CN113582838A - Tetrahydroxy sodium stearate and preparation method and application thereof - Google Patents
Tetrahydroxy sodium stearate and preparation method and application thereof Download PDFInfo
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- CN113582838A CN113582838A CN202110755262.9A CN202110755262A CN113582838A CN 113582838 A CN113582838 A CN 113582838A CN 202110755262 A CN202110755262 A CN 202110755262A CN 113582838 A CN113582838 A CN 113582838A
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- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 40
- 239000000194 fatty acid Substances 0.000 claims abstract description 40
- 229930195729 fatty acid Natural products 0.000 claims abstract description 40
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 40
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 33
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 32
- 239000011734 sodium Substances 0.000 claims abstract description 32
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000005188 flotation Methods 0.000 claims abstract description 23
- 235000019253 formic acid Nutrition 0.000 claims abstract description 17
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 claims abstract description 16
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- CUWPQXTXYVCXOM-UHFFFAOYSA-N 2,2,3,3-tetrahydroxyoctadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)(O)C(O)(O)C(O)=O CUWPQXTXYVCXOM-UHFFFAOYSA-N 0.000 claims description 11
- XGARGVMDSHCYSA-UHFFFAOYSA-M sodium 2,2,3,3-tetrahydroxyoctadecanoate Chemical compound OC(C(C(=O)[O-])(O)O)(CCCCCCCCCCCCCCC)O.[Na+] XGARGVMDSHCYSA-UHFFFAOYSA-M 0.000 claims description 11
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 7
- 239000010452 phosphate Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000002367 phosphate rock Substances 0.000 abstract description 4
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 abstract description 4
- 150000001450 anions Chemical class 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 description 34
- 239000002131 composite material Substances 0.000 description 10
- 239000003921 oil Substances 0.000 description 10
- 235000019198 oils Nutrition 0.000 description 10
- 239000006260 foam Substances 0.000 description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000001612 separation test Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000008396 flotation agent Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005580 one pot reaction Methods 0.000 description 2
- 239000012744 reinforcing agent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C59/00—Compounds having carboxyl groups bound to acyclic carbon atoms and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups
- C07C59/01—Saturated compounds having only one carboxyl group and containing hydroxy or O-metal groups
- C07C59/10—Polyhydroxy carboxylic acids
- C07C59/105—Polyhydroxy carboxylic acids having five or more carbon atoms, e.g. aldonic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
- B03D1/021—Froth-flotation processes for treatment of phosphate ores
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/367—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of functional groups containing oxygen only in singly bound form
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
- B03D2203/06—Phosphate ores
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a tetrahydroxy sodium stearate, a preparation method and an application thereof, wherein the preparation method comprises the following steps: s1, preparing tetrahydroxy fatty acid by using linoleic acid, formic acid and hydrogen peroxide; and S2, mixing the tetrahydroxy fatty acid with sodium hydroxide and water, heating to a first preset condition for reaction, discharging after the reaction is finished, and cooling to obtain the sodium tetrahydroxy stearate. According to the sodium tetrahydroxy stearate prepared by the invention, a group capable of being dissociated into anions and three hydroxyl groups with weaker hydrophobicity are formed at the hydrophilic end, so that the formed collector synergist is compounded with the existing collector, and the synergist is applied to the flotation of phosphorite to effectively improve the beneficiation benefit of the traditional collector and improve the separation property of the collector.
Description
Technical Field
The invention relates to the technical field of collecting agent reinforcing agents, and particularly relates to sodium tetrahydroxy stearate, and a preparation method and application thereof.
Background
Along with the continuous rise of the world oil price, natural renewable oil resources are attracted attention, the oil industry in China is in a rapid development period at present, the capacity of the oil industry mainly based on soybean oil is in a surplus trend, natural oil acid obtained by hydrolyzing natural oil is an important source in the oil chemical field, mainly comprises saturated fatty acid and unsaturated fatty acid, and various oil chemicals can be derived from the natural oil acid, so that the natural oil acid is widely developed and applied in the industry. The prior common fatty acid collecting agent has low separation efficiency, poor selectivity, hard water resistance, poor water solubility and poor low-temperature performance due to poor foam fluidity.
Therefore, how to develop a reinforcing agent to improve the performance of a fatty acid collector so as to improve the separation efficiency is a problem to be solved.
Disclosure of Invention
In view of the above, the invention aims to provide sodium tetrahydroxy stearate, a preparation method and an application thereof, so as to solve the problems of poor ore carrying capacity and poor sorting property of the traditional collecting agent.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a tetrahydroxy sodium stearate is characterized in that the molecular structural formula is as follows:
the invention also aims to provide a preparation method of the sodium tetrahydroxy stearate, which comprises the following steps:
s1, preparing tetrahydroxy fatty acid by using linoleic acid, formic acid and hydrogen peroxide;
and S2, mixing the tetrahydroxy fatty acid with sodium hydroxide and water, heating to a first preset condition for reaction, discharging after the reaction is finished, and cooling to obtain the sodium tetrahydroxy stearate.
In the above technical solution, optionally, the preparation of tetrahydroxy fatty acid using linoleic acid, formic acid and hydrogen peroxide in step S1 includes the steps of:
mixing the linoleic acid, the formic acid and the hydrogen peroxide, stirring and heating to a second preset condition for reaction, separating after the reaction is finished to obtain crude tetrahydroxy stearic acid, and then recrystallizing the crude tetrahydroxy stearic acid by ethyl acetate to obtain the tetrahydroxy fatty acid.
In the above technical solution, optionally, the mass ratio of the linoleic acid, the hydrogen peroxide, and the formic acid is 4: (6-10): (3-7).
In the above technical solution, optionally, the second preset condition includes a reaction temperature ranging from 65 ℃ to 80 ℃ and a reaction time ranging from 4h to 8 h.
In the above technical solution, optionally, the concentration of the hydrogen peroxide is 20% to 40%.
In the above technical solution, optionally, the first preset condition in step S2 includes a reaction temperature in a range of 70 ℃ to 120 ℃ and a reaction time in a range of 1h to 4 h.
In the above technical solution, optionally, in step S2, the mass ratio of the tetrahydroxy fatty acid, the sodium hydroxide, and the water is 60: (8-12): (30-120).
The third purpose of the invention is to provide the application of the sodium tetrahydroxy stearate, which is compounded with the fatty acid collecting agent and applied to the reverse flotation of the phosphorite.
In the above technical solution, optionally, the mass ratio of the sodium tetrahydroxystearate to the fatty acid collector is 1: (10-90).
Compared with the prior art, the sodium tetrahydroxy stearate provided by the invention and the preparation method and application thereof have the following advantages:
(1) the method directly synthesizes the tetrahydroxy fatty acid by a one-pot multi-step method, then saponifies the tetrahydroxy sodium stearate to synthesize the tetrahydroxy sodium stearate, and applies the tetrahydroxy sodium stearate to the complex use of the tetrahydroxy sodium stearate and the traditional fatty acid collecting agent, thereby effectively enhancing the ore carrying capacity and the sorting property of the traditional collecting agent.
(2) Compared with the existing collecting agent, the composite collecting agent prepared by using the tetrahydroxy sodium stearate has the advantages of high-efficiency selectivity on collophanite, strong mineral loading capacity, high foam fluidity, short foam scraping time, quick defoaming, no storage and high efficiency, and the dosage of the medicament is 0.65-1.2Kg/t of collophaniteThe foam scraping time is about 2-4min, the defoaming time is about 1-5min, the good collecting performance is achieved, and Ca is collected2\Mg2+The ions have better separation property and are suitable for the collophanite flotation field.
Drawings
FIG. 1 is a flow chart of a method for preparing sodium tetrahydroxystearate according to an embodiment of the present invention;
FIG. 2 is an electrospray mass spectrum of tetrahydroxy fatty acid prepared in the example of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the description of the present invention, it should be noted that the terms "first" and "second" mentioned in the embodiments of the present invention are only used for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
In the description of embodiments of the present application, the description of the term "some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Throughout this specification, the schematic representations of the terms used above do not necessarily refer to the same implementation or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
It should be noted that the term "in.. range" in this embodiment includes both end values, such as "in the range of 1 to 100" including both end values of 1 and 100.
The flotation is to change the hydrophobic and hydrophilic properties of the surface of the mineral by adding a flotation agent and then float the mineral according to the requirement to obtain the target mineral. The conventionally used floating titanium collecting agents mainly comprise MOS, ROB, HO, R-2, R-3, oxidized paraffin soap and emulsified tall oil, but the collecting agents have the defects of high price, narrow adaptive pH value range, poor stability of flotation indexes, high consumption of the collecting agents, unsatisfactory flotation indexes and the like. Therefore, it is of great significance to develop an enhancer to improve the performance of the fatty acid collector to improve the separation efficiency.
In order to achieve the purpose, the invention provides sodium tetrahydroxy stearate, which has the molecular structural formula:
according to the sodium tetrahydroxy stearate provided by the invention, a group capable of being dissociated into anions and three hydroxyl groups with weaker hydrophobicity are formed at the hydrophilic end, so that when the sodium tetrahydroxy stearate is used as a collector synergist and applied to the compounding of the existing collector, the mineral separation benefit of the traditional collector can be effectively improved in the flotation of phosphorite addition, and the separation property of the collector is improved.
Another embodiment of the present invention provides a method for preparing sodium tetrahydroxystearate, comprising the steps of:
s1, preparing tetrahydroxy fatty acid by using linoleic acid, formic acid and hydrogen peroxide;
and S2, mixing the tetrahydroxy fatty acid with sodium hydroxide and water, heating to a first preset condition for reaction, discharging after the reaction is finished, and cooling to obtain the sodium tetrahydroxy stearate.
The invention takes linoleic acid, hydrogen peroxide and formic acid as synthetic raw materials to synthesize tetrahydroxy fatty acid by a one-pot multi-step method, and then generates sodium tetrahydroxy fatty acid after saponification.
Specifically, in step S1, preparing tetrahydroxy fatty acid using linoleic acid, formic acid and hydrogen peroxide includes the steps of:
mixing linoleic acid, formic acid and hydrogen peroxide, stirring and heating to second preset conditions for reaction, separating after the reaction is finished to obtain crude tetrahydroxy stearic acid, and then recrystallizing the crude tetrahydroxy stearic acid by ethyl acetate to obtain tetrahydroxy fatty acid. The reaction has heat release phenomenon, and the dripping speed is strictly controlled so as to ensure that the temperature of the system is basically kept stable.
Wherein the mass ratio of linoleic acid, hydrogen peroxide and formic acid is 4: (6-10): (3-7), preferably, the mass ratio of linoleic acid, hydrogen peroxide and formic acid is 4: 8: 5; the concentration of hydrogen peroxide is 20% -40%, preferably, the concentration of hydrogen peroxide is 30%.
The second preset condition comprises that the reaction temperature is within the range of 65 ℃ to 80 ℃ and the reaction time is within the range of 4h to 8 h.
Specifically, in step S2, the first preset conditions include a reaction temperature in the range of 70 ℃ to 120 ℃ and a reaction time in the range of 1h to 4 h.
Wherein the mass ratio of the tetrahydroxy fatty acid to the sodium hydroxide to the water is 60: (8-12): (30-120), preferably, the mass ratio of the tetrahydroxy fatty acid to the sodium hydroxide to the water is 60: 10: 75.
another embodiment of the present invention provides a use of sodium tetrahydroxystearate as described above, comprising: the tetrahydroxy sodium stearate and the fatty acid collecting agent are compounded and applied to the reverse flotation of the phosphorite.
Further, the mass ratio of the sodium tetrahydroxy stearate to the fatty acid collector is 1: (10-90), preferably, the mass ratio of the sodium tetrahydroxystearate to the fatty acid collector is 1: 50.
the collophanite used in the embodiment of the invention is a collophanite of Yunan Haikou, and the chemical composition of the main elements is shown in Table 1:
TABLE 1 composition of major elements of a collophanite
The invention provides a using method of tetrahydroxy sodium stearate, which comprises the following steps:
preparing a composite collecting agent from sodium tetrahydroxy stearate and a fatty acid collecting agent according to a proportion;
grinding collophanite to fineness of-74 mu m and mass fraction of 75-90%, pouring into a flotation tank, adding water to obtain ore pulp with mass concentration of 20-35%, adding a phosphorus inhibitor into the ore pulp, then adding a composite collecting agent into the ore pulp, wherein the adding amount of the composite collecting agent is 0.65-1.2Kg/t collophanite, fully and uniformly stirring, and then performing flotation in the flotation tank by adopting a roughing process.
The flotation mode adopted by the invention is not limited to the method, and the mass fraction of the optimal grinding fineness (-0.74mm) accounts for 78.8% under the design condition of the preferential flotation process flow; the dosage of the medicament is 0.72 kg/t; acid inhibitor 20% sulfuric acid (YP) was used in the flotation agent for the rougher flotation test of the minerals at 10.85kg/t, respectively.
Compared with the existing collecting agent, the composite collecting agent provided by the invention has the advantages of high-efficiency selectivity on collophanite, strong ore loading capacity, high foam fluidity, short foam scraping time, quick defoaming and no problem of groove overflow caused by difficult foam elimination, and the dosage of the agent is 0.65-1.2Kg/t of collophanite. Wherein the foam scraping time is about 2-4min, the defoaming time is about 1-5min, the collecting performance is good, and Ca is collected2\Mg2+The ions have better separation property and are suitable for the collophanite flotation field.
On the basis of the above embodiments, the present invention will be further illustrated by the following specific examples of the preparation method and application of sodium tetrahydroxystearate. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by mass.
Example 1
The embodiment provides a preparation method of sodium tetrahydroxy stearate, which comprises the following steps:
s1, preparing tetrahydroxy fatty acid, namely mixing linoleic acid, hydrogen peroxide and formic acid according to the ratio of m (linoleic acid): m (30% H)2O2) Putting m (HCOOH) in a material ratio of 4:7:4.5 into a four-mouth reaction bottle with an electric stirrer, a thermometer, a dropping funnel and a condensing tube, and putting the reaction bottle into a constant-temperature water bath; stirring and heating to 30-35 ℃, and then dropwise adding hydrogen peroxide at a constant speed; after the dripping is finishedAnd after the temperature is stable, the temperature of the system is adjusted to 65-70 ℃ and the reaction is stopped after 6 hours. After the reaction is finished, transferring the reaction solution into a separating funnel, washing the reaction solution with hot water to be neutral, removing water and a solvent by rotary evaporation to obtain a viscous liquid, namely a tetrahydroxy stearic acid (THSA) crude product, and recrystallizing the tetrahydroxy stearic acid (THSA) crude product with ethyl acetate to obtain the tetrahydroxy fatty acid.
S2, preparing tetrahydroxy fatty acid sodium: mixing the tetrahydroxy fatty acid prepared in the step S1 with sodium hydroxide and water in a mass ratio of 60: 10: 70, putting the mixture into a reaction bottle, heating the mixture to 90 ℃, stirring the mixture for reaction for 2 hours, discharging the mixture after the reaction is finished, and cooling the mixture to obtain the sodium tetrahydroxy stearate.
FIG. 2 is an electrospray mass spectrum of the tetrahydroxy fatty acid prepared in step S1, and the electrospray mass spectrum is used for measuring the molecular weight after purification in negative ion mode, and the spectrum is shown in the figure, wherein the peak at 347.41 in the diagram is the [ M-1] peak after one H is lost, and is consistent with the molecular weight of the tetrahydroxy fatty acid of 348.25.
Example 2
The embodiment provides an application of sodium tetrahydroxy stearate in the field of reverse flotation of phosphate ore, which comprises the following steps:
preparing a collecting agent AB-1: the prepared sodium tetrahydroxy stearate (B) and a traditional collecting agent FS (A) provided by Wuhan Qiangsheng science and technology Limited are uniformly mixed according to the ratio of A to B being 11 to 1 to prepare a 2% composite collecting agent which is marked as AB-1, and the rough separation test is carried out on a certain collophanite in Yunnan, and the results are shown in Table 2.
Example 3
The embodiment provides an application of sodium tetrahydroxy stearate in the field of reverse flotation of phosphate ore, which comprises the following steps:
preparing a collecting agent AB-2: the prepared sodium tetrahydroxy stearate (B) and a traditional collecting agent FS (A) provided by Wuhan Qiangsheng science and technology Limited are uniformly mixed according to the ratio of A to B being 5 to 1 to prepare a 2% composite collecting agent which is marked as AB-2, and the rough separation test is carried out on a certain collophanite in Yunnan, and the results are shown in Table 2.
Example 4
The embodiment provides an application of sodium tetrahydroxy stearate in the field of reverse flotation of phosphate ore, which comprises the following steps:
preparing a collecting agent AB-3: the prepared sodium tetrahydroxy stearate (B) and a traditional collecting agent FS (A) provided by Wuhan Qiangsheng science and technology Limited are uniformly mixed according to the ratio of A to B being 3 to 1 to prepare a 2% composite collecting agent which is marked as AB-3, and the rough separation test is carried out on a certain collophanite in Yunnan, and the results are shown in Table 2.
Example 5
The embodiment provides an application of sodium tetrahydroxy stearate in the field of reverse flotation of phosphate ore, which comprises the following steps:
preparing a collecting agent AB-4: the prepared sodium tetrahydroxy stearate (B) and a traditional collecting agent FS (A) provided by Wuhan Qiangsheng science and technology Limited are uniformly mixed according to the ratio of A to B being 2 to 1 to prepare a 2% composite collecting agent which is marked as AB-4, and the rough separation test is carried out on a certain collophanite in Yunnan, and the results are shown in Table 2.
Example 6
The embodiment provides an application of sodium tetrahydroxy stearate in the field of reverse flotation of phosphate ore, which comprises the following steps:
preparing a collecting agent AB-5: the prepared sodium tetrahydroxy stearate (B) and a traditional collecting agent FS (A) provided by Wuhan Qiangsheng science and technology Limited are uniformly mixed according to the ratio of A to B being 1 to prepare a 2% composite collecting agent which is marked as AB-5, and the rough separation test is carried out on a certain collophanite in Yunnan, and the results are shown in Table 2.
Comparative example 1
Commercial products: collector fs (a) is offered by wuhan dynasty science and technology limited.
TABLE 2 results of roughing tests carried out in examples 2-6 and comparative example 1
As can be seen from the data analysis of Table 2, the effect of the primary roughing by using the collector compounded by the collector A and the collector B provided by the invention at normal temperature is obviously superior to the effect of the existing collector A used alone on the market in the aspects of improving the grade of phosphate concentrate, removing magnesium oxide, enhancing the beneficiation efficiency and the like.
As shown in table 2, when a: B ═ 11:1, namely the mass ratio of the sodium tetrahydroxy stearate to the fatty acid collector is 1: at 11 time, P2O5The grade of the collector A is 2.72 percentage points higher than that of the collector A used alone; the beneficiation efficiency is improved by more than one time compared with that of the collector A used alone; the magnesium removal rate is improved by 45.15 percent; the result shows that the sodium tetrahydroxy stearate as the synergist has good sorting property and can effectively enhance the mineral separation efficiency; and is far superior to the single use of the collector A; meanwhile, the flotation performance of the collector can be effectively enhanced only by adding a small amount of sodium tetrahydroxy stearate in practical flotation application.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (10)
1. A tetrahydroxy sodium stearate is characterized in that the molecular structural formula is as follows:
2. the method of preparing sodium tetrahydroxystearate according to claim 1, comprising the steps of:
s1, preparing tetrahydroxy fatty acid by using linoleic acid, formic acid and hydrogen peroxide;
and S2, mixing the tetrahydroxy fatty acid with sodium hydroxide and water, heating to a first preset condition for reaction, discharging after the reaction is finished, and cooling to obtain the sodium tetrahydroxy stearate.
3. The method for preparing sodium tetrahydroxystearate according to claim 2, wherein the step S1 of preparing tetrahydroxystearate from linoleic acid, formic acid and hydrogen peroxide comprises the steps of:
mixing the linoleic acid, the formic acid and the hydrogen peroxide, stirring and heating to a second preset condition for reaction, separating after the reaction is finished to obtain crude tetrahydroxy stearic acid, and then recrystallizing the crude tetrahydroxy stearic acid by ethyl acetate to obtain the tetrahydroxy fatty acid.
4. The method according to claim 3, wherein the mass ratio of linoleic acid, hydrogen peroxide and formic acid is 4: (6-10): (3-7).
5. The method of claim 3, wherein the second predetermined condition comprises a reaction temperature ranging from 65 ℃ to 80 ℃ and a reaction time ranging from 4h to 8 h.
6. The method of any one of claims 3 to 5, wherein the concentration of hydrogen peroxide is 20% to 40%.
7. The method of claim 2, wherein the first predetermined condition in step S2 includes a reaction temperature ranging from 70 ℃ to 120 ℃ and a reaction time ranging from 1h to 4 h.
8. The method according to claim 7, wherein the mass ratio of the tetrahydroxy fatty acid, the sodium hydroxide and the water in step S2 is 60: (8-12): (30-120).
9. The use of sodium tetrahydroxystearate according to claim 1, wherein the sodium tetrahydroxystearate is combined with a fatty acid collector for reverse flotation of phosphate ore.
10. The use according to claim 9, wherein the mass ratio of the sodium tetrahydroxystearate to the fatty acid collector is 1: (10-90).
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