CN110813540B - Collecting agent composition for flotation and recovery of monazite from zircon heavy sand - Google Patents
Collecting agent composition for flotation and recovery of monazite from zircon heavy sand Download PDFInfo
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- CN110813540B CN110813540B CN201911016666.5A CN201911016666A CN110813540B CN 110813540 B CN110813540 B CN 110813540B CN 201911016666 A CN201911016666 A CN 201911016666A CN 110813540 B CN110813540 B CN 110813540B
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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
- B03D1/01—Organic compounds containing nitrogen
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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
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Abstract
本发明提供一种用于从锆英石重砂中浮选回收独居石的捕收剂组合物，按重量组分计，包括：药剂A 35～50份、药剂B 10～30份、对乙基扁桃酸钠20～40份、甲基异丁基甲醇1～2份。本发明提供的捕收剂组合物选择性高，捕收能力好，能够有效回收锆英石重矿砂中的独居石，与传统浮选药剂相比，本发明提供的捕收剂组合物可提高独居石精矿中稀土氧化物的品位和回收率分别达1和3个百分点以上，并提高锆英石重砂品位2个百分点以上，降低浮选温度10～15℃。
The present invention provides a collector composition for recovering monazite by flotation from heavy zircon sand, which, in terms of components by weight, comprises: 35-50 parts of medicament A, 10-30 parts of medicament B, 20-40 parts of sodium mandelate and 1-2 parts of methyl isobutyl methanol. The collector composition provided by the invention has high selectivity and good collecting ability, and can effectively recover the monazite in the zircon heavy ore sand. Compared with the traditional flotation agent, the collector composition provided by the invention can improve the The grade and recovery rate of rare earth oxides in monazite concentrate are over 1 and 3 percentage points respectively, and the grade of zircon heavy sand is increased by over 2 percentage points, and the flotation temperature is lowered by 10-15 °C.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a collecting agent composition for recovering monazite from zircon heavy sand through flotation.
Background
The high-grade zircon concentrate is generally derived from seashore placer, and at present, the seashore placer is usually treated by adopting combined processes of electric separation, gravity separation, magnetic separation and the like to obtain the higher-grade zircon placer. However, in recent years, due to the increasingly higher complexity of the properties of the seashore placer and the lower separation precision of the physical beneficiation process, the content of other fine-grained accompanying minerals in the zircon heavy sand obtained by the traditional combined flow of electric separation, gravity separation and magnetic separation is gradually increased, and particularly, a large amount of fine-grained monazite minerals associated with zircon appear in the zircon heavy sand. The inclusion of monazite in the zircon heavy sand not only reduces the grade of the zircon, but also causes a great deal of waste of rare earth minerals, and seriously influences the recovery rate of the rare earth elements in the seashore placer. At present, the flotation process is a key process for recovering associated fine-grained monazite in zircon heavy sand and improving the grade of the zircon, the collecting agent is selected to influence the effect of the flotation process, the conventional flotation collecting agent of the monazite is a fatty acid medicament with a long hydrocarbon chain, the medicament and metal ions on the surface of the monazite mainly have physical effects, the medicament selectivity is low, the separation effect is poor, and the ore pulp needs to be heated during flotation, so that the separation cost is greatly increased. Therefore, the construction of an efficient chelating collector system suitable for low-temperature flotation is the core for solving the problem of separation of monazite and zirconite.
Disclosure of Invention
In view of the above, the invention provides the collecting agent composition for flotation and recovery of monazite from zircon heavy sand, which has strong collecting capability and high selectivity, can effectively recover rare earth minerals and reduce the flotation temperature.
The invention provides a collector composition for flotation and recovery of monazite from zircon heavy sand, which comprises the following components in parts by weight: 35-50 parts of a medicament A, 10-30 parts of a medicament B, 20-40 parts of sodium p-ethylmandelate and 1-2 parts of methyl isobutyl carbinol; wherein the medicament A is alpha-substituted fatty acid salt, and the structural formula is as follows:
in the formula, R1Is C10～C15Alkyl of R2Is any one of OH, Cl and Br, R3Is H, Na, K, NH4Any one of the groups;
the structural formula of the medicament B is as follows:
in the formula (II), R'1Is C10～C12Alkyl of R'2Is C1～C2Alkyl or H, R'3Is C1～C3Alkyl of R'4Is H, Na, K, NH4Any one of the groups.
Further, the medicament A is alpha-hydroxy sodium palmitate, and the medicament B is N-lauroyl sarcosine sodium.
Further comprises the following components in percentage by weight: 40 parts of alpha-hydroxy sodium palmitate, 20 parts of N-lauroyl sodium sarcosinate, 39 parts of sodium p-ethylmandelate and 1 part of methyl isobutyl carbinol.
Further comprises the following components in percentage by weight: 45 parts of alpha-hydroxy sodium palmitate, 25 parts of N-lauroyl sodium sarcosinate, 29 parts of sodium p-ethylmandelate and 1.2 parts of methyl isobutyl carbinol.
Further comprises the following components in percentage by weight: 38 parts of alpha-hydroxy sodium palmitate, 15 parts of N-lauroyl sodium sarcosinate, 34 parts of sodium p-ethylmandelate and 1.5 parts of methyl isobutyl carbinol.
Further comprises the following components in percentage by weight: 42 parts of a medicament A, 28 parts of a medicament B, 25 parts of sodium p-ethyl mandelate and 1.8 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
further comprises the following components in percentage by weight: 36 parts of a medicament A, 12 parts of a medicament B, 35 parts of sodium p-ethylmandelate and 2 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
further comprises the following components in percentage by weight: 46 parts of a medicament A, 14 parts of a medicament B, 28 parts of sodium p-ethylmandelate and 2 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
the active metal ions in monazite are respectively La3+、Ce3+La is known from the Lewis acid-base theory3+And Ce3+All belong to strong acid and are easily coordinated with strong basic anions such as O atoms and N atoms, and the agent A, the agent B and the sodium p-ethylmandelate in the collecting agent composition provided by the invention can be coordinated with La in the form of O-O or O-N3+、Ce3+Coordination; and the selectivity of the medicament and mineral action can be improved by the electron-withdrawing effect of the medicament A on the alpha-substituent in the sodium ethylmandelate molecule. Meanwhile, the substituent effect of the alpha position can also improve the dissociation characteristic of the medicament in the ore pulp, thereby reducing the temperature required by flotation. In addition, the addition of methyl isobutyl carbinol can increase the stability of the bubbles in the flotation system.
The collecting agent composition provided by the invention has synergistic effect among the medicament molecules and among groups in the molecules, so that the floatation effect of monazite is effectively improved; according to the collector composition provided by the invention, a new group is introduced at the alpha position of carboxylic acid, and the new group can influence the distribution of electron clouds in molecules, so that a polar group, namely a carboxyl group in a medicament is more selective; the collecting agent composition provided by the invention can achieve the best matching of the collecting capability, selectivity and flotation bubble stability of the agent, the separation of monazite, zirconite and other gangue minerals can be realized by the combined agent in the alkaline range of pH of 10.5-12.0, and the grade and recovery rate of rare earth in a concentrate product can be effectively improved. Compared with the traditional flotation reagent, the collecting agent composition provided by the invention can improve the grade and recovery rate of rare earth oxide in monazite concentrate by more than 1 and 3 percentage points respectively, improve the grade of zircon heavy sand by more than 2 percentage points and reduce the flotation temperature by 10-15 ℃.
Drawings
Figure 1 is a schematic diagram of a closed circuit test procedure for floating monazite from zircon heavy sand using the collector composition provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
The invention provides a collector composition for flotation and recovery of monazite from zircon heavy sand, which is obtained by mixing the following raw materials in parts by weight: 35-50 parts of a medicament A, 10-30 parts of a medicament B, 20-40 parts of sodium p-ethylmandelate and 1-2 parts of methyl isobutyl carbinol; wherein, the medicament A is alpha-substituted fatty acid salt, and the structural formula is as follows:
in the formula, R1Is C10H21、C11H23、C12H25、C13H27、C14H29、C15H31Any one of the alkyl groups of (1), R2Is any one of OH, Cl and Br, R3Is H, Na, K, NH4Any one of the groups; preferably, R1Is C14H29，R2Is OH, R3Na and the medicament A is alpha-hydroxy sodium palmitate;
the structural formula of the medicament B is as follows:
in the formula (II), R'1Is C10H21、C11H23、C12H25Any one alkyl group of (1), R'2Is C1～C2Alkyl or H, R'3Is CH2、C2H4、C3H6Any one alkyl group of (1), R'4Is H, Na, K, NH4Any one of the groups; preferably, R'1Is C11H23，R′2Is CH3，R′3Is CH2，R′4Is Na, and the medicament B is N-lauroyl sarcosine sodium.
In order to make the objects, technical solutions and advantages of the present invention more apparent, a collector composition for flotating and recovering monazite from zircon heavy sand according to the present invention will be further described with reference to the following examples.
Example 1:
the collector composition of example 1 was mixed from the following raw materials in weight parts: 40 parts of alpha-hydroxy sodium palmitate, 20 parts of N-lauroyl sodium sarcosinate, 39 parts of sodium p-ethylmandelate and 1 part of methyl isobutyl carbinol.
Example 2:
the collector composition of example 2 was mixed from the following raw materials in weight parts: 45 parts of alpha-hydroxy sodium palmitate, 25 parts of N-lauroyl sodium sarcosinate, 29 parts of sodium p-ethylmandelate and 1.2 parts of methyl isobutyl carbinol.
Example 3:
the collector composition of example 3 was mixed from the following raw materials in weight parts: 38 parts of alpha-hydroxy sodium palmitate, 15 parts of N-lauroyl sodium sarcosinate, 34 parts of sodium p-ethylmandelate and 1.5 parts of methyl isobutyl carbinol.
Example 4:
the collector composition of example 4 was mixed from the following raw materials in weight parts: 48 parts of alpha-hydroxy sodium palmitate, 30 parts of N-lauroyl sodium sarcosinate, 22 parts of sodium p-ethylmandelate and 2 parts of methyl isobutyl carbinol.
Example 5:
the collector composition of example 5 was mixed from the following raw materials in weight parts: 42 parts of a medicament A, 28 parts of a medicament B, 25 parts of sodium p-ethyl mandelate and 1.8 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
example 6:
the collector composition of example 6 was mixed from the following raw materials in weight parts: 36 parts of a medicament A, 12 parts of a medicament B, 35 parts of sodium p-ethylmandelate and 2 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
the ore samples treated in examples 1 to 6 are zircon heavy sand produced from placer at certain seashore in Hainan island, a laboratory closed flotation test is adopted, the test flow and the chemical system are shown in figure 1, and the specific process of the test flow is as follows: re-sanding zircon until the particle size is 87% of-0.045 mm, making into pulp with proper concentration and adding Na2CO3Carrying out rough concentration on 3000g/t, 1000g/t of sodium hexametaphosphate, 2000g/t of water glass and 800g/t of collecting agent composition to obtain rough concentrate and first tailings; making the rough concentrate into ore pulp with proper concentration and adding Na2CO32500g/t, 800g/t of sodium hexametaphosphate, 1500g/t of water glass and 600g/t of collecting agent composition are subjected to first concentration to obtain first concentrate and first concentrate tail; preparing the first tailings into ore pulp with proper concentration and adding Na2CO3Scavenging at 2000g/t, sodium hexametaphosphate at 1000g/t and water glass at 2000g/t to obtain scavenged concentrate and second tailings;merging the first fine tailings and the scavenging concentrate, grinding the ore until the ore accounts for 80% of the ore with the granularity of-0.037 mm, and returning ore pulp obtained after grinding the ore to the roughing operation; making the first concentrate into ore pulp with proper concentration and adding Na2CO31500g/t, 800g/t of sodium hexametaphosphate, 1000g/t of water glass and 400g/t of the collecting agent composition are subjected to secondary concentration to obtain a second concentrate and a second fine tail, and the second fine tail is returned to the primary concentration operation; making the second concentrate into pulp with proper concentration and adding Na2CO31000g/t, 600g/t of sodium hexametaphosphate, 800g/t of water glass and 300g/t of the collecting agent composition are subjected to third concentration to obtain monazite concentrate and a third fine tail, the third fine tail is returned to the second concentration operation, the dosage of the agent is based on the amount of the zircon heavy sand ore fed into the process, and the temperature in the flotation process is controlled to be 30 +/-2 ℃.
Table 1 shows the grade and recovery of REO (rare earth oxides) from monazite concentrates obtained after closed-circuit flotation tests using the collector compositions of examples 1 to 6, and the data in table 1 show that the REO grade in monazite concentrates is 60.31% -62.45%, the recovery of REO is 87.53% -92.44%, and ZrO in tailings is obtained after flotation of zircon heavy sand from hainan by using the collector compositions of the present invention2The grade is 63.32-63.81%.
TABLE 1 grade and recovery of rare earth oxides in rare earth concentrates
Example 7:
the collector composition of example 7 was mixed from the following raw materials in weight parts: 46 parts of a medicament A, 14 parts of a medicament B, 28 parts of sodium p-ethylmandelate and 2 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
example 8:
the collector composition of example 8 was mixed from the following raw materials in weight parts: 48 parts of medicament A, 19 parts of medicament B, 24 parts of sodium p-ethylmandelate and 1 part of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
example 9:
the collector composition of example 9 was obtained from a mixture of the following raw materials, by weight: 37 parts of medicament A, 14 parts of medicament B, 32 parts of sodium p-ethylmandelate and 1.5 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
the active metal ions in monazite are respectively La3+、Ce3+La is known from the Lewis acid-base theory3+And Ce3+All belong to strong acids and are easily coordinated with strong basic anions such as O atoms and N atoms, and alpha-hydroxy sodium palmitate, N-lauroyl sodium sarcosinate and sodium p-ethylmandelate in the collector composition provided by the embodiment can be coordinated with La in O-O or O-N coordination mode3 +、Ce3+Coordination; and the electron-withdrawing effect of the alpha-hydroxy sodium palmitate on the alpha-substituent in the molecule of the sodium ethyl mandelate can improve the selectivity of the action of the medicament and the mineral; meanwhile, the substituent effect of the alpha position can also improve the dissociation characteristic of the medicament in the ore pulp, thereby reducing the temperature required by flotation. In addition, the addition of methyl isobutyl carbinol can increase the stability of the bubbles in the flotation system.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A collector composition for use in flotation recovery of monazite from zircon heavy sand, comprising, by weight: 35-50 parts of a medicament A, 10-30 parts of a medicament B, 20-40 parts of sodium p-ethylmandelate and 1-2 parts of methyl isobutyl carbinol; wherein the medicament A is alpha-substituted fatty acid salt, and the structural formula is as follows:
in the formula, R1Is C10～C15Alkyl of R2Is any one of OH, Cl and Br, R3Is H, Na, K, NH4Any one of the groups;
the structural formula of the medicament B is as follows:
in the formula (II), R'1Is C10～C12Alkyl of R'2Is C1～C2Alkyl or H, R'3Is C1～C3Alkyl of R'4Is H, Na, K, NH4Any one of the groups.
2. A collector composition for use in flotation recovery of monazite from zircon heavy sand according to claim 1, wherein the agent a is sodium alpha-hydroxypalmitate and the agent B is sodium N-lauroylsarcosine.
3. A collector composition for use in flotation recovery of monazite from zircon heavy sand according to claim 2, comprising, by weight components: 40 parts of alpha-hydroxy sodium palmitate, 20 parts of N-lauroyl sodium sarcosinate, 39 parts of sodium p-ethylmandelate and 1 part of methyl isobutyl carbinol.
4. A collector composition for use in flotation recovery of monazite from zircon heavy sand according to claim 2, comprising, by weight components: 45 parts of alpha-hydroxy sodium palmitate, 25 parts of N-lauroyl sodium sarcosinate, 29 parts of sodium p-ethylmandelate and 1.2 parts of methyl isobutyl carbinol.
5. A collector composition for use in flotation recovery of monazite from zircon heavy sand according to claim 2, comprising, by weight components: 38 parts of alpha-hydroxy sodium palmitate, 15 parts of N-lauroyl sodium sarcosinate, 34 parts of sodium p-ethylmandelate and 1.5 parts of methyl isobutyl carbinol.
6. A collector composition for use in flotation recovery of monazite from zircon heavy sand according to claim 1, comprising, by weight components: 42 parts of a medicament A, 28 parts of a medicament B, 25 parts of sodium p-ethyl mandelate and 1.8 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
7. a collector composition for use in flotation recovery of monazite from zircon heavy sand according to claim 1, comprising, by weight components: 36 parts of a medicament A, 12 parts of a medicament B, 35 parts of sodium p-ethylmandelate and 2 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
8. a collector composition for use in flotation recovery of monazite from zircon heavy sand according to claim 1, comprising, by weight components: 46 parts of a medicament A, 14 parts of a medicament B, 28 parts of sodium p-ethylmandelate and 2 parts of methyl isobutyl carbinol; the structural formula of the medicament A is as follows:
the structural formula of the medicament B is as follows:
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| CN111515029B (en) * | 2020-04-30 | 2022-05-17 | 江西理工大学 | Collecting agent for separating monazite and ilmenite and using method thereof |
| CN111715408B (en) * | 2020-06-30 | 2021-07-02 | 中南大学 | A flotation agent for flotation of fluorite in scheelite and its flotation method |
| CN112495577B (en) * | 2020-12-28 | 2022-03-22 | 海南文盛新材料科技有限公司 | Ore dressing process for separating zirconite by using grading jigger |
| CN118162287B (en) * | 2024-05-14 | 2024-08-06 | 中国矿业大学(北京) | Method for recovering tin from tin polymetallic ore |
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