CN113843048A - Polyhydroxy fatty acid sodium soap and preparation method and application thereof - Google Patents
Polyhydroxy fatty acid sodium soap and preparation method and application thereof Download PDFInfo
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- CN113843048A CN113843048A CN202111079885.5A CN202111079885A CN113843048A CN 113843048 A CN113843048 A CN 113843048A CN 202111079885 A CN202111079885 A CN 202111079885A CN 113843048 A CN113843048 A CN 113843048A
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- fatty acid
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- 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
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- 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
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- 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
Abstract
The invention provides a polyhydroxy fatty acid sodium soap and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing mixed fatty acid with formic acid and hydrogen peroxide to prepare polyhydroxy fatty acid, wherein the mixed fatty acid comprises unsaturated fatty acid; and mixing the polyhydroxy fatty acid with sodium hydroxide and water, reacting under a first preset condition, discharging and cooling after the reaction is finished, and thus obtaining the polyhydroxy fatty acid sodium soap. According to the invention, polyhydroxy fatty acid is directly synthesized by adopting a one-pot multi-step method, and then the polyhydroxy fatty acid sodium soap is synthesized by saponification, and because a plurality of hydroxyl groups with weaker hydrophobicity are added, the prepared polyhydroxy fatty acid sodium soap is applied to the flotation of phosphorite, so that the mineral separation benefit and the sorting property can be effectively improved.
Description
Technical Field
The invention relates to the technical field of phosphorite collecting agents, and particularly relates to a polyhydroxy fatty acid sodium soap and a preparation method and application thereof.
Background
Phosphorite is a strategic non-metallic mineral resource and is the key of phosphate fertilizer production, and the stable supply of the phosphorus resource is related to the world food supply safety problem. The reserves of phosphate rock resources in China are abundant, but with the exploitation and utilization for many years, the remaining phosphate resources are middle-grade and low-grade phosphate rocks, most of the phosphate rock resources are collophanite, the ore exploitation and separation are difficult, the economic treatment cost is high, and the phosphate rock resources can be used for downstream after being processed, separated and purified by minerals. Therefore, the method has great significance for strengthening the research on the development and utilization technology of phosphorus resources, particularly for the research on the development and utilization technology of middle-low grade collophanite resources, realizing the sustainable development of phosphorus resource utilization in China, ensuring national food safety and stable and healthy development of national economy.
The phosphorite flotation is an efficient and feasible separation process and is widely applied to the phosphorite separation industry, and the collecting agent is the core for separating useful minerals and gangue. At present, the composite collector prepared by adding fatty acid saponification products or other modification aids into modified fatty acids is the most widely applied in industry, and compounding or modifying the fatty acid collector is the main research direction for improving the performance of the collector.
Disclosure of Invention
In view of the above, the invention provides a polyhydroxy fatty acid sodium soap and a preparation method and application thereof, and aims to solve the problems that the existing collecting agent has high-efficiency selectivity and strong ore carrying capacity on collophanite.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a sodium polyhydroxy fatty acid soap comprises the following components in percentage by mass: 30 to 80 percent of mixed sodium fatty acid, 5 to 40 percent of dihydroxy sodium stearate and 2 to 40 percent of tetrahydroxy sodium fatty acid.
The invention also aims to provide a preparation method of the polyhydroxy fatty acid sodium soap, which comprises the following steps:
s1, mixing the mixed fatty acid with formic acid and hydrogen peroxide to prepare polyhydroxy fatty acid, wherein the mixed fatty acid comprises unsaturated fatty acid;
s2, mixing the polyhydroxy fatty acid with sodium hydroxide and water, reacting under a first preset condition, discharging and cooling after the reaction is finished, and obtaining the polyhydroxy fatty acid sodium soap.
Alternatively, in step S1, the mixing the mixed fatty acid with formic acid and hydrogen peroxide to prepare polyhydroxy fatty acid comprises the steps of:
and mixing the mixed fatty acid, the formic acid and the hydrogen peroxide, reacting under a second preset condition, and removing a water layer after the reaction is finished to obtain the polyhydroxy fatty acid.
Optionally, in step S1, the mass ratio of the mixed fatty acid, the formic acid, and the hydrogen peroxide is in a range of 4:7:5 to 8:7: 5.
Optionally, in step S1, the second preset condition includes: the reaction temperature is in the range of 65 ℃ to 80 ℃, the reaction time is in the range of 4h to 8h, and the heating rate is in the range of 1 ℃ to 2 ℃ for 1 min.
Optionally, in step S1, the content of the unsaturated fatty acid in the mixed fatty acid is in the range of 5% to 70%, and the concentration of the hydrogen peroxide is in the range of 28% to 32%.
Optionally, in step S2, the first preset condition includes: the reaction temperature is in the range of 70 ℃ to 120 ℃ and the reaction time is in the range of 1h to 4 h.
Optionally, in step S2, the mass ratio of the polyhydroxy fatty acid, the sodium hydroxide, and the water is in the range of 60:8:30 to 60:12: 120.
The third purpose of the invention is to provide an application of the above-mentioned polyhydroxy fatty acid sodium soap, which applies the polyhydroxy fatty acid sodium soap to phosphorite flotation.
Optionally, the specific use method includes: grinding collophanite, pouring the ground collophanite into a flotation tank, adding water and stirring to obtain ore pulp; adding a phosphorus inhibitor and the polyhydroxy fatty acid sodium soap into the ore pulp, and uniformly stirring; and finally, performing flotation in the flotation tank by adopting a roughing process.
Compared with the prior art, the polyhydroxy fatty acid sodium soap provided by the invention and the preparation method and application thereof have the following advantages:
(1) according to the invention, polyhydroxy fatty acid is directly synthesized by adopting a one-pot multi-step method, and then the polyhydroxy fatty acid sodium soap is synthesized by saponification, and because a plurality of hydroxyl groups with weaker hydrophobicity are added, the prepared polyhydroxy fatty acid sodium soap is applied to the flotation of phosphorite, so that the mineral separation benefit and the sorting property can be effectively improved.
(2) The preparation method is simple, low in energy consumption and high in yield, and has the potential of marketization popularization.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, the drawings needed for the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is an infrared spectrum of a polyhydroxy fatty acid in accordance with an embodiment 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.
It should be noted that in the description of the embodiments herein, 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.
The term "in.. range" as used herein includes both ends, such as "in the range of 1 to 100" including both ends of 1 and 100.
The embodiment of the invention provides a polyhydroxy fatty acid sodium soap which comprises the following components in percentage by mass: 30 to 80 percent of mixed sodium fatty acid, 5 to 40 percent of dihydroxy sodium stearate and 2 to 40 percent of tetrahydroxy sodium fatty acid.
It is understood that the flotation is to change the hydrophobic and hydrophilic properties of the mineral surface by the added flotation agent and then to obtain the target mineral by flotation according to the needs. The conventional collectors mainly comprise MOS, ROB, HO, R-2, R-3, oxidized paraffin soap and emulsified tall oil, but the collectors have the defects of high price, narrow adaptive pH value range, poor stability of flotation indexes, high consumption of the collectors, unsatisfactory flotation indexes and the like.
The novel phosphorus ore collecting agent polyhydroxy fatty acid sodium soap provided by the invention contains a plurality of hydroxyl groups with weaker hydrophobicity, so that when the soap is used as a collecting agent for phosphorus ore flotation, the mineral separation benefit can be effectively increased, and the separation property of the collecting agent is improved.
Another embodiment of the present invention provides a preparation method of the above sodium polyhydroxy fatty acid soap, which comprises the following steps:
s1, mixing the mixed fatty acid with formic acid and hydrogen peroxide to prepare polyhydroxy fatty acid, wherein the mixed fatty acid contains unsaturated fatty acid;
s2, mixing the polyhydroxy fatty acid with sodium hydroxide and water, reacting under a first preset condition, discharging and cooling after the reaction is finished, and obtaining the polyhydroxy fatty acid sodium soap.
The invention adopts a one-pot multi-step method to directly synthesize polyhydroxy fatty acid and then saponify to synthesize polyhydroxy fatty acid sodium soap, and has the advantages of simple preparation method, low energy consumption, high yield and market popularization potential.
Specifically, in step S1, mixing the mixed fatty acid with formic acid and hydrogen peroxide to prepare polyhydroxy fatty acid, comprising the steps of: mixing the mixed fatty acid, formic acid and hydrogen peroxide, reacting under a second preset condition, and removing a water layer after the reaction is finished to obtain the polyhydroxy fatty acid.
Wherein the mass ratio of the mixed fatty acid, formic acid and hydrogen peroxide is in the range of 4:7:5 to 8:7: 5.
The second preset condition for the reaction of the mixed fatty acid, the formic acid and the hydrogen peroxide after mixing comprises the following steps: the reaction temperature is in the range of 65 ℃ to 80 ℃, the reaction time is in the range of 4h to 8h, and the heating rate is in the range of 1 ℃ to 2 ℃ for 1 min. Preferably, the temperature rise rate is 1 ℃ for 1min, and the reaction is carried out at 70 ℃ for 6 h.
Further, the content of unsaturated fatty acid in the mixed fatty acid is in the range of 5% to 70%, and the concentration of hydrogen peroxide is in the range of 28% to 32%.
Specifically, in step S2, the first preset conditions for the reaction of the polyhydroxy fatty acid after mixing with sodium hydroxide and water include: the reaction temperature is in the range of 70 ℃ to 120 ℃ and the reaction time is in the range of 1h to 4 h. Preferably, the reaction is carried out at 95 ℃ for 2.5 h.
Wherein the mass ratio of the polyhydroxy fatty acid to the sodium hydroxide to the water is in the range of 60:8:30 to 60:12: 120.
The invention further provides an application of the polyhydroxy fatty acid sodium soap, which is to apply the polyhydroxy fatty acid sodium soap to phosphorite flotation.
The collophanite used in the embodiment of the invention is Hubei Songzi collophanite, and the chemical composition of the main elements is shown in Table 1:
TABLE 1 composition of major elements of a collophanite
The specific using method comprises the following steps:
preparing the prepared polyhydroxy fatty acid sodium soap into 2% collecting agent solution, grinding collophanite, pouring into a flotation tank, adding water and stirring into ore pulp; adding a phosphorus inhibitor and a polyhydroxy fatty acid sodium soap into the ore pulp, and uniformly stirring; and finally, performing flotation in a flotation tank by adopting a roughing process.
Preferably, the collophanite is ground until the grinding fineness is-0.074 mm and the mass fraction reaches 75-90%, the ground collophanite is poured into a flotation tank, water is added to obtain ore pulp with the mass concentration of 20-35%, a phosphorus inhibitor is added, then the collecting agent solution is added into the ore pulp, the adding amount of the collecting agent solution is 0.65-1.2Kg of 1t collophanite, the mixture is fully and uniformly stirred, and then the collophanite is subjected to flotation by adopting a roughing process in the flotation tank.
Compared with the existing collecting agent, the hydroxy fatty acid sodium soap collecting agent provided by the invention has the advantages of high-efficiency selectivity on collophanite, strong ore carrying capacity, high foam fluidity, short foam scraping time, quick defoaming and no problem of overflow caused by difficult foam removal, and the dosage of the agent is 0.65-1.2Kg1 t. Tests show that the foam scraping time is about 2-4min, the defoaming time is about 1-5min, the high-efficiency calcium carbonate collector has good collecting performance and can be used for Ca2\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 the sodium soap of polyhydroxy fatty acid. 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 a polyhydroxy fatty acid sodium soap, which comprises the following steps:
1) preparation of polyhydroxy fatty acids: mixing fatty acid, hydrogen peroxide and formic acid, wherein m (unsaturated fatty acid content) is m (30% H)2O2) Putting the material with the ratio of m (HCOOH) to 8:7:5 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; heating to 30-35 deg.C under stirring, and dripping hydrogen peroxide at uniform speed; the reaction has a heat release phenomenon, the dropping speed is strictly controlled to ensure that the temperature of the system is basically kept stable, after the dropping is finished and the temperature is stable, the temperature of the system is adjusted to 65 ℃ of reaction temperature, and the reaction is stopped after 6 hours; after the reaction is finished, removing a water layer while the reaction is hot, and washing the reaction product to be neutral to obtain polyhydroxy fatty acid;
2) mixing the obtained polyhydroxy fatty acid with sodium hydroxide and water in a mass ratio of 60: 9: 80, putting the mixture into a reaction bottle, heating the mixture to 90 ℃, stirring the mixture for reaction for 1 hour, discharging the mixture after the reaction is finished, and cooling the mixture to obtain the collecting agent polyhydroxy fatty acid sodium soap.
The application comprises the following steps: the sodium soap of polyhydroxy fatty acid prepared in example 1 was prepared as a 2% solution and used in a pilot plant for reverse flotation of phosphate ore, with the results shown in table 2.
The polyhydroxy fatty acid obtained in step 1) of example 1 was characterized by an infrared spectrum, yielding the result diagram shown in FIG. 1; as can be seen from fig. 1, the unsaturated hydrocarbon stretching vibration peak at which C ═ C is present does not appear (generally, a small sharp peak of not more than 3000 is shown)) And appeared to be located at 3345cm-1、3375cm-1And (3) characterizing the strong absorption peak existing in the alcoholic hydroxyl group, wherein the two absorption peaks can be used as the basis for existence. 1706cm-1Is C ═ O base stretching vibration, 1206--1For C-O stretching vibration in carbonyl, 938cm-1Vibration of out-of-plane deformation of carboxyl-OH, 619cm-1Is characterized by n>4, C-C, skeleton vibrational peak. Analysis of the infrared spectrogram shows that each peak on the infrared spectrogram corresponds to the functional group to be possessed one by one, and the raw material oleic acid is converted into 9, 10-dihydroxystearic acid through reaction.
Example 2
This example provides a process for the preparation of a sodium soap of polyhydroxy fatty acid, differing from example 1 in that:
in the step 1), mixing fatty acid, hydrogen peroxide and formic acid according to the ratio of m (content of unsaturated fatty acid): m (30% H)2O2) M (HCOOH) is fed according to the material ratio of 7:7:5, and the reaction temperature is 70 ℃;
the remaining steps and parameters were the same as in example 1.
The sodium soap of polyhydroxy fatty acid prepared in example 2 was prepared as a 2% solution and used in a pilot plant for reverse flotation of phosphate ore, with the results shown in table 2.
Example 3
This example provides a process for the preparation of a sodium soap of polyhydroxy fatty acid, differing from example 1 in that:
in the step 1), mixing fatty acid, hydrogen peroxide and formic acid according to the ratio of m (content of unsaturated fatty acid): m (30% H)2O2) M (HCOOH) is fed according to the material ratio of 6.5:7: 5;
the remaining steps and parameters were the same as in example 1.
The sodium soap of polyhydroxy fatty acid prepared in example 3 was prepared as a 2% solution and used in a pilot plant for reverse flotation of phosphate ore, with the results shown in table 2.
Comparative example 1
Commercial products: collector FS provided by wuhan dynasty science ltd; FS was prepared as a 2% solution and used in a reverse flotation pilot plant for phosphate rock with results as shown in table 2.
TABLE 2 results of roughing tests carried out in examples 1-3 and comparative example 1
As can be seen from the data analysis of Table 2, compared with the traditional collecting agent, the collecting agent of the polyhydroxy fatty acid sodium soap prepared by the invention has obviously excellent performance and good application prospect.
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 sodium polyhydroxy fatty acid soap is characterized by comprising the following components in percentage by mass: 30 to 80 percent of mixed sodium fatty acid, 5 to 40 percent of dihydroxy sodium stearate and 2 to 40 percent of tetrahydroxy sodium fatty acid.
2. The method for preparing a sodium polyhydroxyfatty acid soap according to claim 1, comprising the steps of:
s1, mixing the mixed fatty acid with formic acid and hydrogen peroxide to prepare polyhydroxy fatty acid, wherein the mixed fatty acid comprises unsaturated fatty acid;
s2, mixing the polyhydroxy fatty acid with sodium hydroxide and water, reacting under a first preset condition, discharging and cooling after the reaction is finished, and obtaining the polyhydroxy fatty acid sodium soap.
3. The method of claim 2, wherein the step S1 of mixing the mixed fatty acid with formic acid and hydrogen peroxide to prepare polyhydroxy fatty acid comprises the steps of:
and mixing the mixed fatty acid, the formic acid and the hydrogen peroxide, reacting under a second preset condition, and removing a water layer after the reaction is finished to obtain the polyhydroxy fatty acid.
4. The production method according to claim 3, wherein in step S1, the mass ratio of the mixed fatty acid, the formic acid, and the hydrogen peroxide is in the range of 4:7:5 to 8:7: 5.
5. The method according to claim 4, wherein in step S1, the second preset condition includes: the reaction temperature is in the range of 65 ℃ to 80 ℃, the reaction time is in the range of 4h to 8h, and the heating rate is in the range of 1 ℃ to 2 ℃ for 1 min.
6. The method according to any one of claims 2 to 5, wherein in step S1, the content of the unsaturated fatty acid in the mixed fatty acid is in the range of 5% to 70%, and the concentration of the hydrogen peroxide is in the range of 28% to 32%.
7. The method according to claim 6, wherein in step S2, the first preset condition includes: the reaction temperature is in the range of 70 ℃ to 120 ℃ and the reaction time is in the range of 1h to 4 h.
8. The method according to claim 7, wherein in step S2, the mass ratio of the polyhydroxy fatty acid, the sodium hydroxide and the water is in the range of 60:8:30 to 60:12: 120.
9. Use of the sodium soap of polyhydroxy fatty acid according to claim 1, characterized in that the sodium soap of polyhydroxy fatty acid is used for phosphorite flotation.
10. The application of claim 9, wherein the specific usage method comprises: grinding collophanite, pouring the ground collophanite into a flotation tank, adding water and stirring to obtain ore pulp; adding a phosphorus inhibitor and the polyhydroxy fatty acid sodium soap into the ore pulp, and uniformly stirring; and finally, performing flotation in the flotation tank by adopting a roughing process.
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Cited By (1)
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| CN114656425A (en) * | 2022-04-07 | 2022-06-24 | 昆明理工大学 | Collecting agent applied to cassiterite flotation, synthetic method and application |
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