CN103386368A - Sulfonated ore dressing collecting agent and preparation method thereof - Google Patents
Sulfonated ore dressing collecting agent and preparation method thereof Download PDFInfo
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- CN103386368A CN103386368A CN2012101409914A CN201210140991A CN103386368A CN 103386368 A CN103386368 A CN 103386368A CN 2012101409914 A CN2012101409914 A CN 2012101409914A CN 201210140991 A CN201210140991 A CN 201210140991A CN 103386368 A CN103386368 A CN 103386368A
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Abstract
The invention discloses a sulfonated ore dressing collecting agent and a preparation method thereof. According to the preparation method, the sulfonated ore dressing collecting agent is prepared by taking soybean oil foot, corn oil foot and castor oil foot as raw materials and adopting the steps of preparing, sulfonating, saponifying and refining. According to the sulfonated ore dressing collecting agent and the preparation method thereof, cheap byproducts produced in the process of processing edible oil and lubricating oil are adopted as main raw materials, and the mineral flotation collecting agent which is high in efficiency and low in cost is produced by adopting a sulfonation process. Meanwhile, a solution is provided for processing of byproducts produced in the process of processing the edible oil and the lubricating oil.
Description
Technical field
The present invention relates to a kind of sulfonation beneficiation collecting agent and preparation method thereof, belongs to the technology of preparing of mineral floating medicament.
Background technology
In metal oxide and nonmetal oxide mineral floatation technique, use in a large number the collecting agent of the fractionation product of oil as mineral, as kerosene and light diesel fuel, directly use, unit ton ore deposit consumption is large, and cost is higher, and to the poor selectivity of nonmetal oxide mineral, the rate of recovery is low.
Find through retrieval, publication number is the Chinese invention patent application of 102179311A, in this patent, " disclose a kind of anion collecting agent prepared from illegal cooking oil; it is characterized in that; raw material mainly adopts waste oil; utilize layering-removal of impurities-sulfonation-saponification technology to prepare the anion collecting agent; the preparation method is as follows: adding mass percent concentration in waste oil is 92.5% the industrial concentrated sulfuric acid; mass ratio, waste oil: the concentrated sulfuric acid=1: 0.05-0.1, stir, standing 4-6 hour, make the waste oil layering, obtain thick oil plant; With saturated nacl aqueous solution, thick oil plant is carried out the breakdown of emulsion removal of impurities, mass ratio, thick oil plant: sodium chloride solution=1: 0.1-0.12, to stir, separate, removal of impurities, obtain pure oil plant; With the industrial concentrated sulfuric acid of mass percent concentration 98%, pure oil plant is carried out sulfonation, mass ratio, pure oil plant: the concentrated sulfuric acid=1: 0.7-1, temperature: 100～115 ℃, reaction time: 4-6 hour, obtain the sulfonation oil plant; Be 10% industrial sodium hydroxide solution saponification with mass percent concentration, mass ratio, the sulfonation oil plant: NaOH is molten=and 1: 1.6, temperature: 80～100 ℃; Reaction time: 1-3 hour; Obtain the anion collecting agent." there are several problems in existing technology path: the employing waste oil is raw material, and raw material sources are more single; The production and processing time is long; Lack in the saponification process and detect and control, can not guarantee homogeneity and the stability of product; Lack subtractive process in existing technique, the product water content of gained is high, affects the flotation effect of product.The present invention is directed to the deficiency that prior art exists, a kind of sulfonation beneficiation collecting agent and preparation method thereof is provided.
Summary of the invention
The purpose of this invention is to provide a kind of sulfonation beneficiation collecting agent and preparation method thereof, to solve the above-mentioned problems in the prior art.Adopting cheap byproduct in edible oil and lubricating oil process in the present invention is primary raw material,, by process for sulfonation, produces usefulness high, the mineral floating collecting agent that cost is low.Simultaneously, the present invention processes a solution is provided for the processing of the byproduct in edible oil and lubricating oil process.
For achieving the above object, the present invention is by the following technical solutions:
The invention provides a kind of preparation method of sulfonation beneficiation collecting agent, take soybean oil residue, corn oil foot and castor oil oil foot etc. as raw material, by getting the raw materials ready, sulfonation, saponification and purification step make.Specifically comprise following steps:
(1) get the raw materials ready: the raw material oil foot is squeezed in preheating can, be warming up to 70-80 ℃ standby;
(2) sulfonation: the material in preheating can is squeezed in reactor, and temperature remains on 80-90 ℃, and with the weighing scale of raw material oil foot, slowly adding 8～10% mass percent concentrations is 98% the concentrated sulfuric acid, and limit adds the sulfuric acid limit stirs, can a large amount of heat releases in process; Treat that sulfuric acid all adds complete, continue to stir 30～40 minutes, temperature is no more than 100 ℃;
(3) saponification: the material in reactor is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stir 30-40 minute, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, discharges waste water and intermediate layer from the saponification pot bottom after sedimentation 30-40 minute; Remaining material in the saponification tank is heated to 95～100 ℃, the water that adds saponification tank volume 30% left and right, in the situation that material keeps boiling, adding mass percent concentration is the soda bath of 20-25%, keep soda bath excessive, saponification 1-2 hour, recirculation saponification 1-2 hour, detecting pH value should be more than 13, otherwise continues saponification;
(4) refining: as product qualified in the saponification tank to be squeezed into tube furnace with compression pump, adjust inlet amount and with fire, measure, when material moisture, squeeze into production tube during in 30% left and right, obtain the sulfonation beneficiation collecting agent.
In step (1) the primary raw material oil foot be one or more in cheap byproduct category-A, category-B, C class in edible oil and lubricating oil process:
Category-A: produce the byproduct of soybean oil, namely soybean oil residue, basic composition is monoacid, binary acid, cyclohexane, the mixture that oleic acid etc. are complicated;
Category-B: produce the byproduct of corn oil, namely the corn oil foot, basic composition is monoacid, binary acid, cyclohexane, the mixture that the tert-butyl alcohol etc. are complicated;
The C class: produce the accessory substance of castor oil, namely the castor-oil plant oil foot, basic composition is monoacid, binary acid, cyclohexane, C
8-12Saturated hydrocarbons, the mixture that aromatic hydrocarbon etc. are complicated.
In order better to realize purpose of the present invention, the raw material oil foot is preferably category-A: category-B: the C class is mixed by weight the ratio of 2:1:1.
Described raw material oil foot, caustic soda, the concentrated sulfuric acid are all identical with existing technique, can be from market purchasing.
In said method of the present invention, sulfonating reaction occurs in hydro carbons in 98% the concentrated sulfuric acid and raw material oil foot at a certain temperature, the part hydro carbons changes the sulfonic acid hydrocarbon into, next in saponification, NaOH and sulfonic acid hydrocarbon reaction generate sodium sulfonate, pass through again subtractive process, remove unnecessary Free water, be sulfonation beneficiation collecting agent of the present invention.
The present invention has following beneficial effect: it is primary raw material that the present invention adopts cheap byproduct in edible oil and lubricating oil process,, by process for sulfonation, produces usefulness high, the mineral floating collecting agent that cost is low.Simultaneously, the present invention processes a solution is provided for the processing of the byproduct in edible oil and lubricating oil process.
The specific embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented as prerequisite take technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
(1) get the raw materials ready: category-A raw material oil foot (being soybean oil residue) is squeezed in preheating can, be warming up to 80 ℃ standby.
(2) sulfonation: the material in preheating can is squeezed in reactor, and temperature remains on 80-90 ℃, and with the weighing scale of raw material oil foot, slowly adding 8% concentration is 98% the concentrated sulfuric acid, and limit adds the sulfuric acid limit stirs, can a large amount of heat releases in process.Treat that sulfuric acid all adds complete, continue to stir 30 minutes, temperature is no more than 100 ℃.
(3) saponification: the material in reactor is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stirred 40 minutes, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, and sedimentation was discharged waste water and intermediate layer from the saponification pot bottom after 30 minutes.Remaining material in the saponification tank is heated to 95～100 ℃, the water that adds saponification tank volume 30% left and right, in the situation that material keeps boiling, the soda bath that adds concentration 25%, keep soda bath excessive, saponification 1 hour, recirculation saponification 2 hours, detecting pH value should be more than 13, otherwise continues saponification.
(4) refining: as product qualified in the saponification tank to be squeezed into tube furnace with compression pump, adjust inlet amount and with fire, measure, when material moisture, squeeze into production tube during in 30% left and right, obtain product of the present invention.
The typical technology index of its product is as follows:
| Outward appearance | Black or brown paste |
| PH value | ?13～14 |
| Water content | ?25% |
| The rate of recovery of flotation phosphorus ore | Greater than 90% |
| The taste of flotation gained phosphorus fine powder | Greater than 35%(with P 2O 5) meter |
Embodiment 2
(1) get the raw materials ready: category-B raw material oil foot (being the corn oil foot) is squeezed in preheating can, be warming up to 70 ℃ standby.
(2) sulfonation: the material in preheating can is squeezed in reactor, and temperature remains on 80-90 ℃, and with the weighing scale of raw material oil foot, slowly adding 9% concentration is 98% the concentrated sulfuric acid, and limit adds the sulfuric acid limit stirs, can a large amount of heat releases in process.Treat that sulfuric acid all adds complete, continue to stir 40 minutes, temperature is no more than 100 ℃.
(3) saponification: the material in reactor is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stirred 40 minutes, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, and sedimentation was discharged waste water and intermediate layer from the saponification pot bottom after 30 minutes.Remaining material in the saponification tank is heated to 95～100 ℃, the water that adds saponification tank volume 30% left and right, in the situation that material keeps boiling, the soda bath that adds concentration 25%, keep soda bath excessive, saponification 1 hour, recirculation saponification 2 hours, detecting pH value should be more than 13, otherwise continues saponification.
(4) refining: as product qualified in the saponification tank to be squeezed into tube furnace with compression pump, adjust inlet amount and with fire, measure, when material moisture, squeeze into production tube during in 30% left and right, obtain product of the present invention.
The typical technology index of its product is as follows:
| Outward appearance | Black or brown paste |
| PH value | ?13～14 |
| Water content | ?28% |
| The rate of recovery of flotation phosphorus ore | Greater than 91% |
| The taste of flotation gained phosphorus fine powder | Greater than 34%(with P 2O 5) meter |
Embodiment 3
(1) get the raw materials ready: C class raw material oil foot (being the castor-oil plant oil foot) is squeezed in preheating can, be warming up to 75 ℃ standby.
(2) sulfonation: the material in preheating can is squeezed in reactor, and temperature remains on 80-90 ℃, and with the weighing scale of raw material oil foot, slowly adding 10% concentration is 98% the concentrated sulfuric acid, and limit adds the sulfuric acid limit stirs, can a large amount of heat releases in process.Treat that sulfuric acid all adds complete, continue to stir 40 minutes, temperature is no more than 100 ℃.
(3) saponification: the material in reactor is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stirred 40 minutes, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, and sedimentation was discharged waste water and intermediate layer from the saponification pot bottom after 30 minutes.Remaining material in the saponification tank is heated to 95～100 ℃, the water that adds saponification tank volume 30% left and right, in the situation that material keeps boiling, the soda bath that adds concentration 25%, keep soda bath excessive, saponification 1 hour, recirculation saponification 1 hour, detecting pH value should be more than 13, otherwise continues saponification.
(4) refining: as product qualified in the saponification tank to be squeezed into tube furnace with compression pump, adjust inlet amount and with fire, measure, when material moisture, squeeze into production tube during in 30% left and right, obtain product of the present invention.
The typical technology index of its product is as follows:
| Outward appearance | Black or brown paste |
| PH value | ?13～14 |
| Water content | ?27% |
| The rate of recovery of flotation phosphorus ore | Greater than 90% |
| The taste of flotation gained phosphorus fine powder | Greater than 35%(with P 2O 5) meter |
Embodiment 4
(1) get the raw materials ready: category-A, category-B, C class raw material oil foot are squeezed in preheating can according to the ratio of 2:1:1, be warming up to 80 ℃ standby.
(2) sulfonation: the material in preheating can is squeezed in reactor, and temperature remains on 80-90 ℃, and with the weighing scale of raw material oil foot, slowly adding 9% concentration is 98% the concentrated sulfuric acid, and limit adds the sulfuric acid limit stirs, can a large amount of heat releases in process.Treat that sulfuric acid all adds complete, continue to stir 35 minutes, temperature is no more than 100 ℃.
(3) saponification: the material in reactor is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stirred 40 minutes, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, and sedimentation was discharged waste water and intermediate layer from the saponification pot bottom after 30 minutes.Remaining material in the saponification tank is heated to 95～100 ℃, the water that adds saponification tank volume 30% left and right, in the situation that material keeps boiling, the soda bath that adds concentration 25%, keep soda bath excessive, saponification 1 hour, recirculation saponification 1 hour, detecting pH value should be more than 13, otherwise continues saponification.
(4) refining: as product qualified in the saponification tank to be squeezed into tube furnace with compression pump, adjust inlet amount and with fire, measure, when material moisture, squeeze into production tube during in 30% left and right, obtain product of the present invention.
The typical technology index of its product is as follows:
| Outward appearance | Black or brown paste |
| PH value | ?13～14 |
| Water content | ?26% |
| The rate of recovery of flotation phosphorus ore | Greater than 95% |
| The taste of flotation gained phosphorus fine powder | Greater than 35%(with P 2O 5) meter |
, although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (4)
1. the preparation method of a sulfonation beneficiation collecting agent is characterized in that consisting of following steps:
(1) get the raw materials ready: the raw material oil foot is squeezed in preheating can, be warming up to 70-80 ℃ standby;
(2) sulfonation: the material in preheating can is squeezed in reactor, and temperature remains on 80-90 ℃, and with the weighing scale of raw material oil foot, slowly adding 8～10% mass percent concentrations is 98% the concentrated sulfuric acid, and limit adds the sulfuric acid limit stirs, can a large amount of heat releases in process; Treat that sulfuric acid all adds complete, continue to stir 30～40 minutes, temperature is no more than 100 ℃;
(3) saponification: the material in reactor is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stir 30-40 minute, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, discharges waste water and intermediate layer from the saponification pot bottom after sedimentation 30-40 minute; Remaining material in the saponification tank is heated to 95～100 ℃, the water that adds saponification tank volume 30% left and right, in the situation that material keeps boiling, adding mass percent concentration is the soda bath of 20-25%, keep soda bath excessive, saponification 1-2 hour, recirculation saponification 1-2 hour, detecting pH value should be more than 13, otherwise continues saponification;
(4) refining: as product qualified in the saponification tank to be squeezed into tube furnace with compression pump, adjust inlet amount and with fire, measure, when material moisture, squeeze into production tube 30% the time, obtain the sulfonation beneficiation collecting agent.
2. the preparation method of a kind of sulfonation beneficiation collecting agent according to claim 1, it is characterized in that in step (1) the raw material oil foot be one or more in cheap byproduct category-A, category-B, C class in edible oil and lubricating oil process:
Category-A: produce the byproduct of soybean oil, namely soybean oil residue, basic composition is monoacid, binary acid, cyclohexane, the mixture that oleic acid etc. are complicated;
Category-B: produce the byproduct of corn oil, namely the corn oil foot, basic composition is monoacid, binary acid, cyclohexane, the mixture that the tert-butyl alcohol etc. are complicated;
The C class: produce the accessory substance of castor oil, namely the castor-oil plant oil foot, basic composition is monoacid, binary acid, cyclohexane, C
8-12Saturated hydrocarbons, the mixture that aromatic hydrocarbon etc. are complicated.
3. the preparation method of a kind of sulfonation beneficiation collecting agent according to claim 2 is characterized in that the described raw material oil foot of step (1) is by category-A: category-B: the C class is mixed by weight the ratio of 2:1:1.
4. a sulfonation beneficiation collecting agent, is characterized in that: be the sulfonation beneficiation collecting agent that adopts the described method of claim 1-3 to prepare.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210140991.4A CN103386368B (en) | 2012-05-08 | 2012-05-08 | A kind of sulfonated ore dressing collecting agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210140991.4A CN103386368B (en) | 2012-05-08 | 2012-05-08 | A kind of sulfonated ore dressing collecting agent and preparation method thereof |
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| CN103386368A true CN103386368A (en) | 2013-11-13 |
| CN103386368B CN103386368B (en) | 2017-06-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104056724A (en) * | 2014-06-11 | 2014-09-24 | 北京矿冶研究总院 | Reverse flotation collector for hematite and preparation and use method thereof |
| CN106076652A (en) * | 2016-06-15 | 2016-11-09 | 武汉工程大学 | Fluorite flotation collecting agent based on plant asphalt and its preparation method and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4364824A (en) * | 1981-06-02 | 1982-12-21 | International Minerals & Chemical Corp. | Flotation of phosphate ores containing dolomite |
| CN1623674A (en) * | 2003-12-05 | 2005-06-08 | 福州大学 | Preparation process for floatation ion collector of heavy spar |
| CN101823026A (en) * | 2010-03-18 | 2010-09-08 | 武汉理工大学 | Combined collecting agent for reverse flotation phosphorous reduction of high phosphorus oolitic hematite |
| CN101972708A (en) * | 2010-10-28 | 2011-02-16 | 山东科技大学 | Preparation method of feldspar ore reverse-flotation de-ironing collector |
| CN102179311A (en) * | 2011-03-16 | 2011-09-14 | 内蒙古包钢稀土林峰科技有限公司 | Anion collecting agent prepared from illegal cooking oil |
-
2012
- 2012-05-08 CN CN201210140991.4A patent/CN103386368B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4364824A (en) * | 1981-06-02 | 1982-12-21 | International Minerals & Chemical Corp. | Flotation of phosphate ores containing dolomite |
| CN1623674A (en) * | 2003-12-05 | 2005-06-08 | 福州大学 | Preparation process for floatation ion collector of heavy spar |
| CN101823026A (en) * | 2010-03-18 | 2010-09-08 | 武汉理工大学 | Combined collecting agent for reverse flotation phosphorous reduction of high phosphorus oolitic hematite |
| CN101972708A (en) * | 2010-10-28 | 2011-02-16 | 山东科技大学 | Preparation method of feldspar ore reverse-flotation de-ironing collector |
| CN102179311A (en) * | 2011-03-16 | 2011-09-14 | 内蒙古包钢稀土林峰科技有限公司 | Anion collecting agent prepared from illegal cooking oil |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104056724A (en) * | 2014-06-11 | 2014-09-24 | 北京矿冶研究总院 | Reverse flotation collector for hematite and preparation and use method thereof |
| CN106076652A (en) * | 2016-06-15 | 2016-11-09 | 武汉工程大学 | Fluorite flotation collecting agent based on plant asphalt and its preparation method and application |
| CN106076652B (en) * | 2016-06-15 | 2018-11-06 | 武汉工程大学 | Fluorite flotation collecting agent based on plant asphalt and its preparation method and application |
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| CN103386368B (en) | 2017-06-30 |
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