Collecting agent for reducing collophanite sesquioxide and preparation method and application thereof

Abstract

The invention discloses a collecting agent for reducing collophanite sesquioxide and a preparation method and application thereof.An interfacial activity enhancer, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether are mixed and then stirred, the mixture is put into an ultrasonic device to be subjected to ultrasonic treatment, then the mixture is put into an ether amine salt water solution to be stirred, and the collecting agent is obtained. And the collecting agent for reducing collophanite sesquioxide is obtained. The collecting agent shows high selectivity on collophanite separation, and the problems that reverse flotation products are poor in foam flowability and not prone to being broken can be remarkably solved; according to the application of the collecting agent for reducing the collophanite sesquioxide, the particle size of an ore grinding product can be regulated and controlled, the influence of fine particles generated by over-grinding on the collecting agent can be reduced, the recovery rate of phosphorite and the grade of phosphate concentrate are remarkably improved, and meanwhile deep impurity removal is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of collophanite reverse flotation collectors, and in particular to a collector for reducing collophanite sesquioxides, a preparation method and application thereof. Background Art

[0002] China's phosphate ore is mainly composed of collophanites rich in silicate, carbonate and other gangue minerals. These minerals have the characteristics of complex composition, fine crystals and great difficulty in sorting.

[0003] In the existing field of phosphate flotation technology, direct flotation is usually used to achieve effective separation of phosphate resources that are easy to beneficiate. The conventional single reverse flotation process mainly uses fatty acid soap anionic collectors in a weakly acidic environment to separate associated gangue minerals such as dolomite from phosphate minerals, thereby reducing the content of magnesium oxides and improving the quality of phosphate concentrates. However, this agent still has problems such as high flotation temperature, high tailings grade, and low recovery rate in actual application.

[0004] For phosphate resources with high magnesium content and rich silicon, it is more advantageous to implement direct and reverse flotation or double reverse flotation process. Although the direct and reverse flotation method is limited in application due to the complexity of the process and high cost, the double reverse flotation process shows higher rationality and efficiency in the treatment of such phosphate resources. In this process, the commonly used amine reagents show effectiveness, but also face a series of challenges such as large foaming volume, viscous foam, difficulty in defoaming, poor fluidity, difficulty in handling foam products, poor selectivity and sensitivity to ore slime, which seriously affect the flotation efficiency.

[0005] In summary, there is an urgent need for a collector for reducing the sesquioxides of collophane with high selectivity, good flotation performance, the ability to get rid of strong acid, which can effectively reduce the sesquioxide content in the concentrate product and significantly improve the grade and recovery rate of phosphate ore flotation. Summary of the invention

[0006] The purpose of the present invention is to overcome the shortcomings of the existing collophanite reverse flotation collector, provide a collector for reducing the sesquioxide of collophanite, which can be applied to the reverse flotation process of collophanite, has good flotation performance and high selectivity, can achieve efficient enrichment of P2O5 during the flotation process, effectively reduce the sesquioxide content in the concentrate product and significantly improve the recovery rate of phosphate flotation. In addition, the problem of poor foam fluidity and difficulty in breaking in the reverse flotation product is improved; the near-alkalinity standard requirements for direct discharge of return water are met, which is conducive to environmental sustainable development.

[0007] To achieve the above technical purpose, the technical solution provided by the present invention is: a collector for reducing the sesquioxide of collophanite, characterized in that it is composed of the following components in percentage by mass: 30% to 50% of an aqueous solution of ether amine salt, 30% to 60% of a surfactant enhancer, 5% to 10% of ammonium lauryl sulfate, and 5% to 10% of sorbitan monooleate polyoxyethylene ether, wherein the surfactant enhancer is one of an aqueous solution of alcohol, an aqueous solution of ether, and an aqueous solution of non-polar oil.

[0008] The above-mentioned collector for reducing the sesquioxide of collophanite is characterized in that it is composed of the following components in percentage by mass: 40% of the aqueous solution of the ether amine salt, 40% of the interfacial activity enhancer, 10% of the dodecyl ammonium sulfate, and 10% of the dehydrated sorbitan monooleate polyoxyethylene ether.

[0009] The above-mentioned collector for reducing the sesquioxide of collophanite is characterized in that the mass percentage of ether amine salt in the aqueous solution of ether amine salt is 20% to 40%, the mass percentage of solute in the interfacial activity enhancer is 20% to 40%, the alcohol is one or a combination of polydimethylsiloxane, polydiethylsiloxane and PPG type polypropylene glycol, the ether is polyoxypropylene glycerol ether, and the non-polar oil is aviation kerosene and / or light diesel oil.

[0010] The above-mentioned collector for reducing sesquioxide of collophanite is characterized in that the mass percentage of ether amine salt in the aqueous solution of ether amine salt is 40%, and the mass percentage of solute in the interfacial activity enhancer is 30%.

[0011] Another object of the present invention is to be able to obtain the collector simply and quickly.

[0012] To achieve the above object, the technical solution of the present invention is to provide a method for preparing a collector for reducing sesquioxide of collophanite, characterized in that the method comprises the following steps:

[0013] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring the mixture, and then placing the mixture in an ultrasonic device for ultrasonic dispersion to obtain a mixture;

[0014] Step 2: placing the mixture obtained in step 1 into an aqueous solution of ether amine salt and stirring to obtain a collector.

[0015] The above-mentioned method for preparing a collector for reducing sesquioxide of collophosphate is characterized in that the stirring in step 1 and step 2 is carried out by using a magnetic stirrer, the stirring rate of the magnetic stirrer is 300r / min~500r / min, and the stirring time is 20min~30min; the ultrasonic device in step 1 is an ultrasonic disperser, the ultrasonic temperature is 40℃~50℃, and the ultrasonic time is 30min~60min.

[0016] The third object of the present invention is to be able to apply the collector of the present invention in actual processes, and by optimizing the process, significantly improve the recovery rate of phosphate ore and the grade of phosphate concentrate; at the same time, the process is simple, low-cost, and suitable for industrial application.

[0017] In order to achieve the above object, the technical solution provided by the present invention is: an application of a collector for reducing the sesquioxide of collophanite, characterized in that it comprises the following steps:

[0018] Step 1: prepare grinding water and collophanite sample in equal mass proportions, add the collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, specifically comprising the following steps:

[0019] Step 101, mixing the collophanite sample with the first batch of water, placing the mixture in the rod mill for first-stage grinding to obtain a ore-water mixture;

[0020] Step 102, adding a second batch of water to the ore-water mixture obtained in step 101 to perform a second stage of grinding to obtain a slurry roughing solution;

[0021] Step 103, the roughing liquid obtained in step 102 is screened through a drum screen to obtain coarse ore particles and fine ore slurry, and the coarse ore particles are sequentially returned to perform the third stage of grinding;

[0022] Step 2, feeding the slurry obtained in step 103 into a flotation machine, and adding the collector into the flotation machine to perform flotation roughing to obtain a flotation rough concentrate and a roughing tailing;

[0023] Step 3, feeding the flotation rough concentrate obtained in step 2 into a flotation machine, and adding an acidic adjuster into the flotation machine to adjust the pH to obtain a weakly acidic ore pulp;

[0024] Step 4: adding a de-magnesium collector to the weakly acidic slurry obtained in step 3 and then flotation separation to obtain concentrate and tailings II;

[0025] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0026] The above-mentioned application of a collector for reducing sesquioxides of collophanite is characterized in that the grinding medium of the rod mill in step 1 is a steel rod, and the steel rod is composed of at least three steel rods with different diameters, and the diameters of the three steel rods are Φ75mm, Φ65mm and Φ50mm respectively; the mass ratio of the Φ75mm steel rod, the Φ65mm steel rod and the Φ50mm steel rod is 4:4:2;

[0027] In step 101, the mass of the first batch of water accounts for 60% to 70% of the mass of the grinding water, and the grinding time of the first stage of grinding is 2 minutes; in step 102, the grinding time of the second stage of grinding is 2 minutes.

[0028] The above-mentioned method for using a collector to reduce the sesquioxide of collophanite is characterized in that the amount of the collector in step 2 is 400g to 800g / t of collophanite sample, and the pH of the flotation rough concentrate in step 2 is 7 to 9;

[0029] The acidic regulator in step 3 is phosphoric acid and / or sulfuric acid, and the amount of the acidic regulator is 2kg to 6kg / t of collophanite sample;

[0030] The demagnesiumizing collector in step 4 is oleic acid or cyclohexane acid, and the dosage of the demagnesiumizing collector is 100g to 400g / t of collophanite sample.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] 1. The collector for reducing the sesquioxide of collophanite of the present invention introduces a hydrophilic group etheroxy group into the collector by modifying the etheramine salt obtained by dodecylamine, thereby increasing the solubility of the collector, enhancing the adsorption of the collector at the gas-liquid interface, further improving the foaming performance, and enhancing the collector's collection ability and selectivity for silicate minerals.

[0033] 2. The preparation method of a collector for reducing the sesquioxide of collophanite of the present invention adopts an aqueous solution of alcohol, an aqueous solution of ether or an aqueous solution of non-polar oil as an interfacial activity enhancer, which can effectively ensure that the collector has a good collecting effect while enhancing the fluidity of the foam and making the foam easy to break; since the use of a large amount of sulfuric acid is avoided in the flotation process using the collector, the pH of the flotation rough concentrate is maintained at 7-9, thereby improving the universality of the collector prepared by the present invention.

[0034] 3. The use of a collector for reducing the sesquioxide content of collophanite in the present invention couples fine grinding with targeted flotation enrichment, thereby deeply removing impurities from multiple elements; the particle size is effectively controlled by fine grinding, and the influence of fine particles produced by over-grinding during reverse flotation on the collector is reduced; the collophanite sample is sorted by a double reverse flotation process, and efficient directional enrichment of phosphorus is effectively achieved; the collector prepared by the present invention is used for the first time to efficiently enrich the phosphorus element in the collophanite sample, and the magnesium removal collector is used for the second time to further directional remove the magnesium element in the collophanite sample, thereby greatly reducing the content of sesquioxide in the concentrate.

[0035] 4. The use of a collector for reducing the sesquioxide of collophanite according to the present invention can significantly improve the recovery rate of difficult-to-select silico-calcium phosphate ore and the grade of phosphate concentrate; it avoids the use of a large amount of sulfuric acid in the flotation process using the collector, so that the flotation of the coarse concentrate is in a nearly alkaline environment, effectively reducing the corrosion of the acidic slurry on the flotation equipment, thereby greatly extending the service life of the equipment; the process is simple, low-cost, and suitable for industrial application. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 The present invention is an application flow chart of a collector for reducing sesquioxide of collophanite. DETAILED DESCRIPTION

[0037] The present invention is further described below in conjunction with the accompanying drawings and specific preferred embodiments, but the protection scope of the present invention is not limited thereby. The materials and instruments used in the following embodiments are all commercially available.

[0038] The collophanite used in Examples 1 to 8 of the present invention is taken from calci-silico collophanite in Guizhou. The main minerals of the collophanite are fluorapatite, quartz, mica, dolomite, kaolinite, etc., among which the mass percentage of P2O5 is 28.77%, and the mass percentage of R2O3 (Al2O3+Fe2O3) is 5.39%.

[0039] In the application methods of Examples 1 to 8, the grinding medium of the rod mill is steel rods, which are composed of three steel rods with different diameters, the diameters of the three steel rods are Ф75mm, Ф65mm and Ф50mm respectively; the mass ratio of the Ф75mm steel rod, the Ф65mm steel rod and the Ф50mm steel rod is 4:4:2.

[0040] The technical solution of the present invention is further described in detail below, but the protection scope of the present invention is not limited to the following.

[0041] Example 1

[0042] The collector for reducing the sesquioxide of collophanite of the present embodiment is composed of the following components in percentage by weight: 40% of the aqueous solution of the ether amine salt, 40% of the interfacial activity enhancer, 10% of the dodecyl ammonium sulfate, and 10% of the sorbitan monooleate polyoxyethylene ether.

[0043] The mass percentage of the ether amine salt in the aqueous solution of the ether amine salt is 40%, and the mass percentage of the solute in the interfacial activity enhancer is 30%.

[0044] The interfacial activity enhancer is an aqueous solution of alcohol, and the alcohol is polydimethylsiloxane.

[0045] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0046] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 30 min at a rate of 500 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature being 50° C., and the ultrasonic time being 60 min, to obtain a mixture;

[0047] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt and stir with a magnetic stirrer for 30 minutes at a stirring rate of 500 r / min to obtain a collector.

[0048] The present embodiment provides a method for applying a collector for reducing sesquioxide of collophanite, comprising the following steps:

[0049] Step 1: prepare 1 kg of collophanite sample and 1 kg of grinding water, add the 1 kg of collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, comprising the following steps:

[0050] Step 101, mixing the ore sample with 0.7 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining an ore-water mixture;

[0051] Step 102: adding 0.3 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0052] Step 103, the roughing liquid of the ore pulp obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a fine ore pulp slurry, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.38% of the fine ore pulp slurry.

[0053] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 800 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 9;

[0054] Step 3, feeding the flotation rough concentrate with a pH of 9 obtained in step 2 into a flotation machine, and adding 6 kg / t of phosphoric acid of the collophanite sample into the flotation machine to obtain a weakly acidic slurry;

[0055] Step 4: adding 400 g / t of oleic acid of the collophanite sample to the weakly acidic pulp obtained in step 3 for flotation and concentration to obtain collophanite concentrate and tailings II;

[0056] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0057] According to the application method of Example 1, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 1.

[0058] Table 1

[0059] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 74.10 34.81 77.58 1.75 - Tailings Ⅱ 31.96 17.81 20.43 - - Tailings Ⅰ 4.11 13.83 1.99 - 1.10

[0060] As shown in Table 1, in Example 1, after being treated with the ore dressing agent and process of the present invention, the grade of P2O5 in the obtained collophanite concentrate was increased to 34.81%, the recovery rate of P2O5 was 77.58%, and the content of R2O3 was 1.75%. Compared with the original ore, the grade of P2O5 was increased by 6.04%, and the content of R2O3 was reduced by 3.64%. It is proved that the present invention can effectively separate the collophanite concentrate from the siliceous-calcareous collophanite ore, and can realize the efficient recovery of resources, and the foam fluidity of the reverse flotation roughing tailings is good, easy to break, and can effectively make comprehensive utilization of high-quality collophanite resources.

[0061] Example 2

[0062] The collector for reducing the sesquioxide of collophanite of the present embodiment is composed of the following components in percentage by weight: 50% of the aqueous solution of the ether amine salt, 30% of the interfacial activity enhancer, 10% of the dodecyl ammonium sulfate, and 10% of the sorbitan monooleate polyoxyethylene ether.

[0063] The mass percentage of the ether amine salt in the aqueous solution of the ether amine salt is 40%, and the mass percentage of the solute in the interfacial activity enhancer is 20%.

[0064] The interfacial activity enhancer is an aqueous solution of alcohol, and the alcohol is polydiethylsiloxane.

[0065] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0066] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 20 min at a rate of 300 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature being 40° C., and the ultrasonic time being 30 min, to obtain a mixture;

[0067] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt, stir with a magnetic stirrer for 20 minutes at a rate of 300 r / min, and obtain a collector.

[0068] A method for applying a collector to reduce sesquioxide of collophanite, comprising the following steps:

[0069] Step 1: prepare 1 kg of collophanite sample and 1 kg of grinding water, add the 1 kg of collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, comprising the following steps:

[0070] Step 101, mixing the collophanite sample with 0.6 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining a ore-water mixture;

[0071] Step 102: adding 0.4 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0072] Step 103, the slurry obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a slurry of fine ore, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.35% of the slurry of fine ore.

[0073] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 400 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 7;

[0074] Step 3, feeding the flotation rough concentrate with a pH of 7 obtained in step 2 into a flotation machine, and adding 2kg / t of sulfuric acid of collophanite sample into the flotation machine to obtain a weakly acidic ore pulp;

[0075] Step 4: adding 100 g / t of naphthenic acid to the weakly acidic pulp obtained in step 3 to carry out flotation concentration to obtain a collophanite concentrate and tailings II;

[0076] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0077] According to the application method of Example 2, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 2.

[0078] Table 2

[0079] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 63.93 34.68 77.73 1.95 - Tailings Ⅱ 31.96 17.96 20.13 - - Tailings Ⅰ 4.11 14.83 2.14 - 1.25

[0080] As shown in Table 2, in Example 2, after being processed by the ore dressing process of the present invention, the grade of P2O5 in the obtained collophanite concentrate is increased to 34.68%, and the recovery rate of P2O5 is 77.73%. Compared with the original ore, the grade of P2O5 is increased by 5.91%, and the content of R2O3 is reduced by 3.44%. Obviously, the ore dressing process of the present invention can separate the collophanite concentrate from the silico-calcareous collophanite ore, and can realize the effective recovery of resources, and the reverse flotation tailings have good foaming effect and are easy to break, and can effectively make comprehensive utilization of high collophanite resources.

[0081] Example 3

[0082] The collector for reducing the sesquioxide of collophanite of the present embodiment is composed of the following components in percentage by weight: 30% of the aqueous solution of the ether amine salt, 60% of the interfacial activity enhancer, 5% of the dodecyl ammonium sulfate, and 5% of the sorbitan monooleate polyoxyethylene ether.

[0083] The mass percentage of ether amine salt in the aqueous solution of ether amine salt is 30%, and the mass percentage of solute in the interfacial activity enhancer is 30%.

[0084] The interfacial activity enhancer is an aqueous solution of non-polar oil, and the non-polar oil is light diesel oil.

[0085] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0086] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 25 min at a rate of 400 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature being 45° C., and the ultrasonic time being 50 min, to obtain a mixture;

[0087] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt, stir with a magnetic stirrer for 25 minutes at a stirring rate of 400 r / min, to obtain a collector.

[0088] A method for applying a collector to reduce sesquioxide of collophanite, comprising the following steps:

[0089] Step 1: prepare 1 kg of collophanite sample and 1 kg of grinding water, add the 1 kg of collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, comprising the following steps:

[0090] Step 101, mixing the collophanite sample with 0.65 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining a ore-water mixture;

[0091] Step 102: adding 0.35 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0092] Step 103, the roughing liquid of the ore pulp obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a fine ore pulp slurry, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.28% of the fine ore pulp slurry.

[0093] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 500 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 8;

[0094] Step 3, feeding the flotation rough concentrate with a pH of 8 obtained in step 2 into a flotation machine, and adding a mixed acid solution of phosphoric acid and sulfuric acid of 4 kg / t collophanite sample into the flotation machine to obtain a weakly acidic ore pulp;

[0095] Step 4: adding 300 g / t of oleic acid of the collophanite sample to the weakly acidic pulp obtained in step 3 and performing flotation concentration to obtain collophanite concentrate and tailings II;

[0096] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0097] According to the application method of Example 3, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 3.

[0098] Table 3

[0099] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 71.16 34.75 76.71 1.79 - Tailings Ⅱ 34.64 17.96 20.13 - - Tailings Ⅰ 4.20 14.83 3.16 - 1.15

[0100] As shown in Table 3, in Example 3, after being processed by the ore dressing process of the present invention, the grade of P2O5 in the obtained collophanite concentrate was increased to 34.75%, and the recovery rate of P2O5 was 76.71%. Compared with the original ore, the grade of P2O5 was increased by 5.98%, and the content of R2O3 was reduced by 3.60%. Obviously, the ore dressing process of the present invention can separate the collophanite concentrate from the silico-calcareous collophanite ore, and can realize the effective recovery of resources, and the reverse flotation tailings have good foaming effect and are easy to break, and can effectively make comprehensive utilization of high collophanite resources.

[0101] Example 4

[0102] A collector for reducing the sesquioxide of collophanite in this embodiment is composed of the following components in percentage by mass: 40% of the aqueous solution of the ether amine salt, 50% of the interfacial activity enhancer, 5% of the dodecyl ammonium sulfate, and 5% of the sorbitan monooleate polyoxyethylene ether;

[0103] The mass percentage of ether amine salt in the aqueous solution of ether amine salt is 30%, and the mass percentage of solute in the interfacial activity enhancer is 30%.

[0104] The interfacial activity enhancer is an aqueous solution of ether, and the ether is polyoxypropylene glycerol ether.

[0105] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0106] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 30 min at a rate of 500 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature being 50° C., and the ultrasonic time being 60 min, to obtain a mixture;

[0107] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt, stir with a magnetic stirrer for 30 minutes at a stirring rate of 500 r / min, to obtain a collector.

[0108] A method for applying a collector to reduce sesquioxide of collophanite, comprising the following steps:

[0109] Step 1: prepare 1 kg of collophanite sample and 1 kg of grinding water, add the 1 kg of collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, comprising the following steps:

[0110] Step 101, mixing the collophanite sample with 0.6 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining a ore-water mixture;

[0111] Step 102: adding 0.4 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0112] Step 103, the slurry obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a slurry of fine ore, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.35% of the slurry of fine ore.

[0113] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 700 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 9;

[0114] Step 3: Feed the flotation concentrate with a pH of 9 obtained in step 2 into a flotation machine, and add 5 kg / t of sulfuric acid per ton of collophanite sample into the flotation machine to obtain a weakly acidic pulp.

[0115] Step 4: adding 300 g / t of cyclohexane acid to the weakly acidic pulp obtained in step 3 and performing flotation separation to obtain a collophanite concentrate and tailings II;

[0116] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0117] According to the application method of Example 4, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 4.

[0118] Table 4

[0119] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 74.21 34.24 76.53 1.93 - Tailings Ⅱ 22.64 17.96 20.13 - - Tailings Ⅰ 3.15 14.83 3.34 - 1.20

[0120] As shown in Table 4, in Example 4, after being processed by the ore dressing process of the present invention, the grade of P2O5 in the obtained collophanite concentrate was increased to 35.14%, and the recovery rate of P2O5 was 76.53%. Compared with the original ore, the grade of P2O5 was increased by 5.47%, and the content of R2O3 was reduced by 3.46%. Obviously, the ore dressing process of the present invention can separate the collophanite concentrate from the silico-calcareous collophanite ore, and can realize the effective recovery of resources, and the reverse flotation tailings have good foaming effect and are easy to break, and can effectively make comprehensive utilization of high collophanite resources.

[0121] Example 5

[0122] The collector for reducing the sesquioxide of collophanite of the present embodiment is composed of the following components in percentage by weight: 40% of the aqueous solution of the ether amine salt, 45% of the interfacial activity enhancer, 10% of the dodecyl ammonium sulfate, and 5% of the sorbitan monooleate polyoxyethylene ether.

[0123] The mass percentage of ether amine salt in the aqueous solution of ether amine salt is 25%, and the mass percentage of solute in the interfacial activity enhancer is 35%.

[0124] The interfacial activity enhancer is an aqueous solution of non-polar oil, and the non-polar oil is a mixed solution of aviation kerosene and light diesel oil.

[0125] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0126] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 25 min at a rate of 300 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature being 45° C., and the ultrasonic time being 50 min, to obtain a mixture;

[0127] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt, stir with a magnetic stirrer for 25 minutes at a rate of 300 r / min, and obtain a collector.

[0128] A method for applying a collector to reduce sesquioxide of collophanite, comprising the following steps:

[0129] Step 1: prepare 1 kg of collophanite sample and 1 kg of grinding water, add the 1 kg of collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, comprising the following steps:

[0130] Step 101, mixing the collophanite sample with 0.7 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining a ore-water mixture;

[0131] Step 102: adding 0.3 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0132] Step 103, the slurry obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a slurry of fine ore, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.29% of the slurry of fine ore.

[0133] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 500 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 7;

[0134] Step 3, feeding the flotation rough concentrate with a pH of 7 obtained in step 2 into a flotation machine, and adding 3kg / t of phosphoric acid of the collophanite sample into the flotation machine to obtain a weakly acidic slurry;

[0135] Step 4: adding 200 g / t of oleic acid of the collophanite sample to the weakly acidic pulp obtained in step 3 and performing flotation separation to obtain collophanite concentrate and tailings II;

[0136] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0137] According to the application method of Example 5, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 5.

[0138] Table 5

[0139] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 74.24 34.57 76.89 1.77 - Tailings Ⅱ 22.13 17.69 20.22 - - Tailings Ⅰ 3.63 14.24 2.89 - 1.20

[0140] As shown in Table 5, in Example 5, after being processed by the ore dressing process of the present invention, the grade of P2O5 in the obtained collophanite concentrate is increased to 34.97%, and the recovery rate of P2O5 is 76.89%. Compared with the original ore, the grade of P2O5 is increased by 5.70%, and the content of R2O3 is reduced by 3.62%. Obviously, the ore dressing process of the present invention can separate the collophanite concentrate from the silico-calcareous collophanite ore, and can realize the effective recovery of resources, and the reverse flotation tailings have good foaming effect and are easy to break, and can effectively make comprehensive utilization of high collophanite resources.

[0141] Example 6

[0142] The collector for reducing the sesquioxide of collophanite of the present embodiment is composed of the following components in percentage by weight: 30% of the aqueous solution of the ether amine salt, 55% of the interfacial activity enhancer, 10% of the dodecyl ammonium sulfate, and 5% of the sorbitan monooleate polyoxyethylene ether.

[0143] The mass percentage of the ether amine salt in the aqueous solution of the ether amine salt is 30%, and the mass percentage of the solute in the interfacial activity enhancer is 40%.

[0144] The interfacial activity enhancer is an aqueous solution of alcohol, and the alcohol is PPG type polypropylene glycol;

[0145] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0146] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 20 min at a rate of 400 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature being 50° C., and the ultrasonic time being 30 min, to obtain a mixture;

[0147] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt, stir with a magnetic stirrer for 20 minutes at a stirring rate of 400 r / min, and obtain a collector.

[0148] A method for applying a collector to reduce sesquioxide of collophanite, comprising the following steps:

[0149] Step 1: Prepare 1 kg of collophanite sample, 1 kg of grinding water, and prepare for three-stage grinding, including the following steps:

[0150] Step 101, mixing the collophanite sample with 0.7 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining a ore-water mixture;

[0151] Step 102: adding 0.3 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0152] Step 103, the slurry obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a slurry of fine ore, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.34% of the slurry of fine ore.

[0153] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 600 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 8;

[0154] Step 3, feeding the flotation rough concentrate with a pH of 8 obtained in step 2 into a flotation machine, and adding 4 kg / t of sulfuric acid of collophanite sample into the flotation machine to obtain a weakly acidic slurry;

[0155] Step 4: adding 300 g / t of naphthenic acid to the weakly acidic pulp obtained in step 3 to carry out flotation concentration to obtain a collophanite concentrate and tailings II;

[0156] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0157] According to the application method of Example 6, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 6.

[0158] Table 6

[0159] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[Recovery rate of P2O5 / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 75.11 33.91 75.98 1.88 - Tailings Ⅱ 20.29 18.34 21.23 - - Tailings Ⅰ 4.60 14.28 2.79 - 1.10

[0160] As shown in Table 6, in Example 6, after being processed by the ore dressing process of the present invention, the grade of P2O5 in the obtained collophanite concentrate was increased to 34.91%, and the recovery rate of P2O5 was 75.98%. Compared with the original ore, the grade of P2O5 was increased by 5.14%, and the content of R2O3 was reduced by 3.51%. Obviously, the ore dressing process of the present invention can separate the collophanite concentrate from the silico-calcareous collophanite ore, and can realize the effective recovery of resources, and the reverse flotation tailings have good foaming effect and are easy to break, and can effectively make comprehensive utilization of high collophanite resources.

[0161] Example 7

[0162] The collector for reducing the sesquioxide of collophanite of the present embodiment is composed of the following components in percentage by weight: 40% of the aqueous solution of the ether amine salt, 40% of the interfacial activity enhancer, 10% of the dodecyl ammonium sulfate, and 10% of the sorbitan monooleate polyoxyethylene ether.

[0163] The mass percentage of ether amine salt in the aqueous solution of ether amine salt is 30%, and the mass percentage of solute in the interfacial activity enhancer is 30%.

[0164] The interfacial activity enhancer is an aqueous solution of non-polar oil; and the non-polar oil is aviation kerosene.

[0165] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0166] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 30 min at a rate of 500 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature being 40° C., and the ultrasonic time being 30 min, to obtain a mixture;

[0167] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt, stir with a magnetic stirrer for 30 minutes at a stirring rate of 500 r / min, to obtain a collector.

[0168] A method for applying a collector to reduce sesquioxide of collophanite, comprising the following steps:

[0169] Step 1: prepare 1 kg of collophanite sample and 1 kg of grinding water, add the 1 kg of collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, comprising the following steps:

[0170] Step 101, mixing the collophanite sample with 0.6 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining a ore-water mixture;

[0171] Step 102: adding 0.4 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0172] Step 103, the slurry obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a slurry of fine ore, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.35% of the slurry of fine ore.

[0173] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 500 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 7;

[0174] Step 3, feeding the flotation rough concentrate with a pH of 7 obtained in step 2 into a flotation machine, and adding 5 kg / t of phosphoric acid of the collophanite sample into the flotation machine to obtain a weakly acidic slurry;

[0175] Step 4: adding 400 g / t of naphthenic acid to the weakly acidic pulp obtained in step 3 to carry out flotation concentration to obtain a collophanite concentrate and tailings II;

[0176] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0177] According to the application method of Example 7, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 7.

[0178] Table 7

[0179] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 73.29 35.01 76.24 1.89 - Tailings Ⅱ 23.44 16.34 21.12 - - Tailings Ⅰ 3.27 13.15 2.64 - 1.20

[0180] As shown in Table 7, in Example 7, after being processed by the ore dressing process of the present invention, the grade of P2O5 in the obtained collophanite concentrate was increased to 35.01%, and the recovery rate of P2O5 was 75.94%. Compared with the original ore, the grade of P2O5 was increased by 6.24%, and the content of R2O3 was reduced by 3.50%. Obviously, the ore dressing process of the present invention can separate the collophanite concentrate from the silico-calcareous collophanite ore, and can achieve effective resource recovery. The reverse flotation tailings have good foaming effect and are easy to break, and can effectively utilize the high-quality collophanite resources.

[0181] Example 8

[0182] The collector for reducing the sesquioxide of collophanite of the present embodiment is composed of the following components in percentage by weight: 38% of the aqueous solution of the ether amine salt, 50% of the interfacial activity enhancer, 6% of the dodecyl ammonium sulfate, and 6% of the sorbitan monooleate polyoxyethylene ether.

[0183] The mass percentage of ether amine salt in the aqueous solution of ether amine salt is 35%, and the mass percentage of solute in the interfacial activity enhancer is 35%.

[0184] The interfacial activity enhancer is an alcohol aqueous solution, and the alcohol is a mixed alcohol solution of polydimethylsiloxane and diethylsiloxane.

[0185] A method for preparing a collector for reducing sesquioxide of collophanite comprises the following steps:

[0186] Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring with a magnetic stirrer for 30 min at a rate of 400 r / min, placing in an ultrasonic disperser for ultrasonic dispersion, the ultrasonic temperature is 40° C., and the ultrasonic time is 30 min to obtain a mixture;

[0187] Step 2: Place the mixture obtained in step 1 into an aqueous solution of ether amine salt, stir with a magnetic stirrer for 30 minutes at a rate of 400 r / min, and obtain a collector.

[0188] A method for applying a collector to reduce sesquioxide of collophanite, comprising the following steps:

[0189] Step 1: prepare 1 kg of collophanite sample and 1 kg of grinding water, add the 1 kg of collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, comprising the following steps:

[0190] Step 101, mixing the collophanite sample with 0.6 kg of the first batch of water, placing the mixture in the rod mill for 2 min of first grinding, and obtaining a ore-water mixture;

[0191] Step 102: adding 0.4 kg of a second batch of water to the ore-water mixture obtained in step 101, and performing a second grinding for 2 min to obtain a slurry roughing solution;

[0192] Step 103, the roughing liquid of the ore pulp obtained in step 102 is screened by a drum screen to obtain coarse ore particles and a fine ore pulp slurry, and the coarse ore particles are sequentially returned to perform the third stage of grinding; the material with a grinding fineness of less than 0.074 mm accounts for 71.28% of the fine ore pulp slurry.

[0193] Step 2: feeding the slurry obtained in step 103 into a flotation machine, and adding 500 g / t of the collector of the collophanite sample into the flotation machine for flotation roughing to obtain a flotation rough concentrate and roughing tailings with a pH of 8;

[0194] Step 3, feeding the flotation rough concentrate with a pH of 8 obtained in step 2 into a flotation machine, and adding 5 kg / t of phosphoric acid of the collophanite sample into the flotation machine to obtain a weakly acidic ore pulp;

[0195] Step 4: adding 400 g / t of oleic acid of the collophanite sample to the weakly acidic pulp obtained in step 3 for flotation and concentration to obtain collophanite concentrate and tailings II;

[0196] Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

[0197] According to the application method of Example 8, a flotation test was conducted on the obtained collector for reducing the sesquioxide of collophanite. The experimental data are shown in Table 8.

[0198] Table 8

[0199] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[Content of R2O3 / %]]> Flotation foam volume / L Concentrate 75.12 34.29 74.38 1.93 - Tailings Ⅱ 20.64 16.48 22.02 - - Tailings Ⅰ 4.24 12.21 3.60 - 1.15

[0200] As shown in Table 8, in Example 8, after being processed by the ore dressing process of the present invention, the grade of P2O5 in the obtained collophanite concentrate was increased to 34.29%, and the recovery rate of P2O5 was 74.38%. Compared with the original ore, the grade of P2O5 was increased by 5.52%, and the content of R2O3 was reduced by 3.46%. Obviously, the ore dressing process of the present invention can separate the collophanite concentrate from the silico-calcareous collophanite ore, and can realize the effective recovery of resources, and the reverse flotation tailings have good foaming effect and are easy to break, and can effectively make comprehensive utilization of high collophanite resources.

[0201] Comparative Example 1

[0202] The collophanite sample and application method of Example 6 were used to recover the collophanite sample, except that no aqueous solution of PPG type polypropylene glycol was added. Specific mineral processing test indicators are shown in Table 9.

[0203] Table 9

[0204]

[0205]

[0206] It can be seen from the results in Table 9 that without adding the aqueous solution of PPG type polypropylene glycol, the grade and recovery rate of P2O5 obtained are not much different from the test indicators of Example 6, but the fluidity of the rough flotation foam is extremely poor, and the amount of residual foam is far greater than the test indicators of Example 6, and scavenging cannot be performed.

[0207] Comparative Example 2

[0208] The collophanite sample and application method of Example 4 are used to recover the collophanite sample, except that diethyl phthalate solution is used instead of the aqueous solution of polyoxypropylene glycerol ether. Specific mineral processing test indicators are shown in Table 10.

[0209] Table 10

[0210] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 58.19 33.90 68.91 1.9 - Tailings Ⅱ 7.88 12.95 3.74 - - Tailings Ⅰ 5.30 3.31 19.17 - 3.13

[0211] It can be seen from the results in Table 10 that when the aqueous solution of polyoxypropylene glycerol ether is replaced by diethyl phthalate solution, the P2O5 recovery rate obtained is significantly lower than the test index of Example 4, and the amount of residual froth in flotation is significantly greater than the test index of Example 4.

[0212] Comparative Example 3

[0213] The collophanite sample and application method in Example 7 are used to recycle the collophanite sample, except that no aqueous solution of aviation kerosene is added. Specific mineral processing test indicators are shown in Table 11.

[0214] Table 11

[0215] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 62.71 33.82 71.65 1.9 - Tailings Ⅱ 2.01 13.25 3.49 - - Tailings Ⅰ 35.98 21.42 24.86 - 3.57

[0216] It can be seen from the results in Table 11 that without adding aviation kerosene to the aqueous solution, the grade and recovery rate of P2O5 obtained are not much different from the test indicators of Example 7, but the fluidity of the rough flotation foam is extremely poor, and the amount of residual foam is far greater than the test indicators of Example 7, and scavenging cannot be performed.

[0217] Comparative Example 4

[0218] The collophanite sample and application method of Example 3 are used to recover the collophanite sample, except that cocamidopropylamine oxide is used instead of the aqueous solution of the etheramine salt. Specific mineral processing test indicators are shown in Table 12.

[0219] Table 12

[0220] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 70.13 31.97 76.96 2.17 - Tailings Ⅱ 1.91 13.20 0.87 - - Tailings Ⅰ 8.25 18.78 5.32 - 2.34

[0221] It can be seen from the results in Table 12 that when cocamidopropylamine oxide is used instead of the aqueous solution of the ether amine salt, the grade of P2O5 obtained is significantly lower than the test index of Example 3.

[0222] Comparative Example 5

[0223] The collophanite sample and application method of Example 3 are used to recover the collophanite sample, except that dodecylamine polyoxyethylene ether is used instead of the aqueous solution of the etheramine salt. Specific mineral processing test indicators are shown in Table 13.

[0224] Table 13

[0225] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 73.68 31.26 79.06 2.23 - Tailings Ⅱ 2.37 12.68 1.03 - - Tailings Ⅰ 7.63 20.76 5.44 - 3.44

[0226] It can be seen from the results in Table 13 that when dodecylamine polyoxyethylene ether is used to replace the aqueous solution of the ether amine salt, the grade of P2O5 obtained is significantly lower than the test index of Example 3.

[0227] Comparative Example 6

[0228] The collophanite sample and application method of Example 1 are used to recover the collophanite sample, except that an etheramine is used instead of the aqueous solution of the etheramine salt. Specific mineral processing test indicators are shown in Table 14.

[0229] Table 14

[0230] product Yield / % <![CDATA[P2O5 grade / %]]> <![CDATA[P2O5 recovery rate / %]]> <![CDATA[R2O3 content / %]]> Flotation foam volume / L Concentrate 69.77 32.21 77.14 2.01 - Tailings Ⅱ 2.19 15.05 1.13 - - Tailings Ⅰ 8.94 17.92 5.50 - 3.35

[0231] It can be seen from the results in Table 14 that when an etheramine is used instead of the aqueous solution of the etheramine salt, the grade of P2O5 obtained is significantly lower than the test index of Example 1.

[0232] In summary, in the collector prepared by the preparation process of the present invention, the grade of P2O5 is improved by selecting the raw materials, the amount of foam in the tailings is low, and the foam fluidity is good. Comparative Examples 4 to 6 illustrate that the ether amine salt modified by dodecylamine can introduce a hydrophilic group ether oxygen group into the collector prepared by the present invention, thereby increasing the solubility of the agent, enhancing the adsorption of the agent at the gas-liquid interface, further improving the foaming performance, and enhancing the capture ability and selectivity of the ether amine for silicate minerals.

[0233] The raw materials of the present invention are also limited to the aqueous solution of alcohol, wherein the alcohol is one or more of polydimethylsiloxane, polydiethylsiloxane, and PPG-type polypropylene glycol; the aqueous solution of ether is particularly selected from the aqueous solution of polyoxypropylene glycerol ether; and the aqueous solution of non-polar oil is one or more of aviation kerosene and light diesel oil. Comparative Examples 1 to 3 illustrate that the selected surfactant enhancer can reduce the amount of tailings foam in the flotation process of the collector prepared by the present invention, facilitate crushing, improve the flotation efficiency, and optimize the flotation process.

[0234] The above is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as above in the preferred embodiment, it is not used to limit the present invention. Any technician familiar with the art can make many possible changes and modifications to the technical solution of the present invention by using the methods and technical contents disclosed above without departing from the spirit and technical solution of the present invention, or modify it into an equivalent embodiment of equivalent changes. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention, still fall within the scope of protection of the technical solution of the present invention.

Claims

1. A collector for reducing sesquioxide of collophanite, characterized in that: The invention is composed of the following components in percentage by mass: 30% to 50% aqueous solution of ether amine salt, 30% to 60% interfacial activity enhancer, 5% to 10% ammonium dodecyl sulfate, and 5% to 10% sorbitan monooleate polyoxyethylene ether. The interfacial activity enhancer is one of an aqueous solution of alcohol, an aqueous solution of ether and an aqueous solution of non-polar oil.

2. A collector for reducing collophane sesquioxide according to claim 1, characterized in that: The invention is composed of the following components in percentage by weight: 40% of the aqueous solution of the ether amine salt, 40% of the interfacial activity enhancer, 10% of the dodecyl ammonium sulfate and 10% of the sorbitan monooleate polyoxyethylene ether.

3. A collector for reducing sesquioxide of collophanite according to claim 1, characterized in that: The mass percentage of ether amine salt in the aqueous solution of ether amine salt is 20% to 40%, the mass percentage of solute in the interfacial activity enhancer is 20% to 40%, the alcohol is one or a combination of polydimethylsiloxane, polydiethylsiloxane and PPG type polypropylene glycol, the ether is polyoxypropylene glycerol ether, and the non-polar oil is aviation kerosene and / or light diesel oil.

4. A collector for reducing sesquioxide of collophanite according to claim 3, characterized in that: The mass percentage of the ether amine salt in the aqueous solution of the ether amine salt is 40%, and the mass percentage of the solute in the interfacial activity enhancer is 30%.

5. A method for preparing a collector for reducing sesquioxide of collophanite as claimed in claim 1, characterized in that: The following steps are involved: Step 1, mixing the surfactant, ammonium lauryl sulfate and sorbitan monooleate polyoxyethylene ether, stirring the mixture, and then placing the mixture in an ultrasonic device for ultrasonic dispersion to obtain a mixture; Step 2: placing the mixture obtained in step 1 into an aqueous solution of ether amine salt and stirring to obtain a collector.

6. The method for preparing a collector for reducing sesquioxide of collophanite according to claim 5, characterized in that: The stirring in step 1 and step 2 is carried out by a magnetic stirrer, the stirring rate of the magnetic stirrer is 300r / min~500r / min, and the stirring time is 20min~30min; the ultrasonic device in step 1 is an ultrasonic disperser, the ultrasonic temperature is 40℃~50℃, and the ultrasonic time is 30min~60min.

7. A use of a collector for reducing sesquioxide of collophanite as claimed in claim 1, characterized in that: The following steps are involved: Step 1: prepare grinding water and collophanite sample in equal mass proportions, add the collophanite sample into a rod mill at one time, and then add the grinding water into the rod mill in batches for three-stage grinding, specifically comprising the following steps: Step 101, mixing the collophanite sample with the first batch of water, placing the mixture in the rod mill for first-stage grinding to obtain a ore-water mixture; Step 102, adding a second batch of water to the ore-water mixture obtained in step 101 to perform a second stage of grinding to obtain a slurry roughing solution; Step 103, the roughing liquid obtained in step 102 is screened through a drum screen to obtain coarse ore particles and fine ore slurry, and the coarse ore particles are sequentially returned to perform the third stage of grinding; Step 2, feeding the slurry obtained in step 103 into a flotation machine, and adding the collector into the flotation machine to perform flotation roughing to obtain a flotation rough concentrate and a roughing tailing; Step 3, feeding the flotation rough concentrate obtained in step 2 into a flotation machine, and adding an acidic adjuster into the flotation machine to adjust the pH to obtain a weakly acidic ore pulp; Step 4: adding a de-magnesium collector to the weakly acidic slurry obtained in step 3 and then flotation separation to obtain concentrate and tailings II; Step 5: Feed the rougher tailings obtained in step 2 into a flotation machine, perform three flotation sweeps on the rougher tailings, and return the middlings in sequence to obtain tailings I.

8. The method for using a collector for reducing sesquioxide of collophanite according to claim 7, characterized in that: In step 1, the grinding medium of the rod mill is a steel rod, and the steel rod is composed of at least three steel rods with different diameters, and the diameters of the three steel rods are Φ75mm, Φ65mm and Φ50mm respectively; the mass ratio of the Φ75mm steel rod, the Φ65mm steel rod and the Φ50mm steel rod is 4:4:2; In step 101, the mass of the first batch of water accounts for 60% to 70% of the mass of the grinding water, and the grinding time of the first stage of grinding is 2 minutes; in step 102, the grinding time of the second stage of grinding is 2 minutes.

9. The method for using a collector for reducing sesquioxide of collophanite according to claim 7, characterized in that: The amount of the collector in step 2 is 400g-800g / t of collophanite sample, and the pH of the flotation rough concentrate in step 2 is 7-9; The acidic regulator in step 3 is phosphoric acid and / or sulfuric acid, and the amount of the acidic regulator is 2kg to 6kg / t of collophanite sample; The demagnesiumizing collector in step 4 is oleic acid or cyclohexane acid, and the dosage of the demagnesiumizing collector is 100g to 400g / t of collophanite sample.

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