CN110586331B - Modified chitosan inhibitor and flotation separation method thereof - Google Patents
Modified chitosan inhibitor and flotation separation method thereof Download PDFInfo
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- CN110586331B CN110586331B CN201910928866.1A CN201910928866A CN110586331B CN 110586331 B CN110586331 B CN 110586331B CN 201910928866 A CN201910928866 A CN 201910928866A CN 110586331 B CN110586331 B CN 110586331B
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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
- B03D1/012—Organic compounds containing sulfur
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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
- B03D1/02—Froth-flotation processes
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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
- B03D1/08—Subsequent treatment of concentrated product
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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
- B03D1/08—Subsequent treatment of concentrated product
- B03D1/082—Subsequent treatment of concentrated product of the froth product, e.g. washing
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/08—Subsequent treatment of concentrated product
- B03D1/087—Subsequent treatment of concentrated product of the sediment, e.g. regrinding
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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
- B03D2201/06—Depressants
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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
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Abstract
The invention discloses a modified chitosan inhibitor and a flotation separation method thereof, wherein the preparation method of the modified chitosan inhibitor comprises the following steps: dissolving chitosan in an acetic acid aqueous solution, adding thiosemicarbazide, uniformly stirring, clarifying the solution, adding formaldehyde, controlling the reaction temperature to be 20-60 ℃, and reacting for 1-12 hours to obtain a solution containing the modified chitosan inhibitor. The inhibitor has the advantages of low toxicity, safe use, convenient addition, easy obtainment of raw materials and the like, and can well achieve the purpose of reducing impurities in the molybdenum concentrate. The inhibitor can effectively inhibit impurity minerals such as chalcopyrite, pyrite, galena, bismuthate and the like.
Description
Technical Field
The invention relates to a modified chitosan inhibitor and a flotation separation method thereof, belonging to the technical field of molybdenum polymetallic sulfide ore dressing.
Background
Molybdenum is a high-melting-point rare metal, and has relatively stable chemical properties, and the metal molybdenum has the advantages of high strength, high melting point, corrosion resistance, grinding resistance and the like, and also has small expansion coefficient and good electric and heat conduction performance, so that the molybdenum is widely applied to the technical fields of national economy and high technology such as electronic science and technology, metal processing, aerospace and the like.
The molybdenum content is relatively small, and the average content in the earth crust is 1.1 multiplied by 10-6wt%, mainly in the form of sulfides, in huge porphyry-type molybdenum deposits or accretion in huge porphyry-type copper deposits, and in small quantities in sandstone-type and quartz vein-type deposits. The molybdenum resource in China is relatively rich and is the second place in the worldCompared with foreign molybdenum resources, the grade of the molybdenum ore deposit in China is obviously lower, and the molybdenum ore deposit is the associated ore. Therefore, the high-efficiency comprehensive utilization of the molybdenum resource has great significance for the high-quality development of the economy of China.
Flotation is one of the main methods for the efficient and comprehensive utilization of molybdenum resources. For co-associated molybdenum ore, the flotation process typically employed is a hybrid flotation-re-separation process. In the molybdenum bulk concentrate, besides part of valuable metals such as copper and lead, the molybdenum bulk concentrate also contains a small amount of minerals such as pyrite, pyrrhotite and gangue, so the bulk concentrate needs to be subjected to a re-separation flotation process to obtain qualified molybdenum concentrate. However, the impurities such as chalcopyrite, galena, pyrite, and molybdenite have good floatability, which makes the subsequent separation extremely difficult. Currently, the methods for extracting molybdenum and reducing impurities mainly utilize inorganic inhibitors (such as sodium (hydrogen) sulfide, cyanide, potassium dichromate, nocks reagent, etc.) and organic inhibitors (such as sodium thioglycolate, DPS, Orfom D8, M8, etc.). However, the traditional inorganic inhibitor usually has high toxicity and is easy to cause huge damage to human bodies and ecological environment, so that the use of the traditional inorganic inhibitor is limited and is gradually eliminated; although the existing organic inhibitor is greatly improved compared with the traditional inorganic inhibitor, the existing organic inhibitor has poor adaptability to target minerals, and the inhibition effect needs to be further improved. Therefore, the research and development of the novel molybdenum-extracting impurity-reducing inhibitor have important strategic significance for reasonably developing and efficiently utilizing molybdenum resources in China.
Disclosure of Invention
In view of the above, the invention aims to solve the problems of high toxicity, difficult wastewater treatment, serious environmental pollution and the like of inorganic inhibitors in the prior art and simultaneously solve the technical defects of poor ore adaptability, large dosage, poor inhibition effect and the like of the existing organic inhibitors. The modified chitosan inhibitor not only has the advantages of low toxicity, safe use, convenient addition, easy obtainment of raw materials and the like, but also has strong inhibiting power on chalcopyrite, galena, pyrite, bismuthate and other sulfide ores, and can well achieve the purpose of molybdenum extraction and impurity reduction, so the modified chitosan inhibitor can be widely applied to the flotation separation process of molybdenum-lead, molybdenum-sulfur, molybdenum-bismuth, copper-molybdenum, copper-lead-molybdenum and other multi-metal sulfide ores so as to improve the separation index.
In order to achieve the purpose, the invention adopts the following technical scheme:
a modified chitosan inhibitor is prepared by the following steps:
dissolving chitosan in an acetic acid aqueous solution, adding thiosemicarbazide, uniformly stirring, clarifying the solution, adding formaldehyde, controlling the reaction temperature to be 20-60 ℃, and reacting for 1-12 hours to obtain a solution containing modified chitosan, namely the modified chitosan inhibitor;
the modified chitosan inhibitor is a compound with a structure shown in a formula (I),
further, putting 20mL of acetic acid into a 250mL three-necked bottle, adding 150mL of water, fully stirring, adding 8.0g of chitosan in batches, setting the temperature to be 30 ℃, and stirring until the chitosan is completely dissolved, wherein the solution in the three-necked bottle is in a transparent state; stirring for 30min, adding 4.5g of thiosemicarbazide, and continuing stirring until the reactants are completely dissolved and the solution in the three-necked bottle becomes transparent; continuously stirring for 1h, dripping 1mL of 40% formaldehyde into a three-necked bottle, continuously reacting for 10h under full stirring, and adjusting the pH value by using acid and alkali until the bottle is a transparent solution, thus obtaining the inhibitor.
A method for flotation separation of molybdenum from molybdenum bulk concentrate by using a modified chitosan inhibitor comprises the following steps:
s1, rough selection: adding water glass, a molybdenum collecting agent, a foaming agent and a modified chitosan inhibitor into the molybdenum bulk concentrate in sequence, and performing rough concentration for 2-4 min to obtain rough concentrate and rough tailings;
s2, molybdenum scavenging: adding a molybdenum collecting agent, a foaming agent and a modified chitosan inhibitor into the roughed tailings, and carrying out scavenging twice, wherein the time of scavenging twice is 2-5 min, so as to obtain molybdenum scavenging middlings and molybdenum scavenging tailings;
s3, molybdenum concentration: adding a modified chitosan inhibitor into the rough concentration concentrate, wherein the dosage of the modified chitosan inhibitor is 0.2-10.0 kg of the modified chitosan inhibitor, namely 0.2-10.0 kg/t, for treating each ton of molybdenum bulk concentrate, stirring for 1-3 min, and carrying out molybdenum concentration for 2-5 min to obtain a first molybdenum concentration concentrate and a first molybdenum concentration middling;
adding a modified chitosan inhibitor into the first molybdenum concentration concentrate, wherein the using amount of the modified chitosan inhibitor is less than or equal to 5.0kg/t, stirring for 1-3 min, and carrying out molybdenum concentration for 2-5 min to obtain a second molybdenum concentration concentrate and a second molybdenum concentration middling;
adding a modified chitosan inhibitor into the second molybdenum concentration concentrate, wherein the using amount of the modified chitosan inhibitor is less than or equal to 2.0kg/t, stirring for 1-3 min, and performing molybdenum concentration for 2-5 min to obtain a third molybdenum concentration concentrate and a third molybdenum concentration middling;
and adding a modified chitosan inhibitor into the third molybdenum concentration concentrate, wherein the dosage of the modified chitosan inhibitor is less than or equal to 1.0kg/t, stirring for 1-3 min, and carrying out molybdenum concentration for 2-5 min to obtain a fourth molybdenum concentration concentrate and a fourth molybdenum concentration middling.
Further, the molybdenum collector is a hydrocarbon oil collector, including but not limited to kerosene and diesel oil.
Further, the foaming agent is one or more of C8-C12 alcohol, 2# oil and methyl isobutyl carbinol.
Furthermore, in the step S1, the dosage of the water glass is less than or equal to 5.0kg/t, the dosage of the modified chitosan inhibitor is 0.2-15.0 kg/t, the dosage of the molybdenum collecting agent is less than or equal to 30.0g/t, and the dosage of the foaming agent is less than or equal to 20.0 g/t.
Further, in the first molybdenum scavenging in the step S2, the using amount of the molybdenum collecting agent is less than or equal to 20.0g/t, the using amount of the foaming agent is less than or equal to 10.0g/t, and the using amount of the modified chitosan inhibitor is 0.2-5.0 kg/t.
Further, in the first molybdenum scavenging in the step S2, the using amount of the molybdenum collecting agent is less than or equal to 10.0g/t, the using amount of the foaming agent is less than or equal to 5.0g/t, and the using amount of the modified chitosan inhibitor is 0.2-2.0 kg/t.
According to the technical scheme provided by the invention, the modified chitosan inhibitor provided by the invention is prepared by taking chitosan as a first raw material and carrying out Mannich reaction on the first raw material and thiosemicarbazide; the modified chitosan inhibitor has strong inhibiting effect on pyrite, bismuthate, chalcopyrite, galena and the like, and can achieve the purpose of reducing the content of impurities in molybdenum concentrate. The molybdenum extraction and impurity reduction inhibitor provided by the invention has the advantages of low toxicity, safe use, convenient addition, easily obtained raw materials and the like, has strong inhibiting power on pyrite, bismuthate ore, chalcopyrite, galena and the like, and can well achieve the purpose of reducing the impurity content in molybdenum concentrate, so that the molybdenum extraction and impurity reduction inhibitor can be widely applied to the separation and mineral processing process of multi-metal sulfide ores such as molybdenum sulfide, molybdenum bismuth, copper molybdenum, molybdenum lead, copper lead molybdenum and the like so as to improve the separation index.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic flow diagram of the flotation separation of the modified chitosan depressants of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the term "one or more" when used in the presence of raw materials or reagents means at least two kinds, and if not specifically stated, any ratio is indicated when the raw materials or reagents are used in several kinds.
Example 1
The embodiment 1 of the invention discloses a modified chitosan inhibitor and a flotation separation method thereof, and the technical scheme is as follows:
20mL of acetic acid was added to a 250mL three-necked flask, 150mL of water was added, and 8.0g of chitosan was added in portions after sufficient stirring, followed by stirring at 30 ℃ until the chitosan was completely dissolved, at which time the solution in the three-necked flask was transparent. After about 30min, 4.5g of thiosemicarbazide (equivalent to 0.5 times the molar amount of pyran ring) was added and stirring was continued until the reaction was completely dissolved, at which time the flask became transparent again. And (3) continuing stirring for 1h, dropwise adding 1mL of 40% formaldehyde into the three-necked bottle, continuing to react for 10h under sufficient stirring, and adjusting the pH value with acid and alkali until the interior of the bottle is a transparent solution to obtain the modified chitosan inhibitor.
Performing mixed flotation on the copper-molybdenum polymetallic sulfide ore to prepare copper-molybdenum bulk concentrate; the molybdenum grade of the copper-molybdenum bulk concentrate is 8.36 percent, and the copper grade is 1.29 percent. And carrying out flotation on the copper-molybdenum bulk concentrate by adopting the one-roughing, two-sweeping and four-refining process in the above content so as to obtain molybdenum concentrate. Through tests: the grade of the molybdenum concentrate is 48.26%, the copper content is 0.086%, and the molybdenum recovery rate is 48.22%.
Example 2
The embodiment 2 of the invention discloses a modified chitosan inhibitor and a flotation separation method thereof, and the technical scheme is as follows:
performing mixed flotation on the molybdenum-lead polymetallic sulfide ore to prepare copper-molybdenum bulk concentrate; the molybdenum grade of the molybdenum bulk concentrate is 9.44%, and the lead grade is 1.31%. The molybdenum-lead bulk concentrate is subjected to flotation by adopting the one-rough two-sweep four-fine process in the above content, and the modified chitosan inhibitor prepared in example 1 is used as a lead inhibitor, so that molybdenum concentrate is prepared. Through experiments, the method comprises the following steps: the grade of the molybdenum concentrate is 50.36%, the lead content is 0.058%, and the molybdenum recovery rate is 46.66%.
Example 3
The embodiment 3 of the invention discloses a flotation separation method of a modified chitosan inhibitor, which adopts the following technical scheme:
when the modified chitosan inhibitor provided by the embodiment 1 of the invention is used for carrying out a flotation separation test on the molybdenum-lead and copper-molybdenum pure mineral artificial mixed ore, when the dosage of the inhibitor is 10mg/L, the molybdenum-lead and copper-molybdenum pure mineral artificial mixed ore is better separated, at the moment, the grade of molybdenum can reach more than 52.66%, and the content of copper and lead is respectively 2.58% and 1.76%.
In conclusion, the embodiment of the invention has the advantages of low toxicity, safe use, convenient addition, easily obtained raw materials and the like, has strong inhibiting power on chalcopyrite, galena, pyrite, bismuthate and the like, and can well achieve the aim of reducing impurities in molybdenum concentrate, thereby being widely applied to separation and mineral processing processes of multi-metal sulfide ores such as molybdenum sulfide, molybdenum bismuth, copper molybdenum, molybdenum lead, copper lead molybdenum and the like so as to improve the separation index.
As shown in fig. 1, a flotation separation method of a modified chitosan inhibitor adopts a flotation process of 'one rough sweep and four fine', and the medicament dosage in fig. 1 does not include a left endpoint value of '0'; "kg/t" indicates how many kilograms of chemical agent are added per ton of molybdenum bulk concentrate, and "g/t" indicates how many grams of chemical agent are added per ton of molybdenum bulk concentrate.
In conclusion, the thiourea compound flotation separation inhibitor prepared by the embodiment of the invention has the advantages of low toxicity, safe use, convenient addition, easily obtained raw materials and the like, can be directly used or diluted for use, can also be used alone or mixed with other inhibitors, has strong inhibition capability on chalcopyrite, galena, pyrite, bismuthate ore, sphalerite and the like, and can well achieve the purpose of flotation separation of multi-metal sulfide ores, so that the thiourea compound flotation separation inhibitor can be widely applied to the flotation separation process of the multi-metal sulfide ores such as copper lead, lead zinc, molybdenum lead, molybdenum sulfur, molybdenum bismuth, copper molybdenum, copper lead molybdenum and the like so as to improve the separation index.
Claims (7)
1. The modified chitosan inhibitor is characterized by being prepared by the following steps:
dissolving chitosan in an acetic acid aqueous solution, adding thiosemicarbazide, uniformly stirring, clarifying the solution, adding formaldehyde, controlling the reaction temperature to be 20-60 ℃, and reacting for 1-12 hours to obtain a solution containing modified chitosan, namely a modified chitosan inhibitor;
the modified chitosan inhibitor is a compound with a structure shown in a formula (I),
2. a method for flotation separation of molybdenum from molybdenum bulk concentrate using the modified chitosan suppressive agent of claim 1, wherein the steps are as follows:
s1, rough selection: adding water glass, a molybdenum collecting agent, a foaming agent and the modified chitosan inhibitor into the molybdenum bulk concentrate in sequence, and performing rough concentration for 2-4 min to obtain rough concentrate and rough tailings;
s2, molybdenum scavenging: adding a molybdenum collecting agent, a foaming agent and the modified chitosan inhibitor into the roughed tailings, and carrying out twice scavenging, wherein the time of the twice scavenging for molybdenum is 2-5 min, so as to obtain molybdenum scavenging middlings and molybdenum scavenging tailings;
s3, molybdenum concentration: adding the modified chitosan inhibitor into the rough concentration concentrate, wherein the amount of the modified chitosan inhibitor is 0.2-10.0 kg of the modified chitosan inhibitor, namely 0.2-10.0 kg/t, for treating each ton of molybdenum bulk concentrate, stirring for 1-3 min, and carrying out molybdenum concentration for 2-5 min to obtain a first molybdenum concentration concentrate and a first molybdenum concentration middling;
adding the modified chitosan inhibitor into the first molybdenum concentration concentrate, wherein the using amount of the modified chitosan inhibitor is less than or equal to 5.0kg/t, stirring for 1-3 min, and carrying out molybdenum concentration for 2-5 min to obtain a second molybdenum concentration concentrate and a second molybdenum concentration middling;
adding the modified chitosan inhibitor into the second molybdenum concentration concentrate, wherein the using amount of the modified chitosan inhibitor is less than or equal to 2.0kg/t, stirring for 1-3 min, and carrying out molybdenum concentration for 2-5 min to obtain a third molybdenum concentration concentrate and a third molybdenum concentration middling;
and adding the modified chitosan inhibitor into the third molybdenum concentration concentrate, wherein the dosage of the modified chitosan inhibitor is less than or equal to 1.0kg/t, stirring for 1-3 min, and carrying out molybdenum concentration for 2-5 min to obtain a fourth molybdenum concentration concentrate and a fourth molybdenum concentration middling.
3. The method for separating molybdenum from molybdenum bulk concentrate by flotation through the modified chitosan inhibitor as claimed in claim 2, wherein the molybdenum collector is a hydrocarbon oil collector, including but not limited to kerosene and diesel oil.
4. The method for separating molybdenum from molybdenum bulk concentrate through flotation by using the modified chitosan inhibitor as claimed in claim 2, wherein the foaming agent is one or more of C8-C12 alcohol, 2# oil and methyl isobutyl carbinol.
5. The method for separating molybdenum from molybdenum bulk concentrate through flotation by using the modified chitosan inhibitor as claimed in claim 2, wherein the amount of the sodium silicate used in the step S1 is less than or equal to 5.0kg/t, the amount of the modified chitosan inhibitor is 0.2-15.0 kg/t, the amount of the molybdenum collector is less than or equal to 30.0g/t, and the amount of the foaming agent is less than or equal to 20.0 g/t.
6. The method for separating molybdenum from molybdenum bulk concentrate through flotation by using the modified chitosan inhibitor according to claim 2, wherein in the first molybdenum scavenging in the step S2, the dosage of the molybdenum collector is less than or equal to 20.0g/t, the dosage of the foaming agent is less than or equal to 10.0g/t, and the dosage of the modified chitosan inhibitor is 0.2-5.0 kg/t.
7. The method for separating molybdenum from molybdenum bulk concentrate through flotation by using the modified chitosan inhibitor according to claim 2, wherein in the first molybdenum scavenging in the step S2, the dosage of the molybdenum collector is less than or equal to 10.0g/t, the dosage of the foaming agent is less than or equal to 5.0g/t, and the dosage of the modified chitosan inhibitor is 0.2-2.0 kg/t.
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