CN102247935B - Ore dressing collector and preparation method thereof - Google Patents
Ore dressing collector and preparation method thereof Download PDFInfo
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- CN102247935B CN102247935B CN 201110122581 CN201110122581A CN102247935B CN 102247935 B CN102247935 B CN 102247935B CN 201110122581 CN201110122581 CN 201110122581 CN 201110122581 A CN201110122581 A CN 201110122581A CN 102247935 B CN102247935 B CN 102247935B
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- electrolysis
- ore dressing
- pcl
- collecting agent
- oleic acid
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Abstract
The invention discloses an ore dressing collector and a preparation method thereof. The ore dressing collector consists of the following raw materials in percentage by weight: 75 to 80 percent of oleic acid, 3 to 5 percent of surfactant, 5 to 7 percent of N,N-dimethylformamide-dimethyl sulfate, and 10 to 15 percent of chloride. The oleic acid is subjected to electrolytic dissociation and chemical modification by the steps of activation, electrolyzation, separation and introduction of an active group so as to form the ore dressing collector with high activity, dispersibility and selectivity. The ore dressing collector is particularly suitable for ore dressing of minerals such as non-metallic fluorite, kyanite, barite, metal white tungsten, hematite reverse flotation and the like, particularly the ore dressing at low temperature (more than or equal to 2 DEG C).
Description
Technical field:
The present invention relates to a kind of beneficiation collecting agent and preparation method thereof, particularly a kind of for nonmetal fluorite, kyanite, barite, low temperature beneficiation collecting agent of the mineral ore dressings such as the white tungsten of metal, hematite reverse flotation and preparation method thereof.
Background technology:
The collecting agent that present domestic nonmetal ore-dressing industry is used mainly is with the series products of oleic acid as primary raw material, oleic acid is a kind of important collecting agent of non-sulfide flotation, yet there is the not anti-hard water of poor selectivity in such collecting agent, poorly water-soluble is not low temperature resistant, the bad dispersibility consumption is large, the shortcomings such as concentrate grade is low need ore pulp is carried out heat treated in ore dressing process, and power consumption is large; And lean ore is many, rich ore is few in the present mineral resources, and difficult ore dressing is many, easily ore dressing is few, for ore-dressing technique has increased difficulty; Domestic and international existing pertinent literature and patent Introduction product all can not reach the requirement that northern area realizes not heating the ore pulp ore dressing winter; China Patent No. 200910021853.2 discloses a kind of collecting agent of flotation at low temperature fluorite, slurry temperature is 10 ℃ of normally flotation fluorites, and the long-term water temperature of northern area is below 10 ℃, thus northern area especially in the winter time ore dressing must heat ore pulp, production cost is large; These conditions make present Mineral Processing Industry be badly in need of a kind of can the application and the selective effective collecting agent of collecting being lower than under 10 ℃ the cryogenic conditions.
Summary of the invention:
Purpose of the present invention be exactly to provide a kind of for present Mineral Processing Industry, especially north cold area to the present situation of lower temperature collector active demand, can realize low temperature (〉=2 ℃) ore dressing and reach beneficiation collecting agent of preferably ore dressing effect and preparation method thereof.
The object of the present invention is achieved like this: a kind of beneficiation collecting agent, it is characterized in that it by following raw material by weight component form:
A kind of or two or more 3～5%, N in oleic acid 75～80%, dodecyl sodium sulfate, sodium cetanesulfonate, DTAC, the two dodecyl dimethyl ammonium chloride, N-dimethylformamide-dimethyl suflfate 5～7%, POCl
3, PCl
3, PCl
5In a kind of or two or more 10～15%.
Preparation method of the present invention is:
1), activation: with a kind of in oleic acid and dodecyl sodium sulfate, sodium cetanesulfonate, DTAC, the two dodecyl dimethyl ammonium chloride or two or morely under 20～30 ℃ of conditions, mix according to the above ratio;
2), electrolysis: the mixed liquor of the first step is added in the electrolysis of hydrochloric acid liquid of 1mol/L and carry out electrolysis, electrolysis temperature is 25～35 ℃, and anodic current density is 1000～1500A/m
2, electrolysis time 0.5～1.5h;
3), separate: the mixed liquor after electrolysis finishes imports in the separator, carries out oil phase and aqueous phase separation, obtains oil phase;
4), introduce active group: in oil phase, add according to the above ratio N, N-dimethylformamide-dimethyl suflfate and POCl
3, PCl
3, PCl
5In a kind of or two or more, under 40～55 ℃ of heating conditions, react 20～30min, collecting agent gets product.
Electrolysis negative and positive the two poles of the earth material is respectively iron and graphite in the electrolysis step of the present invention.
The present invention carries out electrochemical modification to oleic acid after oleic acid is activated, and molecular weight is diminished, and introduces active group, generates the new collector with high activity, polymolecularity, high selectivity.
The present invention compared with prior art has the following advantages:
Owing to adopted oleic acid, a kind of or two or more in dodecyl sodium sulfate, sodium cetanesulfonate, DTAC, the two dodecyl dimethyl ammonium chloride, N, N-dimethylformamide-dimethyl suflfate, POCl
3, PCl
3, PCl
5In a kind of or two or more by a certain percentage the reaction form, utilized the step of activation, electrolysis, separation, introducing active group, thereby, by the electrochemistry dissociation technique, destroy the macro-radical of oleic acid, and in the oleic acid macro-radical, introduce active group, active function groups, high polar group, make the organic content decrease of HMW in the oleic acid solutions after the modification, make modified oil acid activity, dissolubility, dispersiveness, the enhancing such as selective, thereby can under the few condition of low temperature and consumption, obtain preferably collecting effect.
1. good dispersion, the intrinsic shortcoming of oleic acid is exactly that the bad dispersibility consumption is large, and the present invention has improved the dispersiveness of oleic acid greatly, makes the consumption of collecting agent be reduced to original 1/2～1/3.
2. good water solubility under the cryogenic conditions, the present invention has improved the water-soluble of collecting agent greatly, can use under 〉=2 ℃ lower temperature, and ore dressing process need not ore pulp is carried out heat treated, can greatly reduce beneficiation cost, makes Mineral Processing Enterprises realize energy-saving and emission-reduction.
3. selectively good, the present invention has selective preferably, is used for mineral processing production and can greatly improves product grade, improves product recovery rate, is more suitable for the ore-dressing technique of lean ore, difficult ore dressing.
The specific embodiment:
Embodiment 1
With the product of the present invention of preparation 1000kg, get oleic acid 760kg, dodecyl sodium sulfate 20kg, sodium cetanesulfonate 30kg, N, N-dimethylformamide-dimethyl suflfate 55kg, POCl
365kg, PCl
370kg, its preparation method is:
1. oleic acid is poured in the stirred tank, slowly added dodecyl sodium sulfate and sodium cetanesulfonate, the limit edged stirs, and this step carries out under 20～30 ℃ of conditions;
2. the mixed liquor with previous step adds in the hydrochloric acid solution of 1mol/L, makes electrode with graphite, iron, and graphite is anode, and iron is negative electrode, and anodic current density is 1000A/m
2Condition under carry out electrolysis, electrolysis temperature is 35 ℃, electrolysis time 0.5h;
3. the mixed liquor after electrolysis finishes imports in the separator, carries out oil phase and aqueous phase separation, obtains oil phase;
4. add N in the oil phase that obtains, N-dimethylformamide-dimethyl suflfate and POCl
3, PCl
3, being warming up to 40 ℃, collecting agent gets product behind the reaction 30min.
Embodiment 2
With the product of the present invention of preparation 1000kg, get oleic acid 780kg, sodium cetanesulfonate 25kg, two dodecyl dimethyl ammonium chloride 20kg, N, N-dimethylformamide-dimethyl suflfate 50kg, PCl
3125kg, its preparation method is:
1. oleic acid is poured in the stirred tank, slowly added sodium cetanesulfonate and two dodecyl dimethyl ammonium chloride, the limit edged stirs, and this step carries out under 20～30 ℃ of conditions;
2. the mixed liquor with previous step adds in the hydrochloric acid solution of 1mol/L, makes electrode with graphite, iron, and graphite is anode, and iron is negative electrode, and anodic current density is 1200A/m
2Condition under carry out electrolysis, electrolysis temperature is 30 ℃, electrolysis time 1h;
3. the mixed liquor after electrolysis finishes imports in the separator, carries out oil phase and aqueous phase separation, obtains oil phase;
4. add N in the oil phase that obtains, N-dimethylformamide-dimethyl suflfate and PCl
3, being warming up to 50 ℃, collecting agent gets product behind the reaction 25min.
Embodiment 3
With the product of the present invention of preparation 1000kg, get oleic acid 780kg, DTAC 40kg, N, N-dimethylformamide-dimethyl suflfate 60kg, PCl
5120kg, its preparation method is:
1. oleic acid is poured in the stirred tank, slowly added DTAC, the limit edged stirs, and this step carries out under 20～30 ℃ of conditions;
2. the mixed liquor with previous step adds in the hydrochloric acid solution of 1mol/L, makes electrode with graphite, iron, and graphite is anode, and iron is negative electrode, and anodic current density is 1400A/m
2Condition under carry out electrolysis, electrolysis temperature is 25 ℃, electrolysis time 1.5h;
3. the mixed liquor after electrolysis finishes imports in the separator, carries out oil phase and aqueous phase separation, obtains oil phase;
4. add N in the oil phase that obtains, N-dimethylformamide-dimethyl suflfate and PCl
5, being warming up to 55 ℃, collecting agent gets product behind the reaction 20min.
Collecting agent operating position of the present invention, under 2 ℃ of conditions, flotation fluorite effect is such as table
Table
Can be found out by table: under cryogenic conditions, the collecting agent of this patent invention can obtain the higher rate of recovery and work of high quality in the few situation of consumption.
Claims (3)
1. beneficiation collecting agent, it is characterized in that it by following raw material by weight component form:
A kind of or two or more 3～5%, N in oleic acid 75～80%, dodecyl sodium sulfate, sodium cetanesulfonate, DTAC, the two dodecyl dimethyl ammonium chloride, N-dimethylformamide-dimethyl suflfate 5～7%, POCl
3, PCl
3, PCl
5In one or more 10～15%.
2. by the preparation method of a kind of beneficiation collecting agent described in the claim 1, it is characterized in that it is comprised of following steps:
1), activation: with a kind of in oleic acid and dodecyl sodium sulfate, sodium cetanesulfonate, DTAC, the two dodecyl dimethyl ammonium chloride or two or morely under 20～30 ℃ of conditions, mix according to the above ratio;
2), electrolysis: the mixed liquor of the first step is added in the electrolysis of hydrochloric acid liquid of 1mol/L and carry out electrolysis, anodic current density is 1000～1500A/m
2, electrolysis temperature is 25～35 ℃, electrolysis time 0.5～1.5h;
3), separate: the mixed liquor after electrolysis finishes imports in the separator, carries out oil phase and aqueous phase separation, obtains oil phase;
4), introduce active group: in oil phase, add according to the above ratio N, N-dimethylformamide-dimethyl suflfate and POCl
3, PCl
3, PCl
5In one or more, under 40～55 ℃ of heating conditions, react 20～30min, collecting agent gets product.
3. the preparation method of a kind of beneficiation collecting agent described in the claim 2 is characterized in that electrolysis negative and positive the two poles of the earth material is respectively iron and graphite in the described electrolysis step.
Priority Applications (1)
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| CN 201110122581 CN102247935B (en) | 2011-05-13 | 2011-05-13 | Ore dressing collector and preparation method thereof |
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|---|---|---|---|
| CN 201110122581 CN102247935B (en) | 2011-05-13 | 2011-05-13 | Ore dressing collector and preparation method thereof |
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| CN102247935A CN102247935A (en) | 2011-11-23 |
| CN102247935B true CN102247935B (en) | 2013-03-20 |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102764700B (en) * | 2012-08-01 | 2013-09-25 | 中钢集团马鞍山矿山研究院有限公司 | Preparation method of low temperature resisting fluorite flotation collector |
| CN103639059A (en) * | 2013-12-11 | 2014-03-19 | 广西大学 | Beneficiation method for carbonic mud barite ore |
| CN104399592B (en) * | 2014-10-24 | 2017-02-15 | 广德县瑞龙新型材料有限公司 | Fluorite floatation process |
| CN104475268A (en) * | 2014-12-03 | 2015-04-01 | 紫金矿业集团股份有限公司 | Method for recycling alunite from copper ore flotation tailings |
| CN104941814B (en) * | 2015-05-06 | 2017-04-05 | 广西大学 | The preparation method of the supplementary catching agent of recovery of gold and silver in a kind of raising tennantite |
| CN105457743A (en) * | 2015-11-16 | 2016-04-06 | 湖南有色金属研究院 | Beneficiation method of micro-fine particle graphite ores for producing high-carbon graphite |
| CN106378263B (en) * | 2016-09-27 | 2018-06-22 | 中国地质科学院郑州矿产综合利用研究所 | Low-alkali-consumption scheelite collecting agent and application thereof |
| CN107138288B (en) * | 2017-05-27 | 2019-11-12 | 洛阳振北工贸有限公司 | A kind of low temperature fluorite collecting agent |
| CN107350086B (en) * | 2017-07-06 | 2019-03-22 | 西南科技大学 | Combined capturing and collecting agent and preparation method and application for flotation olive pyroxenite type ilmenite |
| CN108855628A (en) * | 2018-06-01 | 2018-11-23 | 洛阳丰瑞氟业有限公司 | A kind of Fluorspar Powder production collecting agent preparation method |
| CN110015727B (en) * | 2019-05-09 | 2021-07-09 | 安徽工业大学 | Method for removing micro-plastics in water body by electrolytic air flotation |
| CN111468306A (en) * | 2020-05-26 | 2020-07-31 | 河南天鸿选矿科技有限公司 | Fluorite ore flotation collecting agent |
| CN114471954B (en) * | 2021-03-26 | 2022-10-11 | 中南大学 | Application of N- (2-oxahydrocarbyl) -beta-carbonyl amide compound in fluorite flotation |
| CN113245065B (en) * | 2021-06-09 | 2022-04-26 | 东北大学 | Micro-fine particle quartz reverse flotation combined collecting agent and reverse flotation method |
| CN115582224A (en) * | 2022-09-30 | 2023-01-10 | 昆明理工大学 | Flotation combined reagent and application thereof, and method for flotation desilication of micro-fine particle zinc oxide ore |
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|---|---|---|---|---|
| US4208275A (en) * | 1979-01-24 | 1980-06-17 | The United States Of America As Represented By The Secretary Of The Interior | Froth flotation using lanolin modifier |
| SU1604487A1 (en) * | 1988-12-19 | 1990-11-07 | Ленинабадский Ботанический Сад Института Ботаники Ан Таджсср | Method of flotation of fluorite-bearing ores |
| SU1609497A1 (en) * | 1989-01-13 | 1990-11-30 | Институт химии им.В.И.Никитина | Method of flotation of fluorite-bearing ores |
| CN1919466A (en) * | 2006-01-23 | 2007-02-28 | 攀枝花钢铁有限责任公司钛业分公司 | Collector for flotation collecting ilmenite and its preparation method |
| CN101507948A (en) * | 2009-04-03 | 2009-08-19 | 陕西新星浮选剂有限责任公司 | Cold condition fluorite flotation collector |
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2011
- 2011-05-13 CN CN 201110122581 patent/CN102247935B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4208275A (en) * | 1979-01-24 | 1980-06-17 | The United States Of America As Represented By The Secretary Of The Interior | Froth flotation using lanolin modifier |
| SU1604487A1 (en) * | 1988-12-19 | 1990-11-07 | Ленинабадский Ботанический Сад Института Ботаники Ан Таджсср | Method of flotation of fluorite-bearing ores |
| SU1609497A1 (en) * | 1989-01-13 | 1990-11-30 | Институт химии им.В.И.Никитина | Method of flotation of fluorite-bearing ores |
| CN1919466A (en) * | 2006-01-23 | 2007-02-28 | 攀枝花钢铁有限责任公司钛业分公司 | Collector for flotation collecting ilmenite and its preparation method |
| CN101507948A (en) * | 2009-04-03 | 2009-08-19 | 陕西新星浮选剂有限责任公司 | Cold condition fluorite flotation collector |
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