOJH¶GHYHULOPLúWLU
;5)DQDOL]LQGHQHOGHHGLOHQVRQXoODUDdL]HOJH
J|UHNXYDUVFHYKHULQLQ)H223LoHUL÷LSSP
7L22LoHUL÷LLVHSSPRODUDNEHOLUOHQPLúWLU.X-
YDUVFHYKHULQLQ EH\D]OÕN ³/´ GH÷HULEH\D]OÕNLQ-
GHNVLWHVWLLOHRODUDNEHOLUOHQPLúWLU
dL]HOJH  .XYDUV &HYKHULQLQ .LP\DVDO $QDOL]
6RQXoODUÕ;5)
%LOHúLP 
6L22
$O223
)H223
7L22
&D2 
0J2 
1D22
K22
..a
7RSODP 
a.Õ]GÕUPDND\EÕ
12
2.2. Y|QWHP
$OPLQD ELO\HOL |÷WPH LúOHPL VRQUDVÕ NXYDUV
QXPXQHVL
PHOHNVHULOHULNXOODQÕODUDNVÕQÕÀDQGÕUÕODUDN
NXYDUV QXPXQHOHULQLQ NLP\DVDO DQDOL]OHULQGHNL
)H223 LoHULNOHUL LQFHOHQGL÷LQGH  P¶GHQ LWL-
EDUHQ\NVHN)H223 LoHUL÷LJ|UOPúWU%XGX-
UXPGD |÷WOPú NXYDUV QXPXQHVLQGH WDQH
ER\XWXQD J|UH ]HQJLQOHúWLUPH \DSÕODUDN 
P¶GHQ LWLEDUHQ DOW IUDNVL\RQODU D\UÕOPÕúWÕU YH
NLP\DVDOOLoWHVWOHULQGHPER\XWDUD-
OÕ÷ÕQGDNL QXPXQHQLQ NXOODQÕOPDVÕ DPDFÕ\OD |Q
]HQJLQOHúWLUPHLúOHPL\DSÕOPÕúWÕU
%|\OHFHNXYDUVQXPXQHVLQGHNL)H223LoHUL÷L
SSPYH7L22LoHUL÷LSSPLNHQWDQHER\XWXQD
J|UH|Q]HQJLQOHúWLUPHLúOHPLLOH)H223LoHUL÷L
SSP¶H7L22LoHUL÷LGH SSP¶HGúUOPúWU
(OGHHGLOHQPYHPNXYDUVQX-
PXQHOHULQLQ NLP\DVDO DQDOL]L dL]HOJH ¶GH YHULO-
PLúWLU /Lo LúOHPOHULQH NDWÕOPD\DQ  P IUDN-
VL\RQXLoLQ DQDOL]GH÷HUOHULJ|]|QQGHEXOXQGX-
UXOGX÷XQGDNLP\DVDOLoHUL÷LQHX\JXQVHNW|UOHUGH
NXOODQÕPÕPPNQGU
dL]HOJH7DQH%R\XWXQD*|UH=HQJLQOHúWLUPHøúOHPL
6RQUDVÕ.XYDUV1XPXQHVLQLQ.LP\DVDO$QDOL]L
%LOHúLP P

P
6L22 
$O223 
)H223 
7L22 
&D2  
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DE      $%     
F      &     
DF      $&     
EF      %&     
DEF      $%&     
G      '     
DG      $'     
EG      %'     
DEG      $%'     
FG      &'     
DFG      $&'     
EFG      %&'     
DEFG      $%&'     
aGHQH\VHO)H223X]DNODúWÕUPDYHULPL
EKHVDSODQDQ)H223X]DNODúWÕUPDYHULPL
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-     -
a     $     
E      %     
DE      $%     
F      &     
DF      $&     
EF      %&     
DEF      $%&     
G      '     
DG      $'     
EG      %'     
DEG      $%'     
FG      &'     
DFG      $&'     
EFG      %&'     
DEFG      $%&'     
aGHQH\VHO)H223X]DNODúWÕUPDYHULPL
EKHVDSODQDQ)H223X]DNODúWÕUPDYHULPL
17
H222 LODYHVL\OH +2624 OLoL GHQH\OHUL VRQXFXQGD
)H223 X]DNODúWÕUPD YHULPL '89¶QL HWNLOH\HQ
DQDIDNW|UYHJLULúLPHWNLOHULdL]HOJH¶WHYHULOHQ
HWNLGH÷HUOHULGLNNDWHDOÕQDUDNùHNLO¶GHJ|VWH-
ULOPLúWLU
ùHNLO+222LODYHVL\OH+2624OLoLGHQH\OHULQGHQHOGH
HGLOHQ)H223X]DNODúWÕUPDYHULPOHULQH HWNL HGHQ DQD
IDNW|UOHUYHJLULúLPOHU
.6 RUDQÕ $ +2624 GHULúLPL % YH VÕFDNOÕN
' DQD IDNW|UOHULQLQ '89 ]HULQGH SR]LWLI \|Q-
GHHWNLOL ROGX÷X J|]OHQPLúDQFDN+222 GHULúLPL
& DQD IDNW|U HWNLVLQLQ ROPDGÕ÷Õ VDSWDQPÕúWÕU
H222 GHULúLPL LOH VÕFDNOÕ÷ÕQ ELUOLNWH &' JLULúLP
HWNLVLQLQ SR]LWLI \|QGH HWNLOL ROGX÷X J|UOPú-
WU EX GXUXPGD \NVHN VÕFDNOÕN GH÷HUOHULQGH
H222¶LQ LQGLUJH\LFL HWNLVL\OH )H223 o|]QPHVL
JHUoHNOHúPHNWHGLU
H222LODYHVL\OH+2624OLoLLOH'89LoLQ0LQLWDE
øVWDWLNVHO<D]ÕOÕPÕNXOODQÕODUDNHOGHHGLOHQGHQN-
OHP DúD÷ÕGD YHULOPLúWLU %D÷ÕQWÕ  'HQH\VHO
'89 LOH UHJUHV\RQ PRGHOOHULQGHQ KHVDSODQDQ
'89 DUDVÕQGDNL LOLúNL GD÷ÕOÕPÕ ùHNLO ¶WH J|VWH-
ULOPLúWLU
ùHNLO+222LODYHVL\OH+2624OLoLQGHGHQH\VHO)H223
X]DNODúWÕUPDYHULPLLOHKHVDSODQDQ)H223X]DNODúWÕUPD
YHULPLQLQGD÷ÕOÕPÕ
<)H2 ;;;
 ;;  ;;  ;; 
;;
52 
ùHNLO ¶WH GHQH\VHO YH KHVDSODQDQ '89 DUDVÕQGDNL
GD÷ÕOÕPÕQNÕVPHQX\XPOXROGX÷XJ|UOPHNWHGLU
øNLQFL DúDPDGD +2624 \HULQH RUJDQLN ELU DVLW
RODQ VLWULN DVLW NXOODQÕODUDN \NVHN YHULP HOGH
HGLOPH\H oDOÕúÕOPÕúWÕU DQFDN HOGH HGLOHQ YHULOHU
H222LODYHVL\OH+2624OLoL YHULOHUL\OH dL]HOJH 
NÕ\DVODQGÕ÷ÕQGD'89¶QLQGDKDGúNROGX÷XJ|-
UOPHNWHGLU 'HQH\VHO VRQXoODU $129$ \|QWH-
PL\OHGH÷HUOHQGLULOLS dL]HOJH¶GDNLHWNLQGH÷HU-
OHUGLNNDWH DOÕQDUDNDQDIDNW|UYHJLULúLPHWNLOHUL
ùHNLO¶WHJ|VWHULOPLúWLU
ùHNLO  +222 LODYHVL\OH VLWULN DVLW OLoL GHQH\OHULQGHQ
HOGHHGLOHQ )H223X]DNODúWÕUPDYHULPOHULQHHWNL HGHQ
DQDIDNW|UOHUYHJLULúLPOHU
H222LODYHVL\OHVLWULNDVLWOLoLGHQH\OHULQGHVÕFDN-
OÕN'DQDIDNW|UQQ'89]HULQGHHWNLQROGX-
÷X J|UOPHNWHGLU <NVHN VÕFDNOÕN GH÷HUOHULQGH
\NVHNOLoYHULPOHULHOGHHGLOPHNWHGLU'L÷HUDQD
IDNW|UOHULQOLoYHULPL ]HULQGHHWNLOLROPDGÕ÷ÕEH-
OLUOHQPLúWLU7PIDNW|UOHULQELUELUOHULLOHJLULúLPHW-
NLVLQLQ$%&'\NVHNYHHWNLQROPDVÕQÕQQHGH-
QLRODUDNVÕFDNOÕNDQDIDNW|UQQ GL÷HU IDNW|UOHU
]HULQGHEDVNÕQROPDVÕV|\OHQHELOLU
H222LODYHVL\OHVLWULNDVLWOLoLLOH'89LoLQ0LQLWDE
øVWDWLNVHO <D]ÕOÕPÕ NXOODQÕODUDN HOGH HGLOHQ GHQN-
OHPDúD÷ÕGDYHULOPLúWLU%D÷ÕQWÕ'HQH\VHO'89
LOHUHJUHV\RQPRGHOOHULQGHQKHVDSODQDQ'89DUD-
VÕQGDNLLOLúNLGD÷ÕOÕPÕùHNLO¶WHJ|VWHULOPLúWLU
ùHNLO  +222 LODYHVL\OH VLWULN DVLW OLoLQGH GHQH\VHO
)H223 X]DNODúWÕUPD YHULPL LOH KHVDSODQDQ )H223
X]DNODúWÕUPDYHULPLQLQGD÷ÕOÕPÕ
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Purification of quartz (iron in particular) with chemical prosesses is extremely important for many industries including glass, electronic, detergent, ceramics, paint, refractory and metallurgy. The iron content of quartz is required to be in the range of 0.01-0.1% for its industrial use. Turkish quartz reserves have not been exploited effectively in the glass and electronical industries mainly due to the limitations in the quality and quantity of these resources. There appears to be different physical and chemical methods in industrial scale available for the beneficiation of quartz to reduce its iron content down to the desired levels. Although the physical methods including conventional magnetic separation, new and more expensive super conductive magnetic separation and flotation are commonly employed, the chemical methods have been gaining importance particularly due to the low efficiency of physical methods for iron removal. Iron as the most significant impurity present in quartz ores can be substantially removed by aqueous chemical processes using organic and inorganic acids. In this respect, oxalic acid appears to be one of the most significant leaching reagents for the removal of iron. In this article, the industrial use of quartz, area specific requirements for product quality and chemical methods (with particular reference to oxalic acid systems) used in the purification of quartz are critically reviewed.
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The aim of the work was to decrease the iron content of ferrous quartz sands by fixed-bed column leaching with recycling of the leaching solutions in order to attain a product suitable for industrial use. Dissolution of iron was achieved by treating the sands in an acid medium with a reducing agent (oxalic acid) to convert FeIII into FeII.The factors assumed to affect dissolution of iron, such as temperature, oxalic acid concentration, pH and flow-rate, were studied with a 24 full factorial design in order to assess the main effects and the interactions among the factors.Removal of 46.1% iron gives a product containing 0.0163% Fe2O3 which is fit for industrial applications.
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The purification of quartz using chemical processes is extremely important for many industries, including the glass, electronic, detergent, ceramics, paint, refractory, and metallurgy industries, as well as for advanced technology products. The purpose of this work was to investigate the removal of iron as an impurity from quartz ores using a chemical leaching method with different reagents.The iron content of the quartz ore sample was 310 ppm, and the iron was in the form of Fe2O3. In the first step, pre-enrichment studies were conducted based on the particle size, and the Fe2O3 content of the quartz ore was decreased to 88 ppm. A statistical design of the experiments and an ANOVA (analysis of variance) were performed in the second step to determine the main effects and interactions of the researched factors, which were the concentration of the leaching reagent (H2SO4, HCl, H3PO4, HClO4, and NTA [Nitrilotriacetic acid]), solid/liquid ratio, leaching temperature, and leaching time. The highest Fe2O3 removal was 86.6%, and a 11.8 ppm Fe2O3 content quartz product with a whiteness index (WI) value of 90.6 was obtained after 120 min of treatment at 90°C with a 10% S/L ratio and 1 M H2SO4.
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A study has been made of a leaching process to remove iron from quartziferous industrial minerals using oxalic and sulphuric acid in a drum reactor. The experimental work was necessary because of the paucity of literature on the use of oxalic acid in the treatment of industrial minerals containing iron as an impurity. The positive effect of oxalic acid on the iron extraction yield is clearly observed during leaching in a drum reactor. Iron extraction yields of 35–45% are obtained on treating the quartz with 3 kg/t oxalic acid and 2 kg/t sulphuric acid at 90°C for 4–5 h. Under the same conditions but without oxalic acid the iron extraction yield ranges from 3 to 9%, depending on the sulphuric acid content. Chemical and mineralogical analyses were run on the ore to ascertain where the iron compounds occur on the different mineral components. These analyses were carried out on an as-is sample and on three other samples obtained by magnetic separation. The experimental results indicate that 52% of the iron is found in the mica fraction. These results explain why the maximum iron extraction yield is only 35–45%. A flow-sheet of the process is proposed together with a rough material balance in order to estimate oxalic acid, sulphuric acid and water consumption.