CN107952591A - 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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- CN107952591A CN107952591A CN201711202681.XA CN201711202681A CN107952591A CN 107952591 A CN107952591 A CN 107952591A CN 201711202681 A CN201711202681 A CN 201711202681A CN 107952591 A CN107952591 A CN 107952591A
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- rare earth
- type rare
- octyl ether
- phosphosilicate
- earth mine
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 55
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 54
- 238000005188 flotation Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 14
- 229920001214 Polysorbate 60 Polymers 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 7
- UXBZSSBXGPYSIL-UHFFFAOYSA-N phosphoric acid;yttrium(3+) Chemical compound [Y+3].OP(O)(O)=O UXBZSSBXGPYSIL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 17
- -1 Octyl Ether nitrile Chemical class 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 9
- 235000019353 potassium silicate Nutrition 0.000 claims description 9
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 210000003298 dental enamel Anatomy 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- SSILHZFTFWOUJR-UHFFFAOYSA-M hexadecane-1-sulfonate Chemical compound CCCCCCCCCCCCCCCCS([O-])(=O)=O SSILHZFTFWOUJR-UHFFFAOYSA-M 0.000 claims description 6
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 150000007513 acids Chemical class 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000004088 foaming agent Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 239000000344 soap Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 239000012265 solid product Substances 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 150000002825 nitriles Chemical class 0.000 claims 1
- LGAWFGCTQRLGQE-UHFFFAOYSA-N octan-3-ylphosphonic acid Chemical class CCCCCC(CC)P(O)(O)=O LGAWFGCTQRLGQE-UHFFFAOYSA-N 0.000 claims 1
- DWDQAMUKGDBIGM-UHFFFAOYSA-N phosphanylidyneyttrium Chemical compound [Y]#P DWDQAMUKGDBIGM-UHFFFAOYSA-N 0.000 claims 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000012141 concentrate Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- NKJOXAZJBOMXID-UHFFFAOYSA-N 1,1'-Oxybisoctane Chemical compound CCCCCCCCOCCCCCCCC NKJOXAZJBOMXID-UHFFFAOYSA-N 0.000 abstract description 2
- 235000019864 coconut oil Nutrition 0.000 abstract 1
- 239000003240 coconut oil Substances 0.000 abstract 1
- SSILHZFTFWOUJR-UHFFFAOYSA-N hexadecane-1-sulfonic acid Chemical compound CCCCCCCCCCCCCCCCS(O)(=O)=O SSILHZFTFWOUJR-UHFFFAOYSA-N 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229940125717 barbiturate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PGRMNXHYAZYNPG-UHFFFAOYSA-N fluoro hydrogen carbonate Chemical class OC(=O)OF PGRMNXHYAZYNPG-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052590 monazite Inorganic materials 0.000 description 1
- JRZGPWOEHDOVMC-UHFFFAOYSA-N n-hydroxynaphthalene-1-carboxamide Chemical compound C1=CC=C2C(C(=O)NO)=CC=CC2=C1 JRZGPWOEHDOVMC-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
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, is specially a kind of phosphosilicate type Rare Earth Mine flotation collector and its preparation side
Method and application.
Background technology
It is 18,590,000 t that rare earth oxide commercial reserves has been verified in China, accounts for rare earth reserves have been verified in the world 23.6%,
Gently, in, heavy rare earth element it is complete.The species of rare-earth industry mineral is very much, mainly including 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 used, with the different of phenyl ring using the Rare-earth Mine that bastnaesite is main rare-earth mineral mostly at present
One or more of mixing in hydroximic acid, cycloalkyl hydroxamic acid, naphthyl hydroxamic acid are 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 the requirement for meeting environmental protection.
Report is had no to the industrial utilization of phosphosilicate type Rare Earth Mine at present, only laboratory separation index：Certain REO is contained
The extremely low-grade phosphosilicate type Rare Earth Mine for 1.6% is measured, experiment uses A6494 hydroximic acid collecting agents, 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 obtain the rare earth ore concentrate that REO grades are 14.5%, the rate of recovery is 75%.
The content of the invention
It is an object of the invention to provide a kind of phosphosilicate type Rare Earth Mine flotation collector, its collecting ability is strong, concentrate
The rate of recovery is high, and production cost is low, dosage is few, is sorted when being applied especially in phosphosilicate type Rare Earth Mine or xenotime flotation
Effect is good.
The present invention is achieved through the following technical solutions above-mentioned purpose：
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 group-a- amino -1,1- di 2 ethylhexyl phosphonic acids, 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, comprises the following steps：
(1) Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids are synthesized：Octanol and acrylonitrile are added in the presence of sodium hydroxide
Thermal response, generates Octyl Ether nitrile；Again by Octyl Ether nitrile and pyrophosphoric acid in ethanol Hybrid Heating react, obtain Octyl Ether propyl group-
A- amino -1,1- di 2 ethylhexyl phosphonic acids；
Chemical equation involved by synthesis Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids has：
(2) collecting agent compounds：By Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids made from step (1) and cocinic acid,
Cetyl sulfonate and Tween-60 in mass ratio 5~15:60~80:5~10:1~3 is 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 group-a- amino -1,1- di 2 ethylhexyl phosphonic acids is：Will
Octanol and the sodium hydroxide in mass ratio 100 that concentration is 30-40%:1~3 puts into enamel reaction still, is risen after stirring evenly
Temperature is slow added into the acrylonitrile of 0.9 times of octanol amount, maintains the temperature at 60~70 DEG C to 60~70 DEG C, adds after acrylonitrile again
Stop heating after when reaction 1~2 is small, cool to room temperature, stand centrifugation, remove the sodium hydroxide and soap contaminants of precipitation,
Clear liquid is Octyl Ether nitrile, and filter residue focuses on；By Octyl Ether nitrile, pyrophosphoric acid and ethanol in mass ratio 1:1.1~1.2:1.5~
In 1.8 input enamel reaction stills, 60~70 DEG C, when insulation 5~6 is small are heated to, solid product Octyl Ether is obtained after purification removal of impurities
Propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids.
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
9 are pressed with dilute sulfuric acid:1 mass ratio is formulated.
The beneficial effects of the invention are as follows：
In the phosphosilicate type Rare Earth Mine flotation collector formula of the present invention, Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids
With preferable collecting performance and selectivity so that collecting agent collecting ability is strong, and the concentrate rate of recovery is high；And cocinic acid raw material is easy
, fusing point it is relatively low, it is good with respect to other oleic acid resistance to low temperatures so that phosphosilicate type Rare Earth Mine collecting agent production cost is low, use
Amount is few；Cetyl sulfonate is not required to add in use also with certain frothing capacity in addition to collecting ability at the same time
Add foaming agent.The phosphosilicate type Rare Earth Mine flotation collector of the present invention is especially in phosphosilicate type Rare Earth Mine or xenotime flotation
Good separation effect during middle application, has filled up the blank in phosphosilicate type Rare Earth Mine industrial utilization field.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, with reference to specific embodiment 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 octyl groups
Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids, 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：
By the sodium hydroxide in mass ratio 100 that octanol and concentration are 30-40%:2 put into enamel reaction still, and stirring is equal
60 DEG C are warming up to after even, is slow added into the acrylonitrile of 0.9 times of octanol amount, maintains the temperature at 70 DEG C, after adding acrylonitrile, reaction
2 it is small when after stop heating, cool 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；
By Octyl Ether nitrile, pyrophosphoric acid and ethanol in mass ratio 1:1.2:In 1.8 input enamel reaction stills, 70 DEG C are heated to,
Keep the temperature 5 it is small when, purification removal of impurities after obtain product Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids；
Gained Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids are pressed with cocinic acid, cetyl sulfonate and Tween-60
Mass ratio 10：80：8：2 stir evenly after obtain phosphosilicate type Rare Earth Mine flotation collector.
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 top layer ore deposit, raw ore REO grades are 1.6%, and granularity is -2mm after crushing.Raw material passes through
The material that -0.074mm contents are 79% is obtained after ball mill ore grinding, using single flotation sorting process, using laboratory XFD types
Small type flotation machine slightly sweeps three smart flows through one, carries out float test under normal temperature condition, its regime of agent is：Roughing acidifying water glass
Glass (presses 9 by the waterglass and dilute sulfuric acid of modulus 2.6:1 mass ratio is formulated) 2500g/t raw ores, collecting agent 600g/
T raw ores；Scan acidified sodium silicate 500g/t raw ores, collecting agent 200g/t raw ores；Single-minded acidified sodium silicate 200g/t
Raw ore, collecting agent 100g/t raw ores；The diacid waterglass 100g/t raw ores of essence, collecting agent 50g/t raw ores, essence three are empty
In vain.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 octyl groups
Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids, 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：
By the sodium hydroxide in mass ratio 100 that octanol and concentration are 30-40%:3 put into enamel reaction still, and stirring is equal
70 DEG C are warming up to after even, is slow added into the acrylonitrile of 0.9 times of octanol amount, maintains the temperature at 70 DEG C, after adding acrylonitrile, reaction
1 it is small when after stop heating, cool 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；
By Octyl Ether nitrile, pyrophosphoric acid and ethanol in mass ratio 1:1.1:In 1.6 input enamel reaction stills, 70 DEG C are heated to,
Keep the temperature 6 it is small when, purification removal of impurities after obtain product Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids；
Gained Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids are pressed with cocinic acid, cetyl sulfonate and Tween-60
Mass ratio 15：75：7：3 stir evenly after obtain phosphosilicate type Rare Earth Mine flotation collector.
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 grades are 1.47%, and granularity is -2mm after crushing.Raw material
The material that -0.074mm contents are 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 flows through one, carries out float test under normal temperature condition, its regime of agent is：Roughing acidifying water
Glass (presses 9 by the waterglass and dilute sulfuric acid of modulus 2.6:1 mass ratio is formulated) 3000g/t raw ores, collecting agent 280g/
T raw ores；Scan acidified sodium silicate 500g/t raw ores, collecting agent 80g/t raw ores；Single-minded acidified sodium silicate 200g/t is former
Ore deposit, collecting agent 80g/t raw ores；The diacid waterglass 100g/t raw ores of essence, collecting agent 40g/t raw ores, smart three blank.Examination
Test data and be 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 ore deposit rate of recovery is high；Collecting agent cost by compared with conventional test data, finding the present invention is low, and dosage is few, at normal temperatures
It can realize the utilization to phosphosilicate type Rare Earth Mine.
Basic principle, main feature and the advantages of the present invention of the present invention has 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 modifications of the present invention are possible, 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)
- A kind of 1. phosphosilicate type Rare Earth Mine flotation collector, it is characterised in that：It is made of the material of following quality proportioning：5~ 15 parts of Octyl Ether propyl group-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.
- A kind of 2. preparation method of phosphosilicate type Rare Earth Mine flotation collector, it is characterised in that：Comprise the following steps：(1) Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids are synthesized：Octanol and acrylonitrile are heated instead in the presence of sodium hydroxide Should, generate Octyl Ether nitrile；By Octyl Ether nitrile and pyrophosphoric acid, Hybrid Heating is reacted in ethanol again, obtains Octyl Ether propyl group-a- ammonia Base -1,1- di 2 ethylhexyl phosphonic acids；(2) collecting agent compounds：By Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids made from step (1) and cocinic acid, 16 Alkylsulfonate and Tween-60 in mass ratio 5~15:60~80:5~10:1~3 is 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：It is described Step (1) synthesis Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids specific process parameter be：By the sodium hydroxide in mass ratio 100 that octanol and concentration are 30-40%:1~3 puts into enamel reaction still, and stirring is equal 60~70 DEG C are warming up to after even, the acrylonitrile of 0.9 times of octanol amount is slow added into, maintains the temperature at 60~70 DEG C, add propylene Reacted again after nitrile 1~2 it is small when after stop heating, cool to room temperature, stand centrifugation, remove the sodium hydroxide and soaps of precipitation Impurity, clear liquid are Octyl Ether nitrile, and filter residue focuses on；By Octyl Ether nitrile, pyrophosphoric acid and ethanol in mass ratio 1:1.1~1.2:In 1.5~1.8 input enamel reaction stills, it is heated to 60~70 DEG C, when insulation 5~6 is small, solid product Octyl Ether propyl group-a- amino -1,1- di 2 ethylhexyl phosphonic acids are obtained after purification removal of impurities.
- 4. the 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 ore deposit 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 9 are pressed by the waterglass and dilute sulfuric acid of modulus 2.6:1 mass ratio is formulated.
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