CN1165056A - Synthetic technology for rare-earth mineral collector - Google Patents
Synthetic technology for rare-earth mineral collector Download PDFInfo
- Publication number
- CN1165056A CN1165056A CN 96107505 CN96107505A CN1165056A CN 1165056 A CN1165056 A CN 1165056A CN 96107505 CN96107505 CN 96107505 CN 96107505 A CN96107505 A CN 96107505A CN 1165056 A CN1165056 A CN 1165056A
- Authority
- CN
- China
- Prior art keywords
- rare
- acid
- agent
- hydroxyl
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A process for synthesizing the trapping agent, H205-2-hydroxyl3-naphthymethyl hydroxamic acid, for rare-earth ore includes such steps as sulfonating naphthalene to obtain 2-hydroxyl3-naphthylformic acid as raw material, acylating reaction on methanol as acylating agent, and condensation reaction with oxyammonia in alkaline medium. Said trapping agent features simple synthesizing process, and can be used in floatation to directly trap rare-earth ore concentrate with the grade higher than 50% from raw, tailing or coarse rare-earth ore with metallic recovery rate higher than 80% and no need of toxic sodium fluorosilicate as activating agent.
Description
The present invention relates to a kind of synthesis technique of rare-earth mineral collector, be particularly suitable for rare-earth mineral collector H
2O5Synthetic, belong to the synthetic technology of beneficiation reagent.
Rare-earth minerals such as bastnaesite, monazite are reclaimed in ore dressing from the complex ore of ores containing rare earths thing, must separate effectively with mineral such as the fluorite of association, calcite, barite, apatite.Yet because mineral composition complexity, granularity embedding cloth are tiny, adopting method for floating to reclaim rare-earth mineral is the comparison difficulty.In the last few years, dresser author was devoted to seek a kind of high-efficient collecting agent of rare-earth mineral always, to replace the relatively poor fatty acid collecting agent of selectivity.
A kind of N-hydroxyl cycloalkanoimide (cycloalkyl hydroxamic acid) rare earth catching agent that Baotou tombar thite institute succeeds in developing is used (being published in the 64th page of " rare earth " first phase nineteen eighty-three) aborning.The abundant PETROLEUM PROCESSING of this kind collecting agent utilization is paid product-aphthenic acids and is raw material, through chloride, forms with the hydroxylamine condensation in alkaline medium.Being used to sort rare-earth mineral is the very strong floating agent of a kind of collecting ability, but because poor selectivity for from the high slightly sample ore of impurity content, sorts high-grade (REO＞50%) rare earth ore concentrate, very difficult.In addition, also need add poisonous prodan in the ore dressing process as rare earths activator, both contaminated environment was harmful to health again.
It is moderate to the objective of the invention is to develop a kind of collecting ability, and the rare-earth mineral collector that selectivity is good is to be adapted to the flotation of the lower difficult ore dressing sample of content of rare earth.
The present invention is achieved in that be raw material with naphthalene through the synthetic 2-hydroxyl 3-naphthoic acid that obtains of sulfonation; methyl alcohol is acylation agent; at room temperature carry out acylation reaction to 50～80 ℃; then in alkaline medium; 50～60 ℃ of following and hydroxylamine condensation reactions; to be cooledly add diluted acid to the room temperature and transfer to PH5～6, leave standstill, separate promptly getting rare collecting agent H of going up
2O5Product, i.e. 2-hydroxyl 3-naphthalene formhydroxamic acid, its molecular structural formula is:
Below in conjunction with accompanying drawing the present invention is further described:
Accompanying drawing is a synthesis process flow diagram of the present invention.
Get take naphthalene through sulfonation synthetic 2-hydroxyl 3-naphthoic acid [1] as raw material, methyl alcohol [2] is acylation agent, is warming up to 50～80 ℃ after at room temperature stirring 20～30 minute second month in a season, carries out the acyl group reaction, 10～12 hours reaction time;
(2) hydroxylamine [3] is put into condensation reactor, add again alkali solution [4] after being dissolved in water, then the acyl group product is added in the condensation reactor in batches, under 50～60 ℃, carry out condensation reaction, reacted 4～5 hours, be cooled to room temperature. At last condensation reaction products is put into and left standstill groove, add diluted acid [5] and transfer to PH5～6, leave standstill, separate namely getting rare earth catching agent H2O5-2-hydroxyl 3-naphthalene first hydroxamic acid product.
The present invention compares with N---hydroxyl cycloalkanoimide, and synthesis technique is simple, stable. Prove that through beneficiation test it is selectively good to swim, unit consumption of medicine is few, and rare earth concentrate grade and rare earth yield are high; Get rid of simultaneously poisonous prodan as rare earths activator, prevented environmental pollution, be of value to health.
Embodiment 1:
Take by weighing 2-hydroxyl 3-naphthoic acid 50 grams, put into 1000 milliliters of three-necked bottles, add 100 milliliters of methyl alcohol, at room temperature stir after 20 minutes and be warming up to 60～70 ℃, reacted 10 hours.In 1000 milliliters of three-necked bottles, put into hydroxylamine 26 gram, add 300 milliliters of dissolvings of water after, add 80 milliliters of sodium hydroxide solutions (concentration 30%) again, then the acylation reaction product is joined in the hydroxylamine alkalescence concentration, in 50 ℃ of reactions 4 hours down, be cooled to room temperature.Move at last to leave standstill and add diluted acid in the groove and transfer to PH5～6, leave standstill, separate and obtain rare earth catching agent H
2O5150 grams (moisture 65～70%).
Embodiment 2:
In 1000 liter enamel reaction stills, put into methyl alcohol 800 liters, under stirring state, slowly add 160 kilograms of 2-hydroxyl 3-naphthoic acids, normal temperature stirs after 30 minutes down, is warming up to 60～70 ℃, 12 hours reaction time.Put into 80 kilograms of hydroxylamines in 3000 liter reactors, water dissolves it, adds sodium hydrate aqueous solution (concentration 30%) 250 liters again, adds the product of above-mentioned acylation reaction then in batches, reacts 5 hours down at 60 ℃, is cooled to room temperature.Add diluted acid and transfer to PH5～6, leave standstill, separate H
2O5480 kilograms of products (moisture 65～70%).
Get H
2O5Ammoniacal liquor with 20～25% carries out aminating reaction, is made into the aqueous solution of 2% concentration then, carries out the flotation contrast test with itself and N-hydroxyl cycloalkanoimide, and its result is as shown in the table:
| Collecting agent | Rare earth productive rate (%) | Rare earth grade (%) | Rare earth yield (%) | Unit consumption of medicine kilogram/ton | Expense unit/ton | Remarks |
| H 2O5 | ??35.20 | ??59.63 | ????91.57 | ????5.17 | ?31.72 | |
| N-hydroxyl cycloalkanoimide | ??34.51 | ??51.23 | ????73.36 | ????9.86 | ?36.18 | Adopt prodan to make rare earths activator |
Claims (2)
1. the synthesis technique of a rare-earth mineral collector is finished by acylation reaction with two steps of hydroxylamine condensation reaction, it is characterized in that:
(1) be raw material with 2-hydroxyl 3-naphthoic acid, methyl alcohol is acylation agent, at room temperature stirs after 20～30 minutes and is warming up to 50～80 ℃, reacts 10～12 hours;
(2) (1) reactant is added in the hydroxylamine alkaline solution of becoming reconciled in giving earlier,, be cooled to and add diluted acid after the room temperature and transfer to PH5～6, leave standstill, separate promptly getting rare earth catching agent H in 50～60 ℃ of reactions 4～5 hours down
2O5Product.
2. synthesis technique according to claim 1 is characterized in that said rare earth catching agent H is that to adopt naphthalene be raw material through the synthetic hydroxamic acid of sulfonation, the 2-hydroxyl 3-naphthalene first isoxime acid that makes through acyl groupization and condensation reaction again, and its molecular structural formula is:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96107505A CN1068247C (en) | 1996-05-09 | 1996-05-09 | Synthetic technology for rare-earth mineral collector |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96107505A CN1068247C (en) | 1996-05-09 | 1996-05-09 | Synthetic technology for rare-earth mineral collector |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1165056A true CN1165056A (en) | 1997-11-19 |
| CN1068247C CN1068247C (en) | 2001-07-11 |
Family
ID=5119618
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96107505A Expired - Fee Related CN1068247C (en) | 1996-05-09 | 1996-05-09 | Synthetic technology for rare-earth mineral collector |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1068247C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002066168A1 (en) * | 2001-02-19 | 2002-08-29 | Ausmelt Limited | Improvements in or relating to flotation |
| CN101524670A (en) * | 2009-04-03 | 2009-09-09 | 包头市林峰稀土化工有限公司 | Rare earth collector |
| CN102069037A (en) * | 2011-01-20 | 2011-05-25 | 西安建筑科技大学 | Composite hydrocarbon oil molybdenum flotation collecting agent and preparation method thereof |
| CN104549719A (en) * | 2007-01-05 | 2015-04-29 | 氰特技术公司 | Process for the removal of impurities from carbonate minerals |
| CN106008266A (en) * | 2016-05-20 | 2016-10-12 | 中国地质科学院矿产综合利用研究所 | Green preparation method of hydroximic acid rare earth flotation reagent |
| CN106040436A (en) * | 2016-05-27 | 2016-10-26 | 中国地质科学院矿产综合利用研究所 | Low-temperature-resistant rare earth ore flotation collector, preparation method and application thereof |
| CN108636616A (en) * | 2018-05-22 | 2018-10-12 | 中南大学 | Inhibit the inhibitor and its application method of vulcanization M in a kind of floatation process |
| CN109482360A (en) * | 2018-11-20 | 2019-03-19 | 中国地质科学院矿产综合利用研究所 | Mineral processing technology of rare earth, fluorite and barite associated ore |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1012465B (en) * | 1987-05-07 | 1991-05-01 | 浙江大学 | Medical impulse laser unit |
-
1996
- 1996-05-09 CN CN96107505A patent/CN1068247C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002066168A1 (en) * | 2001-02-19 | 2002-08-29 | Ausmelt Limited | Improvements in or relating to flotation |
| CN104549719A (en) * | 2007-01-05 | 2015-04-29 | 氰特技术公司 | Process for the removal of impurities from carbonate minerals |
| CN101524670A (en) * | 2009-04-03 | 2009-09-09 | 包头市林峰稀土化工有限公司 | Rare earth collector |
| CN101524670B (en) * | 2009-04-03 | 2013-07-24 | 包头市林峰稀土化工有限公司 | Rare earth collector |
| CN102069037A (en) * | 2011-01-20 | 2011-05-25 | 西安建筑科技大学 | Composite hydrocarbon oil molybdenum flotation collecting agent and preparation method thereof |
| CN102069037B (en) * | 2011-01-20 | 2012-09-05 | 西安建筑科技大学 | Composite hydrocarbon oil molybdenum flotation collecting agent and preparation method thereof |
| CN106008266A (en) * | 2016-05-20 | 2016-10-12 | 中国地质科学院矿产综合利用研究所 | Green preparation method of hydroximic acid rare earth flotation reagent |
| CN106040436A (en) * | 2016-05-27 | 2016-10-26 | 中国地质科学院矿产综合利用研究所 | Low-temperature-resistant rare earth ore flotation collector, preparation method and application thereof |
| CN106040436B (en) * | 2016-05-27 | 2019-01-04 | 中国地质科学院矿产综合利用研究所 | Low-temperature-resistant rare earth ore flotation collector, preparation method and application thereof |
| CN108636616A (en) * | 2018-05-22 | 2018-10-12 | 中南大学 | Inhibit the inhibitor and its application method of vulcanization M in a kind of floatation process |
| CN108636616B (en) * | 2018-05-22 | 2019-10-08 | 中南大学 | Inhibit the inhibitor and its application method of vulcanization M in a kind of floatation process |
| CN109482360A (en) * | 2018-11-20 | 2019-03-19 | 中国地质科学院矿产综合利用研究所 | Mineral processing technology of rare earth, fluorite and barite associated ore |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1068247C (en) | 2001-07-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1040029C (en) | Hydrometallurgical process for the recovery of precious metal values from precious metal ores with thiosulfate lixiviant | |
| US4752332A (en) | Treating manganese-containing ores with a metal sulfide | |
| CN108722677B (en) | A kind of O- alkyl-S- hydroxyalkyl xanthate collecting agent and its preparation and application | |
| CN110142143B (en) | Collecting system prepared from W/O/W multiphase emulsion and preparation method and application thereof | |
| CN1068247C (en) | Synthetic technology for rare-earth mineral collector | |
| CA2012971C (en) | Recovery of metal values from ores | |
| CN1327012C (en) | Wet-method for leaching of low-grade high-alkali hybrid copper ore, nickel ore and zinc ore | |
| CN110408777A (en) | A kind of method of fatty acid extracting metals ion | |
| CN108017374B (en) | Method and device for comprehensively utilizing cyanide tailings | |
| CN111690810B (en) | Red mud recycling-soil treatment method | |
| CN104801426B (en) | A kind of Schiff bases caproate mineral floating collecting agent and its preparation method and application | |
| CN104694736B (en) | Calcium roasting floatation separation method for bastnaesite | |
| CN86100710A (en) | A kind of synthesis technique of rare earth catching agent | |
| CN108452949A (en) | A kind of floatation process of ilmenite or bastnaesite | |
| CN113441282A (en) | Application of sodium glucoheptonate in flotation separation of tin and iron | |
| CN1037586C (en) | Method for preparation of collecting agent of oxidized ore | |
| US4466886A (en) | Froth flotation method for recovering minerals | |
| Borges et al. | Solvent extraction of gallium with Kelex 100 from Brazilian weak sodium aluminate solution | |
| CN108793227A (en) | A method of producing nano zine oxide using containing zinc ore crude | |
| CN100348747C (en) | Cerium reverse extracting method from cerium-carrying fluoric organic phase and cerium purifying method | |
| CN115385808B (en) | Preparation method of flotation agent for boron separation and flotation agent | |
| GB2204507A (en) | Method of concentration of difficult-to-concentrate oxidized copper ore | |
| CN117563782A (en) | Molybdenite organic small molecule floatation inhibitor, preparation method and application thereof | |
| CN106947861A (en) | A kind of continuous device for making of rare earth compound precipitation | |
| WO2023191737A1 (en) | A method for obtaining zn and pb metals from zn-pb ore |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: ZHANGJIAKOU JINYAN CHEMICAL CO., LTD. Free format text: FORMER OWNER: BAOTONG RARE-EARTH RESEARCH ACADEMY, MINISTRY OF METALLURGICAL INDUSTRY Effective date: 20011229 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20011229 Address after: 075000 Gao Qiao, West Bridge, Hebei, Zhangjiakou Patentee after: Zhangjiakou Golden Swallow Chemical Co., Ltd. Address before: 014010 the Inner Mongolia Autonomous Region Baotou Kunqu solidarity Street No. 101 Patentee before: Baotou Rare Earth Research Inst., Ministry of Metallurgical Industry |
|
| C56 | Change in the name or address of the patentee |
Owner name: ZHANGJIAKOU CITY JINKE CHEMICALS CO., LTD. Free format text: FORMER NAME OR ADDRESS: ZHANGJIAKOU JINYAN CHEMICAL CO., LTD. |
|
| CP03 | Change of name, title or address |
Address after: 075000 Gao Qiao, West Bridge, Hebei, Zhangjiakou Patentee after: Zhangjiakou Jinke Chemical Co. Ltd. Address before: 075000 Gao Qiao, West Bridge, Hebei, Zhangjiakou Patentee before: Zhangjiakou Golden Swallow Chemical Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20010711 Termination date: 20150509 |
|
| EXPY | Termination of patent right or utility model |