CN104549768B - Froth flotation cation collecting agent and preparation method thereof - Google Patents
Froth flotation cation collecting agent and preparation method thereof Download PDFInfo
- Publication number
- CN104549768B CN104549768B CN201510051045.6A CN201510051045A CN104549768B CN 104549768 B CN104549768 B CN 104549768B CN 201510051045 A CN201510051045 A CN 201510051045A CN 104549768 B CN104549768 B CN 104549768B
- Authority
- CN
- China
- Prior art keywords
- collecting agent
- cation
- flotation
- preparation
- rock phosphate
- 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.)
- Active
Links
Landscapes
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The invention discloses a froth flotation cation collecting agent and a preparation method thereof, and belongs to the technical field of ore dressing. The froth flotation cation collecting agent consists of the following raw materials in percentage by weight: 15-30% of C12-C18 fatty acids, 5-15% of N-chlorosuccinimide, 20-50% of ether amine, 5-20% of industrial fusel, 2-10% of emulsifier, 1-8% of diesel oil and the balanced water. The sum of the raw materials is 100% in percentage by weight. The preparation method comprises the following steps of performing chlorination on the C12-C18 fatty acids and the N-chlorosuccinimide; adding the industrial fusel, the emulsifier and the diesel oil in the mixture of the C12-C18 fatty acids and the N-chlorosuccinimide; and stirring the mixture uniformly and adding water in the mixture to obtain the froth flotation cation collecting agent. Compared with the conventional collecting agent, the froth flotation cation collecting agent is high in selectivity, high in argillization resistance and stable in performance and is low-temprature-resistant; foams are not tacky and dissipate easily; normal-temperature flotation can be realized; chemical consumption is reduced; and R2O3 in concentrates is greatly reduced.
Description
Technical field
The present invention relates to a kind of rock phosphate in powder flotation cation-collecting agent and preparation method thereof, belong to technical field of beneficiation.
Background technology
Yunnan is the area that a phosphate rock resource enriches, and one of rock phosphate in powder main usess are the lifes of phosphoric acid and high concentration phosphate fertilizer
Produce.However, the rock phosphate in powder rich ore in Yunnan is few, in the majority with the collophane of middle-low grade, in particular with downstream phosphorous chemical industry demand
Increase, rock phosphate in powder is constantly exploited, and rich ore is fewer and feweri, and phosphorus ore head grade constantly declines, and the rock phosphate in powder exploited has to pass through
The feed quality requirements of high-concentration phosphoric acid and Phosphate Fertilizer Industry could be met after beneficiation enrichment.
And using based on reverse flotation de-magging, the floatation process of direct flotation enriched phosphorus more than present phosphate rock floating, these flotation works
Skill all adopts anionic collector.The fatty acid such as commonly used oxidized paraffin wax soap, tall oil and its soaps collecting agent return both at home and abroad
Receive phosphate and carbonate.Due to its poor selectivity, the features such as poor to the adaptability of hard water and flotation at low temperature, 80 years last century
Since generation, develop both at home and abroad successively flotation as sorting one of most effective means of phosphorus ore.At present both at home and abroad to phosphate rock floating
Research is main to include floatation process and floating agent.There is following floating agent, such as both at home and abroad: fatty acid collecting
Agent, amide carboxylic acid's class collecting agent, amphoteric collector, phosphate ester and organic phosphoric acid, cationic amine collecting agent, oxyethylene group compound
Class collecting agent etc..But the poor selectivity due to anion (fatty acid) collecting agent, intolerant to hard water is higher using temperature requirement
And dosing is big, production cost is big, or scent of, the shortcomings of production technology is relative complex, and cation (amine) collecting agent,
Preferably, reagent consumption is little, but more sensitive to shale, and foam is tacky for selectivity, and foam is difficult to froth breaking it is difficult to realize flotation froth defeated
Send, cation-collecting agent is rarely employed in actual production.
Therefore developing a kind of cation-collecting agent applied widely, that selectivity is good, collecting ability is strong, flotation speed is fast is
Very necessary.
Content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provides that a kind of collecting ability is strong, anti-argillization
Ability is strong, low production cost, resistance to hard water, stable in properties, dosing are little, selectivity is good, Environmental Safety and adapt to low temperature
Rock phosphate in powder flotation cation-collecting agent, also provides a kind of preparation method of this collecting agent easy to operate, low cost.
The present invention is achieved through the following technical solutions: a kind of rock phosphate in powder flotation cation-collecting agent, by following masses hundred
The raw material dividing ratio forms:
C12～c18 fatty acid 15～30%, n- chlorosuccinimide 5～15%, ether amines 20～50%, industrial fusel
5～20%, emulsifying agent 2～10%, diesel oil 1～8%, water are surplus, and the summation of said components is 100%.
Described ether amines are one of alkyl ether amine, acyl group ether amines or two kinds.
Described industry fusel is isopropanol, n-butyl alcohol, amylalcohol, alcohol, capryl alcohol, dodecyl alcohol, in myristyl alcohol
A kind of or any two kinds.
Described emulsifying agent is op-10, tween 80 or polyethers.
Another object of the present invention is to providing a kind of preparation method of rock phosphate in powder flotation cation-collecting agent, through following
Each step:
(1) by the material preparation of following mass percent:
C12～c18 fatty acid 15～30%, n- chlorosuccinimide 5～15%, ether amines 20～50%, industrial fusel
5～20%, emulsifying agent 2～10%, diesel oil 1～8%, water are surplus, and the summation of said components is 100%；
(2) fatty acid of the c12～c18 in step (1) and n- chlorosuccinimide are entered at 90～120 DEG C of temperature
Row chlorination 3～5 hours, adds ether amines, and reacts 30～60 minutes at temperature is 80～120 DEG C, is subsequently adding work
Industry fusel, and stirring, adds emulsifying agent and diesel oil, agitated uniformly add water afterwards, obtain the homogeneous viscous solution of microemulsion
Body, as rock phosphate in powder flotation cation-collecting agent.
When the rock phosphate in powder flotation cation-collecting agent that the present invention provides uses, first with water, this cation-collecting agent is diluted to
Mass concentration is 2～5% collecting agent solution, and then collecting agent solution is used as the reverse floatation process except ferrum, aluminum of rock phosphate in powder
In, and the flotation temperature in reverse floatation process controls at 20～30 DEG C.
Advantage and effect that the present invention possesses: c12～c18 fat in the rock phosphate in powder flotation cation-collecting agent that the present invention provides
Fat acid hydrocarbon chain is longer, and hydrophobicity is good, has stronger collecting power；N- chlorosuccinimide can make unsaturated bond conversion in fatty acid
For corresponding saturated bond, thus strengthening its collecting performance；Ether amines are cationic surfactant, act primarily as collecting effect；Industry is miscellaneous
Alcohol plays barbotage；Emulsifying agent acts primarily as fusion, and diesel oil can play the effect reducing foam viscosity；The present invention will be several
Medicament carries out mix homogeneously by particular determination order, can strengthen water solublity, preferably plays drug effect.The cation comparing routine is caught
More preferable, the anti-argillization ability of selectivity of the rock phosphate in powder flotation cation-collecting agent that the receipts agent present invention provides is strong, stable in properties, foam
Not tacky, foam easily dissipates, and low temperature resistant, achievable normal temperature flotation, and its reagent consumption is low, and the reagent consumption of raw ore per ton is
100～250g/t, using the present invention cation-collecting agent after rock phosphate in powder flotation phosphorous recovery reach more than 85%, r2o3Removal efficiency
Reach more than 60% (r herein2o3It is sesquichloride, refer to ferrum oxide, aluminium oxide), after making flotation, gained phosphorus concentrate grade improves 4%
More than.Compared to conventional anion collectors application in rock phosphate in powder flotation, significantly reduce the r in concentrate2o3, and medicament disappears
Consumption is low.
Specific embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
(1) by the material preparation of following mass percent:
C12 fatty acid 25%, n- chlorosuccinimide 15%, alkyl ether amine 20%, capryl alcohol and dodecyl alcohol 15%,
Emulsifying agent (op-10) 6%, diesel oil 8%, water are 11%；
(2) fatty acid of the c12 in step (1) and n- chlorosuccinimide are put in reactor in 120 DEG C of temperature
Under carry out chlorination 4 hours, add ether amines, and temperature be 100 DEG C at react 45 minutes, be subsequently adding industrial fusel,
And stir, add emulsifying agent and diesel oil, agitated uniformly add water afterwards, obtain the homogeneous thick liquid of microemulsion, as
Rock phosphate in powder flotation cation-collecting agent.
When gained rock phosphate in powder flotation cation-collecting agent uses, first with water, this cation-collecting agent is diluted to mass concentration
Collecting agent solution for 3%, then by collecting agent solution be used as Yunnan Haikou rock phosphate in powder except de- in ferrum, the reverse floatation process of aluminum
Go out sesquichloride thus the flotation temperature carrying in phosphorus, and reverse floatation process controls at 25 DEG C.
Result is as follows, and head grade is 21.08%, r2o3For 5.49%, after flotation phosphorus concentrate grade is 25.69%,
r2o3For 2.46%, the response rate 91.01%, r2o3Removal efficiency 61.75%.
Embodiment 2
(1) by the material preparation of following mass percent:
C16 fatty acid 30%, n- chlorosuccinimide 5%, acyl group ether amines 25%, n-butyl alcohol and myristyl alcohol 20%,
Emulsifying agent (tween 80) 10%, diesel oil 5%, water 5%；
(2) fatty acid of the c16 in step (1) and n- chlorosuccinimide are put in reactor at 90 DEG C of temperature
Carry out chlorination 3 hours, add ether amines, and react 30 minutes at temperature is 80 DEG C, be subsequently adding industrial fusel, and stir
Mix uniformly, add emulsifying agent and diesel oil, agitated uniformly add water afterwards, obtain the homogeneous thick liquid of microemulsion, as phosphorus ore
Stone flotation cation-collecting agent.
When gained rock phosphate in powder flotation cation-collecting agent uses, first with water, this cation-collecting agent is diluted to mass concentration
Collecting agent solution for 2%, then by collecting agent solution be used as rock phosphate in powder except in ferrum, the reverse floatation process of aluminum, and reverse flotation
Flotation temperature in technique controls at 20 DEG C.
Result is as follows, and head grade is 20.47%, r2o3For 5.78%, after flotation phosphorus concentrate grade is 24.19%,
r2o3For 2.89%, the response rate 90.15%, r2o3Removal efficiency 57.68%.
Embodiment 3
(1) by the material preparation of following mass percent:
C18 fatty acid 15%, n- chlorosuccinimide 8%, ether amines 50%, alcohol 5%, emulsifying agent (polyethers) 2%, bavin
Oil 1%, water are 19%；
Wherein, ether amines are alkyl ether amine and acyl group ether amines；
(2) fatty acid of the c18 in step (1) and n- chlorosuccinimide are put in reactor in 100 DEG C of temperature
Under carry out chlorination 5 hours, add ether amines, and temperature be 120 DEG C at react 60 minutes, be subsequently adding industrial fusel,
And stir, add emulsifying agent and diesel oil, agitated uniformly add water afterwards, obtain the homogeneous thick liquid of microemulsion, as
Rock phosphate in powder flotation cation-collecting agent.
When gained rock phosphate in powder flotation cation-collecting agent uses, first with water, this cation-collecting agent is diluted to mass concentration
Collecting agent solution for 5%, then by collecting agent solution be used as rock phosphate in powder except in ferrum, the reverse floatation process of aluminum, and reverse flotation
Flotation temperature in technique controls at 30 DEG C.
Result is as follows, and head grade is 18.86%, r2o3For 6.75%, after flotation phosphorus concentrate grade is 24.69%,
r2o3For 3.04%, the response rate 85.18%, r2o3Removal efficiency 65.60%.
Embodiment 4
(1) by the material preparation of following mass percent:
C15 fatty acid 20%, n- chlorosuccinimide 12%, alkyl ether amine 35%, isopropanol and amylalcohol 10%, emulsifying
Agent (op-10) 5%, diesel oil 3%, water are 5%；
(2) fatty acid of the c15 in step (1) and n- chlorosuccinimide are put in reactor in 120 DEG C of temperature
Under carry out chlorination 4 hours, add ether amines, and temperature be 100 DEG C at react 45 minutes, be subsequently adding industrial fusel,
And stir, add emulsifying agent and diesel oil, agitated uniformly add water afterwards, obtain the homogeneous thick liquid of microemulsion, as
Rock phosphate in powder flotation cation-collecting agent.
When gained rock phosphate in powder flotation cation-collecting agent uses, first with water, this cation-collecting agent is diluted to mass concentration
Collecting agent solution for 3%, then by collecting agent solution be used as Yunnan Haikou rock phosphate in powder except de- in ferrum, the reverse floatation process of aluminum
Go out sesquichloride thus the flotation temperature carrying in phosphorus, and reverse floatation process controls at 25 DEG C.
Result is as follows, and head grade is 20.34%, r2o3For 5.52%, after flotation phosphorus concentrate grade is 25.14%,
r2o3For 2.88%, the response rate 91.01%, r2o3Removal efficiency 57.77%.
Claims (5)
1. a kind of preparation method of rock phosphate in powder flotation cation-collecting agent is it is characterised in that through following each step:
(1) by the material preparation of following mass percent:
C12～c18 fatty acid 15～30%, n- chlorosuccinimide 5～15%, ether amines 20～50%, industrial fusel 5～
20%th, emulsifying agent 2～10%, diesel oil 1～8%, water are surplus, and the summation of said components is 100%；
(2) fatty acid of the c12～c18 in step (1) and n- chlorosuccinimide are carried out chlorine at 90～120 DEG C of temperature
Generation reaction 3～5 hours, adds ether amines, and reacts 30～60 minutes at temperature is 80～120 DEG C, is subsequently adding industry miscellaneous
Alcohol, and stirring, adds emulsifying agent and diesel oil, agitated uniformly adds water, as rock phosphate in powder flotation cation collecting afterwards
Agent.
2. rock phosphate in powder flotation cation-collecting agent according to claim 1 preparation method it is characterised in that: described ether amines
For one of alkyl ether amine, acyl group ether amines or two kinds.
3. rock phosphate in powder flotation cation-collecting agent according to claim 1 preparation method it is characterised in that: described industry
Fusel is isopropanol, n-butyl alcohol, amylalcohol, one of alcohol, capryl alcohol, dodecyl alcohol, myristyl alcohol or any two kinds.
4. rock phosphate in powder flotation cation-collecting agent according to claim 1 preparation method it is characterised in that: described emulsifying
Agent is op-10, tween 80 or polyethers.
5. the rock phosphate in powder flotation cation-collecting agent that preparation method according to claim 1 obtains, when using, first uses water
This cation-collecting agent is diluted to the collecting agent solution that mass concentration is 2～5%, then collecting agent solution is used as rock phosphate in powder
Except in ferrum, the reverse floatation process of aluminum, and the flotation temperature in reverse floatation process controls at 20～30 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510051045.6A CN104549768B (en) | 2015-02-02 | 2015-02-02 | Froth flotation cation collecting agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510051045.6A CN104549768B (en) | 2015-02-02 | 2015-02-02 | Froth flotation cation collecting agent and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104549768A CN104549768A (en) | 2015-04-29 |
| CN104549768B true CN104549768B (en) | 2017-01-18 |
Family
ID=53067464
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510051045.6A Active CN104549768B (en) | 2015-02-02 | 2015-02-02 | Froth flotation cation collecting agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104549768B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105234005A (en) * | 2015-11-02 | 2016-01-13 | 中国海洋石油总公司 | Collophanite floatation positive ion collecting agent and preparation method and application thereof |
| CN106269272B (en) * | 2016-10-13 | 2018-10-09 | 昆明冶金研究院 | A kind of preparation method of bauxite floatation desilication high-efficient collecting agent |
| CN106583058A (en) * | 2016-12-28 | 2017-04-26 | 云南磷化集团有限公司 | Collophanite reverse flotation collecting agent and preparing method thereof |
| CN110479496B (en) * | 2019-09-20 | 2021-02-26 | 鞍钢集团矿业有限公司 | Iron ore reverse flotation composite amphoteric collecting agent and application thereof |
| CN111482277B (en) * | 2020-06-23 | 2022-06-10 | 四川省地质矿产勘查开发局成都综合岩矿测试中心 | Collecting agent for magnesium-silicon phosphate rock mixed reverse flotation, preparation method and beneficiation method |
| CN112517231B (en) * | 2020-11-18 | 2022-07-12 | 云南磷化集团有限公司 | Flotation method for low-grade carbonate collophanite |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6034271A (en) * | 1996-03-02 | 2000-03-07 | Huels Aktiengesellschaft | Betaine gemini surfactants made from amines |
| CN101088623A (en) * | 2007-06-28 | 2007-12-19 | 武汉理工大学 | Mineral floating collecting agent and its prepn process |
| CN101797536A (en) * | 2010-01-06 | 2010-08-11 | 云南省化工研究院 | Collophanite flotation collector and method for preparing same |
| CN101816981A (en) * | 2010-03-16 | 2010-09-01 | 武汉理工大学 | Environmentally-friendly amine cationic collector and using method thereof |
| CN102941160A (en) * | 2012-12-13 | 2013-02-27 | 贵州大学 | Flotation collector for silicate minerals |
| CN103769307A (en) * | 2013-10-28 | 2014-05-07 | 东北大学 | Collecting agent for water-soluble cations, preparation method thereof and application thereof |
-
2015
- 2015-02-02 CN CN201510051045.6A patent/CN104549768B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6034271A (en) * | 1996-03-02 | 2000-03-07 | Huels Aktiengesellschaft | Betaine gemini surfactants made from amines |
| CN101088623A (en) * | 2007-06-28 | 2007-12-19 | 武汉理工大学 | Mineral floating collecting agent and its prepn process |
| CN101797536A (en) * | 2010-01-06 | 2010-08-11 | 云南省化工研究院 | Collophanite flotation collector and method for preparing same |
| CN101816981A (en) * | 2010-03-16 | 2010-09-01 | 武汉理工大学 | Environmentally-friendly amine cationic collector and using method thereof |
| CN102941160A (en) * | 2012-12-13 | 2013-02-27 | 贵州大学 | Flotation collector for silicate minerals |
| CN103769307A (en) * | 2013-10-28 | 2014-05-07 | 东北大学 | Collecting agent for water-soluble cations, preparation method thereof and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 磷矿捕收剂的发展动向;骆兆军等;《云南冶金》;19990425;第28卷(第2期);第76～80页 * |
| 磷矿浮选捕收剂的研究进展;陈云峰等;《武汉工程大学学报》;20110215;第33卷(第2期);第17～20页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104549768A (en) | 2015-04-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104549768B (en) | Froth flotation cation collecting agent and preparation method thereof | |
| CN101797536B (en) | Collophanite flotation collector and method for preparing same | |
| CN105537003B (en) | Drainage oil type collophanite reverse flotation collecting agent and preparation method thereof | |
| CN103056036B (en) | Preparation method of collophanite normal-temperature direct flotation collecting agent | |
| CN102513221A (en) | Carbonate phosphorite reverse flotation combined collecting agent and preparation method thereof | |
| CN104607321A (en) | Collophanite froth flotation collecting agent and preparation method thereof | |
| CN105435953A (en) | Beneficiation method for molybdenum-containing low-grade mixed copper ore | |
| CN102658242A (en) | Mineral separation process of complex fluorite difficult to separate | |
| CN104107762A (en) | Low-temperature-resistant collophanite reverse flotation collecting agent and preparation method thereof | |
| CN101791591A (en) | Phosphorite low-temperature foam flotation collector and preparation method thereof | |
| CN101099946A (en) | Collophanite floatation method | |
| CN105689149A (en) | Double-reverse flotation method applicable to silico-calcium phosphorite | |
| CN102513220A (en) | Chemical composition for recycling copper concentrate and molybdenum concentrate from copper and molybdenum mixed concentrate pulp | |
| CN102553726A (en) | Composite collector for low-and-medium-temperature phosphate flotation and preparation method thereof | |
| CN104056726A (en) | Fluorite collecting agent and preparation method thereof | |
| CN102205278B (en) | Collophanite flotation collecting agent prepared from rubber seed oil and method for preparing same | |
| CN105344490A (en) | Collophane reverse flotation collector and preparation method thereof | |
| CN106944263B (en) | A kind of Collophane anti-floatation collector and its preparation method and application method | |
| CN108017296A (en) | A kind of grinding aid and its application | |
| CN105498980A (en) | Rutile flotation collector composition and application thereof | |
| CN108480055A (en) | A kind of Scheelite Flotation collecting agent and preparation method thereof | |
| CN104549766A (en) | Formula and preparation method of phosphorite reverse flotation deoxidization magnesium collecting agent | |
| CN107961903B (en) | A kind of composite chemical for floatating of zinc oxide and its preparation method and application | |
| CN105251622A (en) | Beneficiation inhibitor used in lepidolite flotation process | |
| CN103920596B (en) | Collophanite combination flotation collector and preparation method and application thereof |
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 | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 650114 peach tree, Haikou Town, Xishan District, Yunnan, Kunming Patentee after: Yunnan Shengwei Chemical Co. Ltd. Address before: 650114 peach tree, Haikou Town, Xishan District, Yunnan, Kunming Patentee before: YUNNAN COPPER INDUSTRY SUNWARD CHEMICALS CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |