CN107952591B - Phosphosilicate type rare earth ore flotation collector and preparation method and application thereof - Google Patents
Phosphosilicate type rare earth ore flotation collector and preparation method and application thereof Download PDFInfo
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- CN107952591B CN107952591B CN201711202681.XA CN201711202681A CN107952591B CN 107952591 B CN107952591 B CN 107952591B CN 201711202681 A CN201711202681 A CN 201711202681A CN 107952591 B CN107952591 B CN 107952591B
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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
- B03D1/014—Organic compounds containing phosphorus
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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
- B03D1/002—Inorganic compounds
-
- 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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
- B03D2203/06—Phosphate ores
Abstract
The invention discloses a phosphosilicate type rare earth ore flotation collector and a preparation method and application thereof; the phosphosilicate type rare earth ore flotation collector consists of the following materials in parts by mass: 5-15 parts of octyl ether propyl-a-amino-1, 1-diphosphonic acid, 60-80 parts of coconut oil acid, 5-10 parts of hexadecyl sulfonate and 1-3 parts of Tween-60. The phosphosilicate type rare earth ore flotation collector disclosed by the invention is strong in collecting capability, high in concentrate recovery rate, low in production cost and small in dosage, and particularly has a good separation effect when being applied to phosphosilicate type rare earth ore or xenotime flotation.
Description
Technical field
The invention belongs to rare-earth technique field, specially a kind of phosphosilicate type Rare Earth Mine flotation collector and its preparation side
Method and application.
Background technique
It is 18,590,000 t that rare earth oxide commercial reserves has been verified in China, accounts for about rare earth reserves have been verified in the world 23.6%,
Gently, in, heavy rare earth element it is complete.There are many type of rare-earth industry mineral, mainly include oxide-based, fluoro carbonate class, phosphoric acid
Salt, silicates, multiple Barbiturates mineral, the most important three kinds of mineral of industrial abstract rare earth metal are monazite at this stage
[(RE,Th,Y)PO4], bastnaesite [RECO3F] and xenotime [(Y, RE) PO4].Rare earth metal is widely used in cleaning energy
The fields such as source, science and techniques of defence, industrial technology, electronic product.
Alkylhydroxamic acid is mostly used greatly, with the different of phenyl ring with the Rare-earth Mine that bastnaesite is main rare-earth mineral at present
The mixing of one or more of hydroximic acid, naphthenic base hydroxamic acid, naphthalene hydroxamic acid is used as collecting agent, although such collecting agent
Better index is achieved in rare earth flotation, but price is high, dosage is big, and it is undesirable that resultant effect is used alone；Band phenyl ring and naphthalene
The agent degradation of ring is difficult, and tailing water is difficult to meet the requirement of environmental protection.
The industrial utilization of phosphosilicate type Rare Earth Mine is had not been reported at present, only laboratory separation index: certain REO is contained
The extremely low-grade phosphosilicate type Rare Earth Mine that amount is 1.6% is tested and uses A6494 hydroximic acid collecting agent, and 1kg/ tons of dosage
Raw ore, inhibitor are waterglass, and foaming agent is pine tar alcohols, under conditions of being heated up to 45 DEG C, through ore grinding-high concentration pulping-
Floatation process can get the rare earth ore concentrate that REO grade is 14.5%, the rate of recovery is 75%.
Summary of the invention
The purpose of the present invention is to provide a kind of phosphosilicate type Rare Earth Mine flotation collectors, and collecting ability is strong, concentrate
The rate of recovery is high, and production cost is low, dosage is few, sorts when applying especially in phosphosilicate type Rare Earth Mine or xenotime flotation
Effect is good.
The present invention through the following technical solutions to achieve the above objectives:
A kind of phosphosilicate type Rare Earth Mine flotation collector, is made of the material of following quality proportioning: 5~15 parts of Octyl Ethers
Propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid, 60~80 parts of cocinic acids, 5~10 parts of cetyl sulfonate, 1~3 part of Tween-60.
A kind of preparation method of phosphosilicate type Rare Earth Mine flotation collector, comprising the following steps:
(1) it synthesizes Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid: octanol and acrylonitrile is added in the presence of sodium hydroxide
Thermal response generates Octyl Ether nitrile；By Octyl Ether nitrile and pyrophosphoric acid, Hybrid Heating is reacted in ethanol again, obtains Octyl Ether propyl-
A- amino -1,1- di 2 ethylhexyl phosphonic acid；
Chemical equation involved in synthesis Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid has:
(2) collecting agent compounds: by Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid made from step (1) and cocinic acid,
Cetyl sulfonate and Tween-60 5~15:60 in mass ratio~80:5~10:1~3 are mixed evenly, and phosphorus silicon is made
Hydrochlorate type Rare Earth Mine flotation collector.
Further, the specific process parameter of step (1) synthesis Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid are as follows: will
Sodium hydroxide 100:1~3 in mass ratio that octanol and concentration are 30-40% are put into enamel reaction still, are risen after mixing evenly
Temperature is slow added into 0.9 times of octanol amount of acrylonitrile, maintains the temperature at 60~70 DEG C to 60~70 DEG C, adds after acrylonitrile again
Stop heating after reaction 1~2 hour, cool to room temperature, stand centrifugation, remove the sodium hydroxide and soap contaminants of precipitation,
Clear liquid is Octyl Ether nitrile, filter residue centralized processing；By Octyl Ether nitrile, pyrophosphoric acid and ethyl alcohol 1:1.1~1.2:1.5 in mass ratio~
In 1.8 investment enamel reaction stills, 60~70 DEG C are heated to, keeps the temperature 5~6 hours, obtains solid product Octyl Ether after purification removal of impurities
Propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid.
Application of the above-mentioned phosphosilicate type Rare Earth Mine flotation collector in phosphosilicate type Rare Earth Mine or xenotime flotation.
Further, the phosphosilicate type Rare Earth Mine flotation collector is in phosphosilicate type Rare Earth Mine or xenotime flotation
In application, do not add foaming agent, the inhibitor of addition is acidified sodium silicate, the acidified sodium silicate by modulus 2.6 waterglass
It is formulated with dilute sulfuric acid by the mass ratio of 9:1.
The beneficial effects of the present invention are:
In phosphosilicate type Rare Earth Mine flotation collector formula of the invention, Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid
With preferable collecting performance and selectivity, so that collecting agent collecting ability is strong, recovery rate of concentrate is high；And cocinic acid raw material is easy
, fusing point it is lower, other opposite oleic acid resistance to low temperatures are good, so that phosphosilicate type Rare Earth Mine collecting agent production cost is low, uses
Amount is few；Cetyl sulfonate also has certain frothing capacity in addition to collecting ability simultaneously, is not required to add in use
Add foaming agent.Phosphosilicate type Rare Earth Mine flotation collector of the invention is especially in phosphosilicate type Rare Earth Mine or xenotime flotation
Good separation effect when middle application has filled up the blank in phosphosilicate type Rare Earth Mine industrial utilization field.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, combined with specific embodiments below to the present invention
It is further elaborated.
Embodiment 1
The phosphosilicate type Rare Earth Mine flotation collector of the present embodiment is made of the material of following quality proportioning: 10 parts of octyls
Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid, 80 parts of cocinic acids, 8 parts of sodium cetanesulfonates, 2 parts of Tween-60.
The preparation method of the phosphosilicate type Rare Earth Mine flotation collector of the present embodiment:
The sodium hydroxide 100:2 in mass ratio that octanol and concentration are 30-40% is put into enamel reaction still, stirring is equal
It is warming up to 60 DEG C after even, is slow added into 0.9 times of octanol amount of acrylonitrile, maintains the temperature at 70 DEG C, after adding acrylonitrile, reaction
Stop heating after 2 hours, cools to room temperature, static centrifugation removes the sodium hydroxide and soap contaminants of precipitation, and clear liquid is
Octyl Ether nitrile, filter residue centralized processing；
Octyl Ether nitrile, pyrophosphoric acid and ethyl alcohol 1:1.2:1.8 in mass ratio are put into enamel reaction still, are heated to 70 DEG C,
Heat preservation 5 hours obtains product Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid after purification removal of impurities；
Gained Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid is pressed with cocinic acid, cetyl sulfonate and Tween-60
Mass ratio 10:80:8:2 obtains phosphosilicate type Rare Earth Mine flotation collector after mixing evenly.
Application of the phosphosilicate type Rare Earth Mine flotation collector of the present embodiment in phosphosilicate type Rare Earth Mine flotation:
Certain phosphosilicate type Rare Earth Mine surface layer mine, raw ore REO grade are 1.6%, and granularity is -2mm after crushing.Raw material warp
The material that -0.074mm content is 79% is obtained after ball mill ore grinding, using single flotation sorting process, using laboratory XFD type
Small type flotation machine slightly sweeps three smart processes through one, carries out float test, regime of agent under normal temperature condition are as follows: roughing acidifying water glass
Glass (is formulated) 2500g/t raw ore, collecting agent 600g/ by the waterglass and dilute sulfuric acid of modulus 2.6 by the mass ratio of 9:1
T raw ore；Scan acidified sodium silicate 500g/t raw ore, collecting agent 200g/t raw ore；Single-minded acidified sodium silicate 200g/t
Raw ore, collecting agent 100g/t raw ore；The diacid waterglass 100g/t raw ore of essence, collecting agent 50g/t raw ore, essence three are empty
It is white.Test data is shown in Table 1.
Embodiment 2
The phosphosilicate type Rare Earth Mine flotation collector of the present embodiment is made of the material of following quality proportioning: 15 parts of octyls
Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid, 75 parts of cocinic acids, 7 parts of sodium cetanesulfonates, 3 parts of Tween-60.
The preparation method of the phosphosilicate type Rare Earth Mine flotation collector of the present embodiment:
The sodium hydroxide 100:3 in mass ratio that octanol and concentration are 30-40% is put into enamel reaction still, stirring is equal
It is warming up to 70 DEG C after even, is slow added into 0.9 times of octanol amount of acrylonitrile, maintains the temperature at 70 DEG C, after adding acrylonitrile, reaction
Stop heating after 1 hour, cools to room temperature, static centrifugation removes the sodium hydroxide and soap contaminants of precipitation, and clear liquid is
Octyl Ether nitrile, filter residue centralized processing；
Octyl Ether nitrile, pyrophosphoric acid and ethyl alcohol 1:1.1:1.6 in mass ratio are put into enamel reaction still, are heated to 70 DEG C,
Heat preservation 6 hours obtains product Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid after purification removal of impurities；
Gained Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid is pressed with cocinic acid, cetyl sulfonate and Tween-60
Mass ratio 15:75:7:3 obtains phosphosilicate type Rare Earth Mine flotation collector after mixing evenly.
Application of the phosphosilicate type Rare Earth Mine flotation collector of the present embodiment in phosphosilicate type Rare Earth Mine flotation:
Rawore in certain phosphosilicate type Rare Earth Mine, raw ore REO grade are 1.47%, and granularity is -2mm after crushing.Raw material
The material that -0.074mm content is 82% is obtained after ball mill ore grinding, using single flotation sorting process, using laboratory XFD
The small type flotation machine of type slightly sweeps three smart processes through one, carries out float test, regime of agent under normal temperature condition are as follows: roughing acidifying water
Glass (is formulated) 3000g/t raw ore, collecting agent 280g/ by the waterglass and dilute sulfuric acid of modulus 2.6 by the mass ratio of 9:1
T raw ore；Scan acidified sodium silicate 500g/t raw ore, collecting agent 80g/t raw ore；Single-minded acidified sodium silicate 200g/t is former
Mine, collecting agent 80g/t raw ore；The diacid waterglass 100g/t raw ore of essence, collecting agent 40g/t raw ore, smart three blank.Examination
It tests data and is shown in Table 1.
1 test data of table
It can be seen that by above-mentioned test data, collecting agent of the invention is strong to phosphosilicate type Rare Earth Mine collecting ability, essence
The mine rate of recovery is high；By compared with previous test data, it is found that collecting agent of the invention is at low cost, dosage is few, at normal temperature
The utilization to phosphosilicate type Rare Earth Mine may be implemented.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (5)
1. a kind of phosphosilicate type Rare Earth Mine flotation collector, it is characterised in that: be made of the material of following quality proportioning: 5~
15 parts of Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acids, 60~80 parts of cocinic acids, 5~10 parts of cetyl sulfonate, 1~3
Part Tween-60.
2. a kind of preparation method of phosphosilicate type Rare Earth Mine flotation collector, it is characterised in that: the following steps are included:
(1) it synthesizes Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid: octanol and acrylonitrile being heated in the presence of sodium hydroxide anti-
It answers, generates Octyl Ether nitrile；By Octyl Ether nitrile and pyrophosphoric acid, Hybrid Heating is reacted in ethanol again, obtains Octyl Ether propyl-a- ammonia
Base -1,1- di 2 ethylhexyl phosphonic acid；
(2) collecting agent compounds: by Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid made from step (1) and cocinic acid, 16
Alkylsulfonate and Tween-60 5~15:60 in mass ratio~80:5~10:1~3 are mixed evenly, and phosphosilicate is made
Type Rare Earth Mine flotation collector.
3. the preparation method of phosphosilicate type Rare Earth Mine flotation collector according to claim 2, it is characterised in that: described
The specific process parameter of step (1) synthesis Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid are as follows:
Sodium hydroxide 100:1~3 in mass ratio that octanol and concentration are 30-40% are put into enamel reaction still, stirring is equal
It is warming up to 60~70 DEG C after even, is slow added into 0.9 times of octanol amount of acrylonitrile, maintains the temperature at 60~70 DEG C, add propylene
Stop heating after reacting again after nitrile 1~2 hour, cools to room temperature, stand centrifugation, remove the sodium hydroxide and soaps of precipitation
Impurity, clear liquid are Octyl Ether nitrile, filter residue centralized processing；
Octyl Ether nitrile, pyrophosphoric acid and ethyl alcohol 1:1.1~1.2:1.5 in mass ratio~1.8 are put into enamel reaction still, are heated to
60~70 DEG C, 5~6 hours are kept the temperature, obtains solid product Octyl Ether propyl-a- amino -1,1- di 2 ethylhexyl phosphonic acid after purification removal of impurities.
4. phosphosilicate type Rare Earth Mine flotation collector described in claim 1,2 or 3 is in phosphosilicate type Rare Earth Mine or phosphorus yttrium
Application in mine flotation.
5. phosphosilicate type Rare Earth Mine flotation collector according to claim 4 is in phosphosilicate type Rare Earth Mine or xenotime
Application in flotation, it is characterised in that: do not add foaming agent, the inhibitor of addition is acidified sodium silicate, the acidified sodium silicate
It is formulated by the waterglass and dilute sulfuric acid of modulus 2.6 by the mass ratio of 9:1.
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| CN110508402B (en) * | 2019-09-16 | 2021-08-24 | 中国地质科学院矿产综合利用研究所 | Low-temperature-resistant double-acid-salt rare earth ore flotation collector and preparation method and application thereof |
| CN110813541B (en) * | 2019-10-24 | 2021-05-28 | 商洛学院 | Collector combination for flotation of monazite and xenotime from fine-grained seashore placer |
| CN113522532B (en) * | 2021-05-13 | 2022-06-24 | 西北矿冶研究院 | Collecting foaming agent for copper-nickel sulfide ore dressing and preparation method thereof |
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