NGHIEN c t r u THU NHAN TONG OXIT DAT HIEM Ttr QUANG DAT HIEM KON TUM NGUYEN KHAI
BANG PHU'ONG PHAP AXIT
VO VAN TAN - HUYNH THI TU OANH Trudng Dgi hoc Suphgm - Dai hgc Hue Tom tat: Da nghien cim thu nhan tdng oxit dit hi£m tu quSng dit hilm nguyen khai a Kon Tum bang phuong pbap axit vdi: H3SO4, HNO3, HCl.
Ket qua nghien ciru cbo thay, d^ thu nhan tdng oxit dSt hi6m dat hieu suat cao can phai thuc hien trong nh&ng di^u kien: H2SO4 II M, thdi gian 150 phut d nhiet dp sdi cua hon hpp, ty Ie axit/quang = 4:1 (mL/g) va kicb thudc quang < 0,125 mm.
I.MODAU
Trong nhimg nam gan day, cac nguyen td dat hilm da trd thanh vat lieu chi6n lupc cho cac nganh cdng nghe cao nhu dipn - dipn tu, hat nhan, quang bpc, vu tru, vat lieu sieu dan, sieu nam cham, luy6n kim, xiic tac, thiiy tinh va gom sir ky thugt cao, phan bon vi Iirpng... O Viet Nam, cac cdng ty khai thac sa khoang d Ha Tinb, Quang Tri, Thira Thien Hu6, Binh Djnh, Ninh Thu§n... chi mdi lam giau va phan chia thanh cac Ioai tinb quang nhu Ilmenite, Monazite (cd chua cac nguyen td dit hiem), Rutil va Zircon, [2], [3], [4], [5], [6], [7] chu yen de xuSt khau dudi dang tinb quang cho Trung Qudc, Nhat Ban... nen hieu qua ldnh te rat thip. Vi vay, viec nghien cuu de tach cac nguyen td dSt hi6m tir cac logi quang chua dit hiSm nham nang cao gia tri kinh te, khai liiac va sir dung mpt each cd hieu qua tai nguyen dSt nudc la vdn d8 thdi sir.
Khu vuc Kon Tum, Budn Ma Thudt da tir lau dirpc xem la vimg phong phii khoang san, dac bi?t la vang, da quy va cac kim logi quy hiSm. Cac tinh toan so bp trong mpt sd khu vuc nhu or Sdng Cdn, Cdn Chd Rd, Dac Se Pay cho trii lupng du bao khoang san thori va cac nguyen t6 dat hiem len den con sd hang chuc trieu t3n, trong dd cd cac nguyen to dit hi6m nhom nSng chiem ty le cao [I], [2], Do dd, viec thu hdi dit hiem a khu vuc Kon Tum - Budn Ma Thuot can dupc dau tu nghien ciiu dung muc, xung dang vdi trien vpng Idn cua chiing.
Trong phgm vi bai bao nky, chiing toi trinh bay mpt sd ket qua budc diu vk nghien ciru thu nhSn tong cac oxit dat hiem tir quSng dat hiem Kon Tum nguyen khai bang phuang phap axit.
2. TW'C NGHIEM
Quang dat hiSm Kon Tum 0 dgng nguyen khai dupc say khd, nghien nhd va phan loai cd hgt tir 0,074 mm den 0,125 mm.
Cac loai hda chit diing d§ nghien cuu: H2SO4, HCl, HNO3, H2C2O4, NaOH, dung djch NHi... deu cd dp sgch PA.
Tap chi Khoa hoc va Giao due. Tmdng Dai hpc Sir pham Hue ISSN 1859-1612, S6 03(23)/2012, ir. 37-43
VO V.4N TAN - HUYNH THI TU OANH
SiJ dung cac loai axit HCl, HNO3, H2S04 a cac nong i6 khac nhau it phati huy quSng trong binh Kjeldahl c6 gSn sinh han h6i luu 6- khoang thm gian nhat dinh, rot de ngupi;
dims nuoc cat pha loang thanh 10 Ifa, khudy deu cho dtt hiem tach khoi can, ii lang, gan va loc liy p h k dung dich trong Dung djch thu duoc dua ve pH =1 de I091 bo tap chit Sau do ii ling va loc liy phin dung djch trong, ti6p tuc cho dung dich ket tua tong hydroxit dit hiSm bing dung dich NH3. Riia k6t tua Ln(0H)3 bang nuac cat, roi hoa tan Ln(OH)j lai bJng dung dich axit cho din pH = 1,5. Sau do ket tua tong oxalat nguyen t6 dit hiem bing HiCjO, bio hoa o SO'C; ii mu6i kit tua trong vong 12 gio roi loc ya rOra kit tia thu duoc bing dung dich H2C204 1 % cho sach tap ch4t (Fe , Ca"*,...). Say kho Ln2(C204)3 o nhi?t do 80°C, l«i nung Ln2(C204)3 » nhiet do 900 C trong vong hai gio dl thu tong oxit dat hilm.
Hieu suit thu nhan t6ng oxit dit hilm (H%) dugc tinh theo cong thuc:
/f%- 2,11 .m - . 1 0 0 % Voi a: la luong t6ng oxit dit hiem thu dugc, (g).
m: lugng quang dung de nghien ciru, (g).
3. KET QUA VA THAO LUAN
3.1. Thinh phin hoa hoc cua quang dit hilm Kon Turn nguyen khai
Thiinh phin cac nguyen t6 hoa hpc trong quang dit hilm Kon Tum nguySn khai da xic dinh bing phuong phap XRF dugc trinh bay o bang 1.
Bang I. Thdnh phdn hda hoc quang ddt hiem Kon Tum nguyen khai
Sti 1 2 3 4 5 6 7 t!
9 10 11 12 13 14 13
Nguyen Id SlO;
FeiO, AljOj BaO MgO K , 0 MnO T i O ; ThO:
PzOj
so.
F C e O . N b ; 0 ; NdiOj
Thanh phan
(%)
23,4100 23.2800 9.7800 9.5900 6.8000 3.1500 3.1100 2.4400 2.2000 1,9700 0.8990 0.8020 0.6760 0.4020 0.3980
Sti 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30
Nguyen to ZrO, CaO N a : 0 YzOj U : 0 3 ZnO PbO SrO UjOg GdjOj PrsO,, Sm205 Cl V , 0 5 DyjOs
Thanh phfin 0,3170 0.2730 0,1970 0,1960 0,1940 0,1670 0,0985 0.0976 0,0900 0.0870 0,0778 0,0769 0,0560 0,0352 0,0318
Stt 31 32 33 34 35 36 37 38 39 40 41 42 43 44
Nguyen to RbjO CuO 1 Er^Oj E u : 0 3 NiO Cr^Oj WO3 SbjOj A r CojO^
S c O j CdO GajOj
Thanh phan 0,0282 0.0224 0,0193 0,0162 0.0145 0.0133 0.0122 0,0106 0,0086 0,0085 0,0078 0,0053 0.0025 0.0017
long nguyen t6 dat hilm co trong quang dit hilm Kon Tum nguyen khai (dugc xic
NGHIEN CUU THU NHAN TONG OXIT DAT HIEM TU" QUANG DAT HIEM KON TUM..
dinh bang quang phe Plasma, tai Vien mo Dia chSt - Ha Dong - Ha Npi) la 2,11%.
Nhu vay quSng dat hiem Kon Tum co chua cac nguyen to dSt hiem thupc loai trung binh; qua tiinh lam giau quang de d u p ^ j ^ quang dit hilm rat phuc tap va hieu suat thap, do do trien khai nghien cuu thu HhSi tong oxit ddt hi§m tir quang dat hiem Kon Tum nguyen khai bing phucmg phap axit don gian va hieu qua hon.
3.2. Anh buvng cua ban chat va ndng do cac loai axit den hieu suat nhu nhan tong oxit dat hiem
(5ac tSi Dgfiiem%ghi8n cilfi anM hu6?ig ciia ban chSt va nong dp cac logi axit den hieu suSt nM^gHSif^^loxit dat hiem tir quang iit hiem Kon Tum nguyen khai dupc tien hanh vai cac loai axit: HCl, HiSOd, HNO3 a cite khoang n6ng dp tii 4-12 M, kich thuoc hat <0,074 mm, phan ung dupc duy tri a nhiet dp soi cita h5n hpp trong thai gian 120 phut. Ket qua nghien cihi anh huang ciia ban chit va ndng dp axit dSn hieu suat thu nhan tong oxit d3t hiem dupc trinh bay a hinh I.
Hinh 1. Anh huang cua bdn chdt vd ndng dg cdc axil HCl, H2SO4, HNO3 den hieu sudt ihu nhdn tdng oxit ddt hiem
Tir hinh 1, cho thay khi xir ly qu3ng dat hiem Kon Tum nguyen khai bang cac logi axit H2SO4, HNO3, HCl vai n6ng dp trong khoang 8-12 M thi hieu suat thu nhan tdng exit dit hiSm tSng nhanh va co sir chenh Ipch theo ban chit ciia ba loai axit.
Dk dam bao kinh te cho qua trinh thu nhan tong oxit dat hiem tir quang dat hiem Kon Tum nguyen khai, chiing toi nhgn thiy sii dung axit H2SO4 de xii ly quang dit hiem Kon Tum nguyen khai la tot nhiit, sau do den axit HNO3 va cuoi cung la axit HCl. De dam bao cho cong ngh? san suat cac logi muoi dat hiem phuc vu cho muc dich chiet tach phan chia cac nguyen to dat hiem rieng re, thi co the su dung nong d6 cac logi
vo VAN TAN - HUYNH THI TU OANH
axit: H2SO4 11 M; HNO3 9 M; HCl 12 M la hieu qua nhlt.
3.3. Anh hirffng cua thoi gian phiin tag din hieu suit thu nhan tong oxit dat hiem Cac thi nghiem nghien cuu anh hu65i.°?ua thgi gian phan ijmg din hieu suit thu nhjn t6ng oxit dit hilm tit quang dit hilnf Kon Tum nguyen khai dugc tien hanh trong di6u kien ty le axit/quSng la 4:1 (mL/g); n6ng dg cacloai axit H2SO4 11 M, HNO3 9 M, HCl 12 M; plian ling vin duy Bi o nhiet do soi cua hon hgp. Thtii gian phSn huy tju^ng dugc 30 tangdin tiidO dladSO ptajt. Klfaqua nghien ciru sit phu thugc ciia hieu suat thu nh|n ting oxilnSlite4pD«ao thm gian phan huy quang dat hiem Kon Tum nguyen khai dugc tritih bay g hinh 2.
Hinh 2. ^n/i huang cita Ihdi gian phdn ung din hi^u sudt Ihu nhdn Idng oxit ddt hiim Tir hinh 2, co the nhan thay v6i ca ba loai axit H2SO4, HNOs, HCl khi tang then gian phan ung tir 30 phut din 180 phiit thi hieu suit thu nhan tong oxit dat hiem tang len.
Hieu suat thu nhan tong oxit dit hiem tir qu^ng dit hilm Kon Tum nguyen khai cao nhlt la H2SO4 trong khoang thoi gian phan huy quSng tit 150 din 180 phiit; HNO3 la 120 phiit; HCl la 150 phiit.
3.4. Anh huvng ciia ty le axit/qu|lng din hieu suat thu nhan tong oxit d i t hilm Cac thi nghiem nghien cuu anh huong ciia ty le axiUquang din hieu suit thu nhan ting oxit dat hiem tu quang dat hiem Kon Tum nguyen khai dugc tiln hanh trong cimg dieu kien nhu nhauvl c8 hat 0,074 mm, n6ng dg axit H2SO4 1 i M, HNO3 9 M, HCl 12 M, nhi6t dp soi hSn hgp. Nhung ty le axit/qu5ng dugc thay dli tit 1:1 din 6:1 (mL/g). Kit qua nghien ciiu anh huong cua ty le axit/qujng din hieu suit Ihu nhan tdng oxit dit hilm tit quang dat hiem Kon Tum nguyen khai dugc trinh bay a hinh 3.
NGHIEN CUU THU KtLKS TONG OXTT DAT HEM TU QUANG DAT HIEM KON TUM .
Ty 1^ aiot/quang, '.rrUg)
Hinh 3. Anh huang cua ty le axil/qudng din hieu sudt thu nhdn tdng oxit ddt hiem Tir hinh 3, cho thiy ty 18 axit/quang anh huang rat lan dSn hieu suat thu nhan tong oxit dat hiem tir quang dit hiSm Kon Tum nguyen khai bing phuang phap axit. Trong trucmg hap nay chung toi chpn ty 1? axit/quang hieu qua cao nhat la: H2SO4 la 4:1 (mL/g); HNO3 la 5:1 (mL/g); va HCl la 5:1 (mL/g).
3.5. Anh biroiig cua kich thirac hat quang den hieu suat thu nh^n tong oxit dat hiem
Trong truang hpp nay chung toi chpn cac dieu kien toi iru 6 tren de khao sat anh huong ciia kich diuac hgt quang dat hiem Kon Tum nguyen khai dSn hieu suat thu nh|in t6ng oxit dit hi6m dupc. Nhung kich thuac hat quang dat hiem Kon Tum nguyen khai dupc thay d6i tir nho han 0,074 den 0,125 mm. Kdt qua nghien ciiu anh hucmg ciia kich thuac hat qu3ng dat hiSm Kon Tum nguyen khai den hieu suat thu nhgn tong oxit dit hidm dupc trinh bay tren hinh 4.
g 65
• 07 0 OB 0.09 D.1D 0 11 0 12 0.13 Kich thii6t: hat. <mm]
Hinh 4. Anh hudng cua kich thuac hgt quang din hieu sudt thu nhdn long oxit ddt hiem
vo V A N T A N - HUYNH THI TU OANH
Tir hinh 4, co tbi nhan thiy ring Idch thuac hgt quang cang nho thi khoi lupng tong oxit dat hiSm thu dupc cang tang va hieu suit thu nhan tong oxit dit hidm cang Ion. Vai kich Ihuoc hat quang <6,074 mm duoc xii ly trong cac didu kien nhu tren thi hieu suit thu nhgn la cao nhit.
Ham lupng cac oxit dit hidm trong san phim dupc xac djnh bing phuang phap XRF (tai phong phat tridn thidi bi va phan tich Vien Khoa hpc Vat lieu, Vien Khoa hpc va Cong nghe Viet Nam) dupc trinh bay a bang 2.
Bang 2. Thdnh phdn hda cua mdu sdn phdm ddf hiem thu dugc tir quang ddt hiem d Kon Tum nguyen khai
stt 1 2 3 4 5 6 7
Cong thirc hoa hoc
CeO, La.Oi YjO, EuiOj NdjOj Sni:Oj ErjO,
Tbanb pban
(%)
39,05 18,34 14,31 3,45 17,39
1,08 0,28
Stt
8 9 10 11 12 13
Cdng thirc b6a boc
Pr.Oi, DyjOj GdjOj SC2O3 BaO ThOj
Tbanb phan
(%)
3.06 0,30 1,20 0,01 0,34 1,15
4. KET LUAN
Lln diu tien nghien cuu thu nhan ting oxit dit hilm ttr qu&ng dit hilm KonTum nguyen khai bing phuang phap axit.
Da khao sat ban chit va ning do cac loai axit: H2SO4, HNO3, HCl, ty le axitrqu^ng, thoi gian phan hiiy quang, kich thuoc hat qu§ng din hieu suit thu nhan tong oxit dat hiem tir quang dit hiem Kon Tum nguyen khai. Vgi ndng do axit H2SO4 IIM, thoi gian phan ling 150 phit, ty le axifquang = 4:1 (mL/g) Ihi hieu suit thu nhan tong oxit dit hilm dat 84%, la cao hon cac loai axit HNO3 HCl.
San pham tong oxit dat hilm thu dugc chiia diy du cac Ioai oxit dit hilm, cac tap chit Si02, FeiOj, AI2O3... da dugc loai bo hoan toan.
TAI LIEU THAM KHAO
[1] Le Tien Dung - Nguyin Van L|ch - Vu Quang Tien - Tiln Tinh - Nguyin Xuan TUng (1995). Dac diem cuong dp phong xa mat tk va tiem nSng quang phong xa, dat hiem va kun loai Mem khu vuc nam Kon Tum-Buon Ma Thuot Tap chi Bia chdt,
so 228(5-6), u. 23-29. ' [2] Biii Minh Ly - Trin Thj Thanh Van - Ngo Quic Bmi (1994), Phan tioh dinh luong
Uran, Thon va cac nguyen to dat hiem ttong m6t sl mau monazite s Trung Viet Nam. Tap chi Hda hoc, T,32 (2), tr.48-52.
NGHIEN C i m THU NTL^N TONG OXIT D.4T H E M TU QUANG DAT HIEM KON TUM.
[3] Vo Van Tan - Trin Ducrng - Trao Thi Phuong Thao (2012). Xac dinh cac dieu kien toi uu thu nhan long oxyt dat hiem tir monazite Ha TTnh bang phuong phap quy hoach thuc nghiem. Tgp chi Hda hgc vd &ng dung. So 1(11), tr. 1-5.
[4] v e v a n Tan - T r u a n g Thi Cao Vinh (2011). Recovery of the total oxides of the rare earths from monazit in Quang N a m . Tap chi Khoa hoc - Dgi hgc Hue, Tgp 69, S6 6, tr. 101-106.
[5] V 3 Van Tan - V6 Quang Mai (2010). Nghien cuu thiiy luyen monazit Quang Tri thu tdng oxit dat hidm. Tap chi Hoa hgc, T. 48(4A), tr. 470-474.
[6] V 6 Van Tan - Vu Hoang Thanh (2006). Nghien cuu thu nhan t6ng oxit dat hiem tu monazit Binh Dinh. Tgp chi hoa hgc vd Ung dung. So 5(53), tr. 41-44.
[7] Vo Van Tan (2004). Nghien cuu thu tong oxyt dSt hidm tii monazit TT-Hue bang phuang phap kiem a ap suit cao. Tgp chi Hda hgc, T. 42(4), tr. 422-425.
Title: RECOVERY OF THE TOTAL OXIDES OF THE RARE EARTHS FROM THE CRUDE RARE EARTHS ORE IN KONTUM BY THE ACID METHOD
A b s t r a c t : The recovery of the total oxides of the rare earths from the cmde rare earths ore in Kon Turn by the acid H2SO4, HNO3, HCl have been studied. It was found that the recovery of the total oxides of the rare earths reching high up should be carried out under the following conditions: I I M H i S 0 4 with in 150 minutes at the boil temperature of mixture, the ratio of acid/ore = 4:1 (mL/g) and ore size <0.125 mm.
PGS. TS. V 6 VAN TAN
Khoa Hoa hoc, Tnrong DHSP - Dsii h9c HuS DT: 0903.253.794, Email: [email protected] H U Y N H THI TU OANH
Hpc vien cao hoc, Trucrng Dai hoc Su pham - Dai hoc Hue DT: 0935.271.221, Email: [email protected]
