CN103387849A - Novel oxyparaffin soap and preparation method thereof - Google Patents
Novel oxyparaffin soap and preparation method thereof Download PDFInfo
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- CN103387849A CN103387849A CN2012101414471A CN201210141447A CN103387849A CN 103387849 A CN103387849 A CN 103387849A CN 2012101414471 A CN2012101414471 A CN 2012101414471A CN 201210141447 A CN201210141447 A CN 201210141447A CN 103387849 A CN103387849 A CN 103387849A
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Abstract
The invention discloses novel oxyparaffin soap and a preparation method thereof. The preparation method comprises the steps of material preparation, oxidation, saponification and compoudation. A phosphorus-containing compound is used as a catalyst. Compared with a conventional process, the preparation method shortens oxidation time, and the content of effective substances in an oxidation product reaches over 60%. A final product formed by compounding the novel oxyparaffin soap with tallol has good selectivity for mineral materials and increases the grade and recovery rate of the mineral materials.
Description
Technical field
The present invention relates to a kind of Chemicals, particularly a kind of novel oxidized paraffin wax soap and preparation method thereof, belongs to the technology of preparing of Chemicals.
Background technology
Oxidized paraffin wax soap is the mineral flotation agent of commonly using, and is widely used in the floatation process of metal and nonmetal oxide mineral.Existing production technique exists following deficiency: use potassium permanganate to be catalyzer, and long reaction time, in the production thing, working substance content is low, increases production cost; The poor selectivity of the finished product to mineral, the ore dressing grade is low, and flotation effect haves much room for improvement.
Find through retrieval, publication number is the Chinese invention patent application of CN1974730A, this patent open " a kind of process of producing oxygenated paraffin soap is characterized in that being comprised of following steps:
(1). get the raw materials ready: a certain amount of paraffin is squeezed in preheating can, impurities removal, Fen Shui, dewater and be warming up to 120 ℃ after the insulation standby, additive sylvite and manganese salt drop in dissolving vessel by 0.3～0.8 ‰ by charging capacity 1.5～2 ‰, soda ash, add after water-solubleization standby, get the caustic soda of inventory 50% left and right, make after the alkaline solution of concentration 25-30% standby;
(2). the preparation of oxidized petroleum waves: material preheated in preheating can is squeezed in oxidizing tower, simultaneously by 40 cubic metres/tons per hour air quantity to air feed in oxidizing tower, heat supply, catalyst solution is squeezed in tower, when temperature of charge in tower reaches 160 ± 2 ℃, start to cause, kept 0.5 hour, wind supply quantity is brought up to 50 cubic metres/tons per hour, being cooled to 150 ± 2 ℃ starts to excite, after two hours, in tower, material is cooled to 120-130 ℃, start oxidation, wind supply quantity is increased to 60 cubic metres/tons per hour simultaneously, temperature-resistant, 80 cubic metres/tons per hour after 12 hours is brought up to air quantity in oxidation, temperature-resistant, start to detect acid number after exciting end, when oxidizing tower material acid number reaches 80-85mgKOH/g, oxidation finishes, after oxidation finishes, in tower, material stops heat supply and is cooled to 120 ℃, simultaneously wind supply quantity is reduced to 40 cubic metres/tons per hour, start tower, material in oxidizing tower is squeezed in the saponification tank that tankage 30-40%75 ℃ hot water is housed, to react simultaneously the oil-soluble acid that generates and evenly squeeze into the saponification tank,
(3). saponification: a. washing: the oxidized petroleum waves temperature that will squeeze into the saponification tank is adjusted to 85 ℃ of left and right, with steam or air, transfer to material and seethe state, stir with open steam during lower than 85 ℃ when temperature of charge in the saponification tank, use pneumatic blending during higher than 85 ℃ instead when temperature of charge, stirred at least 40 minutes, after stopping, stirring is incubated sedimentation under 85-90 ℃ of condition, sedimentation was discharged waste water and middle layer from the saponification pot bottom after 30 minutes, till detection washing rear oxidation cerinic acid value was slightly acidic to the waste water pH value, defective will the repetition washed; B. saponification: the oxidized petroleum waves qualified to washing in the saponification tank, with being steam heated to 95-100 ℃, the water that adds simultaneously inventory 35% left and right, under material boiling situation, add the alkaline solution of getting ready in oxidized petroleum waves, adding alkali number calculates by oxidized petroleum waves alkali charge=acid number per ton * 1.8 * 0.71 * 1.03 (excess base) ÷ concentration ÷ 1000, filled up the alkali after saponification 1 hour, the recirculation saponification more than 1 hour, is checked pH value 13 left and right after saponification finishes, saponification is completed, otherwise continues alkaline saponification; C. separate: after saponification finished, in the saponification tank, material insulation sedimentation was at least 3 hours, and soap lye is squeezed into the soap lye storage tank, surpasses rest time and changes next procedure over to after 24 hours again;
(4). refining: soap lye qualified in storage tank is squeezed into tube furnace through pressure pump, adjust inlet amount and with fire, measure, in squeezing into treatment tank during in 30% left and right, material moisture is the oxidized paraffin wax soap work in-process, after check, adjust free alkali content, moisture, make it reach standard-required, the material qualified finished product that is after testing in treatment tank, and squeeze into finished pot and carry out metering packing." but still there is above-mentioned problem in this patented technology.
Summary of the invention
The purpose of this invention is to provide a kind of novel oxidized paraffin wax soap and preparation method thereof, to solve in prior art, have above-mentioned problem.Oxidized paraffin wax soap in the present invention uses P contained compound to be catalyzer, has shortened oxidation time, and the working substance content of oxidation resultant reaches more than 60%, saves production cost.Be final product after the composite Yatall MA of saponification resultant, its finished product are good to the selectivity of mineral, upgrade and the rate of recovery.
For achieving the above object, the present invention is by the following technical solutions:
The invention provides a kind of preparation method of novel oxidized paraffin wax soap, comprise the steps:
(1) get the raw materials ready: paraffin is squeezed in preheating can, be warming up to 110-120 ℃ standby; With the paraffin weighing scale, after being mixed with solution, 1.5～2 ‰ P contained compounds and 0.5～1 ‰ soda ash adds in preheating can, mix;
(2) oxidation: the material in preheating can is squeezed in oxidizing tower, blow to oxidizing tower by 35-40 cubic meter/tons per hour air quantity, when material in oxidizing tower is warming up to 150-160 ℃, start to excite, air quantity is brought up to 40-50 cubic meter/tons per hour, after 2 hours, in oxidizing tower, the temperature of material reaches 120～125 ℃, keep this temperature, air quantity is brought up to 50-60 cubic meter/tons per hour, start oxidation; The acid number of material in 1 hour detection oxidizing tower, when acid number reached 80～85mgKOH/g, oxidation finished;
(3) saponification: the material in oxidizing tower 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, and sedimentation was discharged waste water and middle 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, adding mass percent concentration is 25% caustic soda soln, keep caustic soda soln excessive, saponification 1-2 hour, recirculation saponification 1-2 hour, detecting pH value should be more than 13, otherwise continues saponification;
(4) composite: the saponification resultant that obtains in step (3) is incubated at 90 ℃, and sedimentation 2-3 hour, discharge waste water, and saponification resultant is squeezed into composite tank, adds Yatall MA, and insulation, at 80-90 ℃, after mixing and stirring, obtains oxidized paraffin wax soap of the present invention.
Component and the weight percent of the described P contained compound of step (1) are:
Polyphosphoric acid 35% ~ 40%
Tetra-sodium 20% ~ 30%
Phosphoric acid 35% ~ 40%
Be preferably:
Polyphosphoric acid 35%
Tetra-sodium 25%
Phosphatase 24 0%
The weight concentration of described polyphosphoric acid is that 105%(is with H
3PO
4Note).
Described P contained compound preparation method, can adopt conventional physical mixed method.
Composite with Yatall MA described in step (4), wherein saponification resultant and Yatall MA according to the ratio of weight ratio 6～8:1～2 for well.
Described Yatall MA is rough Yatall MA, and its acid number should be at 60～80mgKOH/g, this product of many plant produced of Heilungkiang Jiamusi.
Described paraffin, soda ash, caustic soda are all identical with existing technique, can be from market purchasing.
In aforesaid method of the present invention: the composite oxygenant with strong oxidizing property that forms of multiple P contained compound has caused the oxidizing reaction of paraffin under the condition of high temperature, keep the oxidizing reaction of paraffin steadily to carry out rapidly by the air output that strengthens gas blower, the result of oxidation is that the hydro carbons Partial Conversion in paraffin is carboxylic acid, add appropriate alkali lye, in carrying out and saponification reaction, generating saponification resultant, is the finished product after the composite Yatall MA of saponification resultant.
The present invention has following beneficial effect: the prepared modified emulsifying asphalt of the present invention compared with prior art has following outstanding advantages: shortened oxidation time, the working substance content of oxidation resultant reaches more than 60%, saves production cost.Be final product after the composite Yatall MA of saponification resultant, its finished product are good to the selectivity of mineral, upgrade and the rate of recovery.
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: paraffin is squeezed in preheating can, be warming up to 120 ℃ standby.With the paraffin weighing scale, after being mixed with solution, 1.5 ‰ P contained compounds (by polyphosphoric acid 35%, tetra-sodium 25%, phosphatase 24 0% forms) and 0.8 ‰ soda ash add in preheating can, mix.
(2) oxidation: the material in preheating can is squeezed in oxidizing tower, blow to oxidizing tower by 38 cubic metres/tons per hour air quantity, when material in oxidizing tower is warming up to 160 ℃, start to excite, air quantity is brought up to 40 cubic metres/tons per hour, after 2 hours, in oxidizing tower, the temperature of material reaches 120～125 ℃, keep this temperature, air quantity is brought up to 50 cubic metres/tons per hour, start oxidation.The acid number of material in 1 hour detection oxidizing tower, when acid number reached 80～85mgKOH/g, oxidation finished.
(3) saponification: the material in oxidizing tower is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stirred 35 minutes, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, and sedimentation was discharged waste water and middle 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 caustic soda soln that adds concentration 25%, keep caustic soda soln excessive, saponification 1 hour, recirculation saponification 1 hour, detecting pH value should be more than 13, otherwise continues saponification.
(4) composite: the saponification resultant that obtains in step (3) is incubated at 90 ℃, and sedimentation 3 hours, discharge waste water, saponification resultant, Yatall MA are joined in composite tank according to the ratio of 8:1, insulation, at 80 ℃, after mixing and stirring, obtains oxidized paraffin wax soap of the present invention.
Embodiment 2
(1) get the raw materials ready: paraffin is squeezed in preheating can, be warming up to 110 ℃ standby.With the paraffin weighing scale, after being mixed with solution, 2 ‰ P contained compounds (by polyphosphoric acid 37%, tetra-sodium 28%, phosphoric acid 35% forms) and 1 ‰ soda ash add in preheating can, mix.
(2) oxidation: the material in preheating can is squeezed in oxidizing tower, blow to oxidizing tower by 35 cubic metres/tons per hour air quantity, when material in oxidizing tower is warming up to 150 ℃, start to excite, air quantity is brought up to 50 cubic metres/tons per hour, after 2 hours, in oxidizing tower, the temperature of material reaches 120～125 ℃, keep this temperature, air quantity is brought up to 60 cubic metres/tons per hour, start oxidation.The acid number of material in 1 hour detection oxidizing tower, when acid number reached 80～85mgKOH/g, oxidation finished.
(3) saponification: the material in oxidizing tower is squeezed in the saponification tank, added the water of saponification tank volume 30% left and right, temperature is controlled at 80～90 ℃, stirred 30 minutes, after stopping stirring, temperature remains on 85 ℃ and carries out sedimentation, and sedimentation was discharged waste water and middle 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 caustic soda soln that adds concentration 25%, keep caustic soda soln excessive, saponification 1 hour, recirculation saponification 1 hour, detecting pH value should be more than 13, otherwise continues saponification.
(4) composite: the saponification resultant that obtains in step (3) is incubated at 90 ℃, and sedimentation 3 hours, discharge waste water, saponification resultant, Yatall MA are joined in composite tank according to the ratio of 8:1, insulation, at 80 ℃, after mixing and stirring, obtains oxidized paraffin wax soap of the present invention.
Embodiment 3
(1) get the raw materials ready: paraffin is squeezed in preheating can, be warming up to 115 ℃ standby.With the paraffin weighing scale, after being mixed with solution, 1.8 ‰ P contained compounds (by polyphosphoric acid 40%, tetra-sodium 25%, phosphoric acid 35% forms) and 0.5 ‰ soda ash add in preheating can, mix.
(2) oxidation: the material in preheating can is squeezed in oxidizing tower, blow to oxidizing tower by 40 cubic metres/tons per hour air quantity, when material in oxidizing tower is warming up to 155 ℃, start to excite, air quantity is brought up to 45 cubic metres/tons per hour, after 2 hours, in oxidizing tower, the temperature of material reaches 120～125 ℃, keep this temperature, air quantity is brought up to 55 cubic metres/tons per hour, start oxidation.The acid number of material in 1 hour detection oxidizing tower, when acid number reached 80～85mgKOH/g, oxidation finished.
(3) saponification: the material in oxidizing tower 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 middle 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 caustic soda soln that adds concentration 25%, keep caustic soda soln excessive, saponification 1 hour, recirculation saponification 1 hour, detecting pH value should be more than 13, otherwise continues saponification.
(4) composite: the saponification resultant that obtains in step (3) is incubated at 90 ℃, and sedimentation 3 hours, discharge waste water, saponification resultant, Yatall MA are joined in composite tank according to the ratio of 8:1, insulation, at 80 ℃, after mixing and stirring, obtains oxidized paraffin wax soap of the present invention.
Above embodiment by getting the raw materials ready, oxidation, saponification and composite step form, and adopts P contained compound as catalyzer, shortened compared with the prior art oxidization time, the working substance content of oxidation resultant reaches more than 60%.With the finished product of the composite formation of Yatall MA, good to the selectivity of mineral, upgrade and the rate of recovery.
, 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 (6)
1. the preparation method of a novel oxidized paraffin wax soap is characterized in that being comprised of following steps:
(1) get the raw materials ready: paraffin is squeezed in preheating can, be warming up to 110-120 ℃ standby; With the paraffin weighing scale, after being mixed with solution, 1.5～2 ‰ P contained compounds and 0.5～1 ‰ soda ash adds in preheating can, mix;
(2) oxidation: the material in preheating can is squeezed in oxidizing tower, blow to oxidizing tower by 35-40 cubic meter/tons per hour air quantity, when material in oxidizing tower is warming up to 150-160 ℃, start to excite, air quantity is brought up to 40-50 cubic meter/tons per hour, after 2 hours, in oxidizing tower, the temperature of material reaches 120～125 ℃, keep this temperature, air quantity is brought up to 50-60 cubic meter/tons per hour, start oxidation; The acid number of material in 1 hour detection oxidizing tower, when acid number reached 80～85mgKOH/g, oxidation finished;
(3) saponification: the material in oxidizing tower 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, and sedimentation was discharged waste water and middle 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, adding mass percent concentration is 25% caustic soda soln, keep caustic soda soln excessive, saponification 1-2 hour, recirculation saponification 1-2 hour, detecting pH value should be more than 13, otherwise continues saponification;
(4) composite: the saponification resultant that obtains in step (3) is incubated at 90 ℃, and sedimentation 2-3 hour, discharge waste water, and saponification resultant is squeezed into composite tank, adds Yatall MA, and insulation, at 80-90 ℃, after mixing and stirring, obtains oxidized paraffin wax soap.
2. the preparation method of a kind of novel oxidized paraffin wax soap according to claim 1 is characterized in that P contained compound component and the weight percent in described step (1) is:
Polyphosphoric acid 35% ~ 40%
Tetra-sodium 20% ~ 30%
Phosphoric acid 35% ~ 40%.
3. the preparation method of a kind of novel oxidized paraffin wax soap according to claim 2 is characterized in that described P contained compound component and weight percent are:
Polyphosphoric acid 35%
Tetra-sodium 25%
Phosphatase 24 0%
4. the preparation method of according to claim 1-3 described a kind of novel oxidized paraffin wax soaps of any one, is characterized in that in described step (4), and composite with Yatall MA, wherein saponification resultant and Yatall MA weight ratio are 6～8:1～2.
5. the preparation method of a kind of novel oxidized paraffin wax soap described according to claim 4, is characterized in that described Yatall MA is rough Yatall MA, and its acid number is at 70～80mgKOH/g.
6. a novel oxidized paraffin wax soap, is characterized in that: be the oxidized paraffin wax soap that adopts the described method of claim 1-5 to prepare.
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| CN2012101414471A CN103387849A (en) | 2012-05-08 | 2012-05-08 | Novel oxyparaffin soap and preparation method thereof |
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| CN2012101414471A CN103387849A (en) | 2012-05-08 | 2012-05-08 | Novel oxyparaffin soap and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108543630A (en) * | 2018-04-11 | 2018-09-18 | 东北大学 | A method of preparing apatite collecting agent using paraffin base oil |
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2012
- 2012-05-08 CN CN2012101414471A patent/CN103387849A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108543630A (en) * | 2018-04-11 | 2018-09-18 | 东北大学 | A method of preparing apatite collecting agent using paraffin base oil |
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Application publication date: 20131113 |