CN116854132A - 一种深度净化制备高品质焦锑酸钠的方法 - Google Patents
一种深度净化制备高品质焦锑酸钠的方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 55
- CIWAOCMKRKRDME-UHFFFAOYSA-N tetrasodium dioxido-oxo-stibonatooxy-lambda5-stibane Chemical compound [Na+].[Na+].[Na+].[Na+].[O-][Sb]([O-])(=O)O[Sb]([O-])([O-])=O CIWAOCMKRKRDME-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000746 purification Methods 0.000 title claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000010931 gold Substances 0.000 claims abstract description 53
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052737 gold Inorganic materials 0.000 claims abstract description 51
- 229910052742 iron Inorganic materials 0.000 claims abstract description 46
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 41
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000002386 leaching Methods 0.000 claims abstract description 38
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 238000003828 vacuum filtration Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 4
- YPMOSINXXHVZIL-UHFFFAOYSA-N sulfanylideneantimony Chemical compound [Sb]=S YPMOSINXXHVZIL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- BJIQCYSMVVESCD-UHFFFAOYSA-N [Sb]([S-])([O-])[O-].[Na+].[Na+].[Na+] Chemical compound [Sb]([S-])([O-])[O-].[Na+].[Na+].[Na+] BJIQCYSMVVESCD-UHFFFAOYSA-N 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 6
- 229940079101 sodium sulfide Drugs 0.000 description 15
- ZGHLCBJZQLNUAZ-UHFFFAOYSA-N sodium sulfide nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[S-2] ZGHLCBJZQLNUAZ-UHFFFAOYSA-N 0.000 description 15
- 239000000047 product Substances 0.000 description 13
- 229910052785 arsenic Inorganic materials 0.000 description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 5
- 238000004070 electrodeposition Methods 0.000 description 5
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- MJLGNAGLHAQFHV-UHFFFAOYSA-N arsenopyrite Chemical compound [S-2].[Fe+3].[As-] MJLGNAGLHAQFHV-UHFFFAOYSA-N 0.000 description 2
- 229910052964 arsenopyrite Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000001627 detrimental effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
- 229910052683 pyrite Inorganic materials 0.000 description 2
- 239000011028 pyrite Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 description 2
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 150000001463 antimony compounds Chemical class 0.000 description 1
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- MXZVHYUSLJAVOE-UHFFFAOYSA-N gold(3+);tricyanide Chemical compound [Au+3].N#[C-].N#[C-].N#[C-] MXZVHYUSLJAVOE-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
一种深度净化制备高品质焦锑酸钠的方法,含锑难处理金矿在硫化钠溶液中浸出,使锑以硫代亚锑酸钠形式进入溶液;向浸出液中加入含锑难处理金矿初步除铁,使大部分配合溶解的铁析出;向初步除铁后液中加入活性炭深度除铁,使溶液中残余的铁被吸附脱除;深度除铁后液在高温下通入氧气氧化产出焦锑酸钠产品。本发明的实质是采用初步除铁和活性炭深度除铁两个过程实现了浸出液中铁的彻底脱除,这两段净化除杂过程共同作用,实现了从含锑难处理金矿制备高品质焦锑酸钠产品的目的。
Description
技术领域
本发明涉及冶金领域中湿法冶金过程,特别是采用深度净化方式制备高品质焦锑酸钠的湿法冶金方法。
背景技术
黄金是稀缺的战略性金属,广泛应用于黄金饰品、货币储备和高科技产业。2018年我国的黄金产量为401吨,大约1/3以上产自难处理金矿,随着优质资源的日益消耗,这一比例仍在不断增加。难处理金矿,又称难浸金矿或顽固金矿,它是指即使经过细磨金的氰化浸出率仍然低于80%的矿石,主要有微粒包裹金矿、含铜金矿、含锑金矿、含碳金矿和含碲金矿等。
难处理金矿在氰化法提金之前必须进行预处理,以打开包裹或提升后续金浸出率。目前工业上应用最广泛的难处理金矿预处理方法主要有两段焙烧法、加压氧化法和细菌氧化法。两段焙烧方法是将含砷难处理金矿在两段沸腾炉中焙烧,使砷和硫被氧化形成As2O3和SO2挥发,生成多孔的焙砂。该方法具有工艺简单和处理成本低的优点,得到了广泛应用。加压氧化法是指在高温高压酸性并有氧的情况下,黄铁矿和毒砂被氧化分解,从而使被包裹的金暴露出来。该方法具有处理时间短、金浸出率高和对有害金属敏感性低等优点。细菌氧化法是指通过细菌作用氧化黄铁矿和毒砂,使包裹金充分暴露。该方法具有工艺简单和环境友好的优点。
含锑难处理金矿是一种重要的金矿资源,但是锑对上述预处理方法均有不利影响。在两段焙烧过程中锑易于形成低熔点化合物,对金形成二次包裹,从而导致金的氰化浸出率下降。在加压氧化和生物氧化预处理过程中,部分锑化合物会包覆金矿石表面,阻碍预处理过程和氰化过程的进行。
因此,含锑难处理金矿在进行预处理之前必须完全脱除锑。国内外就关于从含锑难处理金矿中脱除锑进行了大量的研究,工业上通常采用湿法冶金方法选择性脱除锑,根据浸出剂的不同可以分为酸性氯化物体系和碱性硫化钠体系两种。
含锑难处理金矿在酸性氯化物体系浸出锑,其实质是辉锑矿在盐酸溶液中加入氧化剂氧化浸出,使锑以SbCl3形式进入浸出液,选用的氧化剂有Cl2、FeCl3、SbCl5和H2O2等,由于三价锑易于水解的特性,浸出过程需维持较高的氯离子浓度和酸度。从酸性氯化锑溶液中回收锑主要有水解、置换、干馏和电积等方法。根据酸性氯化物体系回收方法的不同,主要的工艺有:氯化浸出-水解工艺、氯化浸出-干馏工艺和氯化浸出-电积工艺等。酸性氧化浸出过程具有锑浸出率高的优点,但是存在试剂消耗大、金溶解损失、设备腐蚀、操作环境差和成本高等缺点。同时,砷和铁均会有不同程度的溶解,给溶液净化和后续提纯带来了很大难度,这些缺点限制了其工业应用。
含锑难处理金矿在硫化钠体系浸出锑,是基于含锑难处理金矿中锑主要以辉锑矿物相存在,使锑以硫代亚锑酸钠形式溶解进入溶液。该方法具有浸出率高和选择性好的优点。从硫代亚锑酸钠的溶液中回收锑的方法主要有中和沉淀法、置换法、电积法和空气氧化法等,这些从硫代亚锑酸钠溶液中回收锑的方法各有利弊,其中空气氧化法和电积法均已经应用于工业实践。
然而,含锑难处理金矿在硫化钠浸出时,会有部分铁等杂质溶解进入浸出液,在后续从浸出液提取锑时,溶液中的铁会影响产品质量,如硫代亚锑酸钠溶液电积时铁会进入阴极,使得阴极锑含铁远远超标。硫代亚锑酸钠采用空气氧化或加压氧化时,铁会沉淀进入焦锑酸钠,使得原本白色的焦锑酸钠产品呈现砖红色,严重影响产品形貌与质量。
有文献指出硫代亚锑酸钠浸出液经过静置48h,可以使大部分铁会以硫化亚铁形式沉淀出来,然而,一方面长时间的静置不利于工业生产的连续性,另一方面溶液静置过程中部分锑也会以硫代亚锑酸钠形式沉淀出来,这对后续锑的回收非常不利。基于此,针对含锑难处理金矿硫化钠浸出液中铁的不利影响,提出一种深度净化制备高品质焦锑酸钠的方法。
发明内容
为了克服难处理金矿硫化钠浸出液中铁的不利影响,本发明提出一种采用两段除铁和高温氧化相结合的方法制备焦锑酸钠,且杂质脱除率高、处理成本低、环境友好、操作简单的湿法冶金方法。
为达到上述目的本发明采用的技术方案是:首先含锑难处理金矿在硫化钠溶液中浸出,使大部分锑和少量的铁和砷溶解进入溶液,液固分离后得到浸出液。其次向浸出液中加入含硫化锑矿物初步除铁,使大部分配合溶解的铁析出,液固分离后得到初步除铁后液。再次向初步除铁后液中加入活性炭深度除铁,使溶液中残余的铁被吸附脱除,液固分离后得到深度除铁后液。最后,深度除铁后液在高温下通入氧气氧化产出焦锑酸钠产品。本发明的实质是采用初步除铁和深度除铁两个过程实现了浸出液中铁的彻底脱除,这两段净化除杂过程共同作用,实现了浸出液净化除杂和制备高品质焦锑酸钠产品的预期效果。
具体的工艺过程和工艺参数如下:
1硫化钠浸出
含锑难处理金矿在硫化钠溶液中浸出锑。配制浓度为10g/L的氢氧化钠溶液,按液体体积L与固体重量kg之比2.0∶1加入含锑难处理金矿,再按硫化锑与硫化钠摩尔比3.3∶1加入硫化钠,控制温度25℃搅拌反应30min,采用真空抽滤方式液固分离,浸出液送后续初步除铁工序,浸出渣用于提取金。
2初步除铁
向浸出液中加入含锑难处理金矿初步除铁。向浸出液中加入硫化钠浸出过程使用矿量15%的含锑难处理金矿,控制温度25℃搅拌反应120min,采用真空抽滤方式液固分离,初步除铁后液送深度除铁工序,初步除铁渣返回浸出。
3深度除铁
向初步除铁后液中加入活性炭吸附深度除铁。向初步除铁后液中加入活性炭,按照每升初步除铁后液加入活性炭30g,控制温度25℃搅拌反应120min,采用真空抽滤方式液固分离,深度除铁后液送高温加压氧化,深度除铁渣洗涤后循环使用。
4高温加压氧化
深度除铁后液在高温下通入氧气氧化产出焦锑酸钠产品。深度除铁后液加入高压反应釜中,通入氧气并控制压力1.2MPa,控制温度120℃搅拌反应360min,采用真空抽滤方式液固分离,沉淀产物洗涤烘干后为高品质焦锑酸钠产品。
本发明适用于处理含锑难处理金矿,其主要成分范围以重量百分比计为(%):Au10~100g/t、As1.0~10.0、Sb1.0~15.0、S8.0~28.0和Fe10.0~35.0。
所述硫化钠和氢氧化钠均为分析纯试剂。
本发明与传统含锑难处理金矿在硫化钠体系制备焦锑酸钠的方法比较,有以下优点:1该方法采用初步除铁和深度除铁两个过程实现了浸出液中铁的彻底脱除,最终经过加压氧化制备了合格的焦锑酸钠产品,实现了浸出液净化除杂和制备高品质焦锑酸钠产品的双重目的。2、浸出液经过两段除铁过程铁的脱除率大于99.0%以上。3、深度除铁后液经过高温加压氧化产出高品质焦锑酸钠产品;4、本发明具有工艺过程简单、技术指标稳定、劳动强度小和生产成本低等优点。
附图说明
图1:本发明工艺流程示意图。
具体实施方式:
实施例1:
含锑难处理金矿原料主要成分以质量百分比计分别为(%):Au30g/t、Sb3.92、As7.67、Fe16.71和S9.26。氢氧化钠、九水合硫化钠均为分析纯试剂,氢氧化钠质量百分数不小于96%,九水合硫化钠质量百分数不小于98%。配制浓度为10g/L的氢氧化钠溶液,按液体体积L与固体重量kg之比2.0∶1加入含锑难处理金矿,再按硫化锑与硫化钠摩尔比3.3∶1加入硫化钠,控制温度25℃搅拌反应30min,采用真空抽滤方式液固分离。向浸出液中加入硫化钠浸出过程使用矿量15%的含锑难处理金矿,控制温度25℃搅拌反应120min,采用真空抽滤方式液固分离。向初步除铁后液中加入活性炭,按照每升初步除铁后液加入活性炭30g,控制温度25℃搅拌反应120min,采用真空抽滤方式液固分离。深度除铁后液加入高压反应釜中,通入氧气并控制压力1.2MPa,控制温度120℃搅拌反应360min,采用真空抽滤方式液固分离,沉淀产物洗涤烘干后为高品质焦锑酸钠产品,锑含量为48.76%,铁和砷含量均小于0.03%。
Claims (1)
1.一种深度净化制备高品质焦锑酸钠的方法,其特征在于包括以下步骤:
(1)硫化钠浸出
配制浓度为10g/L的氢氧化钠溶液,按液体体积L与固体重量kg之比2.0∶1加入含锑难处理金矿,再按硫化锑与硫化钠摩尔比2.7-3.3∶1加入硫化钠,控制温度25℃搅拌反应30min,采用真空抽滤方式进行液固分离,浸出液送初步除铁工序,浸出渣用于提取金;
(2)初步除铁
向浸出液中加入硫化钠浸出过程使用矿量15%的含锑难处理金矿,控制温度25℃搅拌反应120min,采用真空抽滤方式液固分离,初步除铁后液送深度除铁工序,初步除铁渣返回浸出;
(3)深度除铁
向初步除铁后液中加入活性炭,按照每升初步除铁后液加入活性炭30g,控制温度25℃搅拌反应120min,采用真空抽滤方式液固分离,深度除铁后液送高温加压氧化,深度除铁渣洗涤后循环使用;
(4)高温加压氧化
深度除铁后液加入高压反应釜中,通入氧气并控制压力1.2MPa,控制温度120℃搅拌反应360min,采用真空抽滤方式液固分离,沉淀产物洗涤烘干后为高品质焦锑酸钠产品。
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