CN112973969A - Scheelite collecting agent and preparation method thereof - Google Patents
Scheelite collecting agent and preparation method thereof Download PDFInfo
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- CN112973969A CN112973969A CN202110190147.1A CN202110190147A CN112973969A CN 112973969 A CN112973969 A CN 112973969A CN 202110190147 A CN202110190147 A CN 202110190147A CN 112973969 A CN112973969 A CN 112973969A
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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
- B03D1/018—Mixtures of inorganic and organic compounds
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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
The invention discloses a scheelite collecting agent and a preparation method thereof, wherein the scheelite collecting agent comprises the following raw materials in parts by weight: 60-100 parts of plant asphalt, 10-30 parts of oxidized paraffin soap, 10-30 parts of oleic acid, 5-10 parts of anionic surfactant, 1-5 parts of sodium alginate and 5-15 parts of diethyl phthalate. The scheelite collecting agent has the advantages of wide source of raw materials, good stability, simple manufacturing process and low production cost; meanwhile, the efficiency of mineral separation at normal temperature by using the scheelite collecting agent is high, the grade of the obtained scheelite is high, and the yield of concentrate is improved. The scheelite collecting agent disclosed by the invention does not cause damage to the environment and human body, belongs to an environment-friendly collecting agent, and has a wide application prospect.
Description
Technical Field
The invention relates to the technical field of ore flotation, in particular to a scheelite collecting agent and a preparation method thereof.
Background
In the skarn tungsten deposit, wolframite and scheelite, calcite, fluorite and other calcium-containing gangue minerals are closely symbiotic. Although the floatability of wolframite and scheelite is greatly different, the floatability of scheelite is very similar to that of calcium-containing gangue minerals such as calcite and fluorite. Therefore, the separation of scheelite from calcite, fluorite and the like by flotation is very difficult, so that the scheelite obtained by flotation has low taste and high flotation treatment cost.
At present, the scheelite flotation mainly adopts fatty acid collecting agents, wherein the collecting agents comprise oleic acid, Y-17, 731, 733, oleic acid-naphthenic acid soap and the like, the collecting agents are not easy to inhibit calcium-containing gangue minerals, a large amount of inhibitors are required to be added during use to separate the gangue from the scheelite flotation, and meanwhile, the heating treatment is required to improve the scheelite flotation efficiency;
disclosure of Invention
In view of the above problems, the present invention aims to provide a collector capable of floating scheelite at normal temperature, which has low cost of raw materials, does not need to be heated when used, can obtain high-grade scheelite concentrate by checking at normal temperature, and has high recovery rate and yield.
The white tungsten collecting agent comprises the following raw materials in parts by weight:
60-100 parts of plant asphalt,
10-30 parts of oxidized paraffin wax soap,
10-30 parts of oleic acid
5-10 parts of an anionic surfactant,
1-5 parts of sodium alginate, namely,
5-15 parts of diethyl phthalate.
Preferably, the acid value of the plant asphalt is less than or equal to 40.
Preferably, the anionic surfactant is composed of at least two of alpha-sulfonated fatty acid ester, sodium dodecylbenzenesulfonate, and sodium oleyloxyethanesulfonate.
Further preferably, the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and sodium oleoyloxy ethanesulfonate according to the mass ratio of 1:2-5: 3-8.
Another object of the present invention is to provide a method for preparing the white tungsten collector, comprising the steps of:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to the proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 2-10 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 8-11, and then performing heating treatment at 100-200 ℃ for 30-150 min;
(3) adjusting the pH value of the heated mixed solution to be neutral, and separating out oil phase substances after standing;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
Preferably, the water is added in an amount of 3 to 5 times the total weight of the vegetable pitch, the oxidized paraffin soap and the oleic acid.
Preferably, the reagent used for adjusting the pH value of the mixed solution in the step (2) is sodium carbonate or sodium hydroxide.
Preferably, the heating temperature in step (2) is 120-150 ℃, and the heating time is 60-120 min.
Preferably, the reagent used for adjusting the pH value of the mixed solution in the step (3) is sulfuric acid.
Preferably, the sulfuric acid concentration is 50-90 wt%
Compared with the prior art, the invention has the following beneficial effects: the scheelite collecting agent is novel and unique in composition, takes plant asphalt as a main component, utilizes the characteristic that the specific gravity of the plant asphalt is close to that of water, and combines oxidized paraffin soap, oleic acid, a small amount of inhibitor (sodium alginate) and other auxiliaries, so that the scheelite collecting agent can realize efficient collection of scheelite at normal temperature, and the yield and the taste of concentrate are improved. The collecting agent disclosed by the invention is wide in raw material source, good in stability, simple in manufacturing process and low in production cost, does not cause damage to the environment and human bodies, belongs to an environment-friendly collecting agent, and has a wide application prospect.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A white tungsten collecting agent is composed of the following raw materials in parts by weight:
80 parts of plant asphalt with an acid value of 40,
20 parts of oxidized paraffin wax soap, namely,
oleic acid 30 parts
10 parts of an anionic surfactant, namely 10 parts of a surfactant,
1 part of sodium alginate, namely 1 part of sodium alginate,
10 parts of diethyl phthalate.
Wherein the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and oleoyloxy ethyl sodium sulfonate according to the mass ratio of 1:2: 8.
The preparation method of the white tungsten collecting agent comprises the following steps:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to a proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 4 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 11 by using sodium hydroxide, and then performing heating treatment at the heating temperature of 50 ℃ for 60 min;
(3) adjusting the pH value of the heated mixed solution to be neutral by adopting 65 wt% sulfuric acid, standing and separating out an oil phase substance;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
Example 2
A white tungsten collecting agent is composed of the following raw materials in parts by weight:
100 parts of plant asphalt with the acid value of 35,
10 parts of oxidized paraffin wax soap, namely,
oleic acid 10 parts
5 parts of an anionic surfactant, namely 5 parts of a surfactant,
2.5 parts of sodium alginate, namely sodium alginate,
and 15 parts of diethyl phthalate.
Wherein the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and oleoyloxy ethyl sodium sulfonate according to the mass ratio of 1:5: 3.
The preparation method of the white tungsten collecting agent comprises the following steps:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to a proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 5 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 9 by adopting sodium carbonate, and then performing heating treatment at the heating temperature of 120 ℃ for 120 min;
(3) adjusting the pH value of the heated mixed solution to be neutral by adopting sulfuric acid with the concentration of 90 wt%, and separating out oil phase substances after standing;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
Example 3
A white tungsten collecting agent is composed of the following raw materials in parts by weight:
75 parts of plant asphalt with the acid value of 40,
25 parts of oxidized paraffin wax soap,
oleic acid 30 parts
8 parts of an anionic surfactant, namely 8 parts of an anionic surfactant,
5 parts of sodium alginate, namely sodium alginate,
and 5 parts of diethyl phthalate.
Wherein the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and oleoyloxy ethyl sodium sulfonate according to the mass ratio of 1:3: 5.
The preparation method of the white tungsten collecting agent comprises the following steps:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to a proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 3 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 8 by using sodium hydroxide, and then performing heating treatment at the heating temperature of 130 ℃ for 100 min;
(3) adjusting the pH value of the heated mixed solution to be neutral by adopting 50 wt% sulfuric acid, and separating out oil phase substances after standing;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
Example 4
A white tungsten collecting agent is composed of the following raw materials in parts by weight:
60 parts of plant asphalt with an acid value of 40,
15 parts of oxidized paraffin wax soap, namely,
oleic acid 30 parts
7 parts of an anionic surfactant, namely 7 parts of,
4 parts of sodium alginate, namely sodium alginate solution,
12 parts of diethyl phthalate.
Wherein the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and oleoyloxy ethyl sodium sulfonate according to the mass ratio of 1:4: 5.
The preparation method of the white tungsten collecting agent comprises the following steps:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to a proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 3 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 10 by using sodium hydroxide, and then performing heating treatment at the heating temperature of 150 ℃ for 60 min;
(3) adjusting the pH value of the heated mixed solution to be neutral by adopting 55 wt% sulfuric acid, standing and separating out an oil phase substance;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
Example 5
A white tungsten collecting agent is composed of the following raw materials in parts by weight:
90 parts of plant asphalt with an acid value of 40,
20 parts of oxidized paraffin wax soap, namely,
oleic acid 10 parts
10 parts of an anionic surfactant, namely 10 parts of a surfactant,
1 part of sodium alginate, namely 1 part of sodium alginate,
and 15 parts of diethyl phthalate.
Wherein the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and oleoyloxy ethyl sodium sulfonate according to the mass ratio of 1:5: 8.
The preparation method of the white tungsten collecting agent comprises the following steps:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to a proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 5 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 8 by using sodium hydroxide, and then performing heating treatment at the heating temperature of 140 ℃ for 80 min;
(3) adjusting the pH value of the heated mixed solution to be neutral by adopting sulfuric acid with the concentration of 85 wt%, standing and separating out an oil phase substance;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
Comparative example 1
A white tungsten collecting agent is composed of the following raw materials in parts by weight:
20 parts of oxidized paraffin wax soap, namely,
oleic acid 30 parts
10 parts of an anionic surfactant, namely 10 parts of a surfactant,
10 parts of sodium alginate, namely 10 parts of sodium alginate,
10 parts of diethyl phthalate.
Wherein the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and oleoyloxy ethyl sodium sulfonate according to the mass ratio of 1:2: 8.
The preparation method of the white tungsten collecting agent comprises the following steps:
(1) weighing oxidized paraffin soap and oleic acid according to a proportion, fully mixing, and adding water to prepare a mixed solution, wherein the amount of the water is 4 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 11 by using sodium hydroxide, and then performing heating treatment at the heating temperature of 50 ℃ for 60 min;
(3) adjusting the pH value of the heated mixed solution to be neutral by adopting 65 wt% sulfuric acid, standing and separating out an oil phase substance;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
Comparative example 2
And (3) adjusting the weight part of the sodium alginate in the raw material composition of the comparative example 1 to be 1 part, and obtaining the white tungsten collecting agent by using the rest components and the preparation method which are the same as those of the comparative example 1. The composition of the material comprises the following raw materials in parts by weight:
20 parts of oxidized paraffin wax soap, namely,
oleic acid 30 parts
10 parts of an anionic surfactant, namely 10 parts of a surfactant,
1 part of sodium alginate, namely 1 part of sodium alginate,
10 parts of diethyl phthalate.
Comparative example 3
A white tungsten collecting agent is composed of the following raw materials in parts by weight:
80 parts of plant asphalt with an acid value of 40,
20 parts of oxidized paraffin wax soap, namely,
oleic acid 30 parts
1 part of sodium alginate, namely 1 part of sodium alginate,
10 parts of diethyl phthalate.
Wherein the anionic surfactant is prepared by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and oleoyloxy ethyl sodium sulfonate according to the mass ratio of 1:2: 8.
The preparation method of the white tungsten collecting agent comprises the following steps:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to a proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 4 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 11 by using sodium hydroxide, and then performing heating treatment at the heating temperature of 50 ℃ for 60 min;
(3) adjusting the pH value of the heated mixed solution to be neutral by adopting 65 wt% sulfuric acid, standing and separating out an oil phase substance;
(4) and (3) weighing sodium alginate and diethyl phthalate in proportion, adding the sodium alginate and the diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
The tungsten ore sample is floated by the collecting agents prepared in the examples 1 to 5 and the comparative examples 1 to 3, and the flotation process is as follows:
1) ore pretreatment: carrying out ore crushing treatment on an original tungsten ore sample to ensure that the fineness of the tungsten ore sample is 350 meshes;
2) flotation: adding the crushed raw tungsten ore sample into a flotation tank, and adding water for size mixing, wherein the weight ratio of the water to the raw tungsten ore sample is 10: 1. Fully stirring uniformly, adding the prepared collecting agent, stirring for 60min, and performing floatation at normal temperature after air inflation and bubbling to obtain a crude product, wherein the using amount of the collecting agent is 0.5 kg/t;
3) and then checking the coarse product again according to the step 2), and repeating for 3 times to obtain fine ore.
The obtained fine scheelite is detected, and the data are shown in Table 1
TABLE 1
| Collecting agent | Grade of fine ore | Yield of | Recovery rate |
| Example 1 | 98.5％ | 31.4％ | 72.9％ |
| Example 2 | 98.0％ | 29.6％ | 68.3％ |
| Example 3 | 97.8％ | 30.2％ | 70.0％ |
| Example 4 | 98.1％ | 28.4％ | 65.5％ |
| Example 5 | 98.2％ | 25.8％ | 69.1％ |
| Comparative example 1 | 82.4％ | 16.6％ | 50.7％ |
| Comparative example 2 | 65.2％ | 8.0％ | 33.2％ |
| Comparative example 3 | 71.5％ | 13.5％ | 47.9％ |
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. The white tungsten collecting agent is characterized by comprising the following raw materials in parts by weight:
60-100 parts of plant asphalt,
10-30 parts of oxidized paraffin wax soap,
10-30 parts of oleic acid
5-10 parts of an anionic surfactant,
1-5 parts of sodium alginate, namely,
5-15 parts of diethyl phthalate.
2. A white tungsten collector according to claim 1 wherein the plant bitumen has an acid number of 40 or less.
3. A white tungsten collector according to claim 1 wherein the anionic surfactant is comprised of at least two of an alpha sulfonated fatty acid ester, sodium dodecyl benzene sulfonate, sodium oleoyloxy ethanesulfonate.
4. The white tungsten collector according to claim 3, wherein the anionic surfactant is formed by mixing alpha-sulfonated fatty acid ester, sodium dodecyl benzene sulfonate and sodium oleoyloxy ethyl sulfonate according to a mass ratio of 1:2-5: 3-8.
5. The method of preparing a white tungsten collector according to any one of claims 1 to 4, comprising the steps of:
(1) weighing the plant asphalt, the oxidized paraffin soap and the oleic acid according to the proportion, fully mixing, and then adding water to prepare a mixed solution, wherein the amount of the water is 2-10 times of the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid;
(2) adjusting the pH value of the mixed solution to 8-11, and then performing heating treatment at 100-200 ℃ for 30-150 min;
(3) adjusting the pH value of the heated mixed solution to be neutral, and separating out oil phase substances after standing;
(4) and (3) weighing the anionic surfactant, sodium alginate and diethyl phthalate in proportion, adding the anionic surfactant, sodium alginate and diethyl phthalate into the oil phase substance obtained in the step (3), and fully mixing to obtain the scheelite collecting agent.
6. The method of preparing a white tungsten collector according to claim 5, wherein the water is added in an amount of 3-5 times the total weight of the plant asphalt, the oxidized paraffin soap and the oleic acid.
7. The method for preparing the white tungsten collector according to claim 5, wherein the reagent used for adjusting the pH value of the mixed solution in the step (2) is sodium carbonate or sodium hydroxide.
8. The preparation method of the white tungsten collector according to claim 5, wherein the heating temperature in the step (2) is 120-150 ℃, and the heating time is 60-120 min.
9. The method for preparing the white tungsten collector according to claim 5, wherein the reagent used for adjusting the pH value of the mixed solution in the step (3) is sulfuric acid.
10. The method of preparing a white tungsten collector according to claim 9, wherein the sulfuric acid concentration is 50-90 wt%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU933117A1 (en) * | 1980-09-25 | 1982-06-07 | Предприятие П/Я А-1997 | Collector for non-sulphide ore flotation |
| CN101757983A (en) * | 2010-01-20 | 2010-06-30 | 中南大学 | Tungsten ore floatation collecting agent and application thereof |
| CN106076652A (en) * | 2016-06-15 | 2016-11-09 | 武汉工程大学 | Fluorite flotation collecting agent based on plant asphalt and its preparation method and application |
| CN108480055A (en) * | 2018-04-13 | 2018-09-04 | 北京矿冶科技集团有限公司 | A kind of Scheelite Flotation collecting agent and preparation method thereof |
| CN108672097A (en) * | 2018-05-14 | 2018-10-19 | 广东省资源综合利用研究所 | A kind of scheelite collecting agent and its preparation method and application |
-
2021
- 2021-02-18 CN CN202110190147.1A patent/CN112973969B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU933117A1 (en) * | 1980-09-25 | 1982-06-07 | Предприятие П/Я А-1997 | Collector for non-sulphide ore flotation |
| CN101757983A (en) * | 2010-01-20 | 2010-06-30 | 中南大学 | Tungsten ore floatation collecting agent and application thereof |
| CN106076652A (en) * | 2016-06-15 | 2016-11-09 | 武汉工程大学 | Fluorite flotation collecting agent based on plant asphalt and its preparation method and application |
| CN108480055A (en) * | 2018-04-13 | 2018-09-04 | 北京矿冶科技集团有限公司 | A kind of Scheelite Flotation collecting agent and preparation method thereof |
| CN108672097A (en) * | 2018-05-14 | 2018-10-19 | 广东省资源综合利用研究所 | A kind of scheelite collecting agent and its preparation method and application |
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