CN110152889A - A kind of silicon calcium quality ore Counterfloatating desiliconization removal of impurities combined capturing and collecting agent and its preparation method and application - Google Patents
A kind of silicon calcium quality ore Counterfloatating desiliconization removal of impurities combined capturing and collecting agent and its preparation method and application Download PDFInfo
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- CN110152889A CN110152889A CN201910482897.9A CN201910482897A CN110152889A CN 110152889 A CN110152889 A CN 110152889A CN 201910482897 A CN201910482897 A CN 201910482897A CN 110152889 A CN110152889 A CN 110152889A
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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
- B03D2203/06—Phosphate ores
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Abstract
The invention discloses a kind of silicon calcium quality ore Counterfloatating desiliconization removal of impurities combined capturing and collecting agents and preparation method thereof, by weight, which includes: 20 ~ 30 parts of tertiary amine acetate, 30 ~ 40 parts of quaternary ammonium salts, 15 ~ 30 parts of lauryl sodium sulfate (SDS), 10 ~ 25 parts of alcohols froth modifiers.1) preparation method is comprising steps of according to the ratio mix raw material；2) be added weight be 49 ~ 99 times of step 1) gains gross weight water in, water-bath be sufficiently stirred to get.Collecting agent raw material sources of the present invention are extensive, cheap, collecting ability is strong, dosage is low, resistance to hard water is strong, selectivity is good, concentrate product index is good, the flotation desilication suitable for silicon calcium quality ore.Collecting agent preparing process of the present invention is simple, and flotation desilication foam is crisp and good fluidity, can be under low temperature environment of mining area and ore pulp solution ph realizes that efficient flotation separation cleans between 6 ~ 9.
Description
Technical field
The invention belongs to mineral floating technical fields, and in particular to a kind of silicon calcium quality ore Counterfloatating desiliconization removal of impurities collecting agent
And its preparation method and application.
Background technique
Phosphorus ore is the important chemical industry raw mineral materials of a variety of phosphorus products such as preparing phosphoric acid, phosphate fertilizer and the object of fine phosphorus chemical
Matter basis, occupies an important position and is acted in national economy and social development, has irreplaceability, non-renewable.With
Continually developing totally for rich ore and Yi Xuan phosphate rock resource, domestic phosphate rock resource scarcity increasingly shows.Accelerate to poor refinement phosphorus
Ore resources fully and rationally use, and have far reaching significance to the sustainable development of China's phosphate rock resource.
The silicate impurities such as quartz largely exist in silicon calcium quality ore stone, and the apatite in the ore of part and dolomite glue
Native mineral etc. are mutually cementing, and symbiosis is complicated, only by the single reverse flotation removing carbonate of tradition be difficult to meet downstream phosphoric acid and
Fine phosphate produces the requirement to phosphorus concentrate.Therefore it to obtain and meet relieving haperacidity, the qualified phosphorus concentrate of system fertilizer requirement, using suitable
Beneficiation method is rejected silicate and is necessary.In phosphate rock floating desiliconization impurity removal process, direct flotation relatively maturation and part
Industrialization is had been carried out, but technics comparing is complicated, collecting agent is based on fatty acid soaps, and type is more, foam is more and dosage
Greatly, final phosphorus concentrate is difficult to settle, and subsequent job is difficult, needs to heat flotation when environment temperature is lower, leads to beneficiation cost
It increases.Compared to direct flotation, Counterfloatating desiliconization simple process, dosing is saved, and is met " floating few suppression is more " principle, is wanted to temperature
Ask low, concentrate is easy to subsequent processing.
The research to phosphate reverse flotation desiliconization collecting agent domestic at present is deposited always mainly based on fatty amine, ether amines class
In several common problems: 1) sensitive to sludge, resistance to hard water is poor, consumption is big；2) flotation froth viscosity is big, poor selectivity；
3) tailing defoaming hardly possible, poor fluidity, can not industrialize；3) synthesis material is at high cost, and preparation is complicated, inadequate environmental protection and economy.Such as CN
102205276A discloses a kind of amides collecting agent, and flotation process is complicated, and dosing is excessive, higher cost, no
Easily defoaming；A kind of ether amine collector that CN 101088623A is announced, synthesis condition is harsh, and cost is not also low, de- in phosphorus ore
The case where phosphorus ore impurity component being selected in silicon practice is lower, and universality is narrow, is also not directed to foam practical improvement.Tertiary amine, quaternary ammonium
The cation-collecting agents such as salt in the desiliconizations such as iron ore, bauxite practice using more, and in phosphate reverse flotation desiliconization using upper
Research it is also constantly of interest by field technique of preparing personnel, as CN 106238215A discloses a kind of quaternary ammonium salt cationic
The synthetic method of collecting agent, and it is applied to phosphate rock floating desiliconization for the first time.But the patent does not announce the improvement feelings of practical flotation froth
Moreover P is only related in embodiment2O5Grade is 23.46%, SiO2The single practical mineral of grade 24%, also do not provide concentrate
SiO2Index and removal effect.In addition in newest disclosed cationic desiliconization collecting agent patented technology, rarely have and be related to cation
The practical application of collecting agent and anionic surfactant composite reagent.
In consideration of it, exploitation environmental protection is cheap, good, the collecting excellent effect of selectivity, foaming properties are good, from a wealth of sources and be easy to real
The combined desiliconization collecting agent used is applied, " one medicine of a mine " is more in line with and matches the processing principle that can factually regulate and control, be quick reality
The existing industrialized effective way of phosphate rock floating desiliconization and phosphorus ore take off silicate impurity key problem urgently to be resolved.
Summary of the invention
In view of the shortcomings of the prior art, it is an object of the present invention to provide a kind of silicon calcium quality ore Counterfloatating desiliconizations to remove
Miscellaneous collecting agent, by weight, which includes:
20 ~ 30 parts of tertiary amine acetate, 30 ~ 40 parts of quaternary ammonium salts, 15 ~ 30 parts of lauryl sodium sulfate (SDS), 10 ~ 25 parts of alcohols bubbles
Foam regulator.
Collecting agent collecting ability provided by the invention is strong, selectivity is good, anti-argillization ability is strong, resistance to hard water, bubble mobility
It is good, environmental protection is cheap, be applicable to flotation at low temperature and can be to carry out efficient separation under faintly acid, neutrality or alkalescent.
In collecting agent of the present invention, due to the presence of lauryl sodium sulfate (SDS), zwitterion pole can be effectively prevented
Property head between in conjunction with too closely and formed precipitating, precipitating when anions and canons collecting agent coexists can be reduced, in addition SDS
Addition surface tension of the amine cation in ore pulp solution system can be greatly lowered, tertiary amine acetate and season can be strengthened
Synergistic function between ammonium salt makes collecting agent have excellent water solubility, collecting performance and stable surface-active.
Collecting agent of the present invention due to zwitterion neutralize and formed special molecular structure, have good anticalcium, magnesium from
The ability of son, i.e., good resistance to hard water ability, while surface nature is insensitive to pH, is applicable to wider ore pulp solution body
System, generally can be between 6.0 ~ -9.0.
Compared to the single amine collector being commonly used on current part industrial practice, collecting agent of the invention be yin-yang from
Sub- hybrid collector, wherein alcohols froth modifier is properly added, while being effectively improved bubble mobility can also be into one
Step promotes the rate of recovery of phosphorus, improves medicament selectivity, it is often more important that desiliconization foam is not more crisp tacky, has good industry
Change application prospect.
It is another object of the present invention to provide the methods for preparing above-mentioned collecting agent, and this method comprises the following steps:
1) by weight, 20 ~ 30 parts of tertiary amine acetate, 30 ~ 40 parts of quaternary ammonium salts, 15 ~ 30 parts of lauryl sodium sulfate (SDS),
10 ~ 25 parts of alcohols froth modifiers, mixing；
2) be added weight be 49 ~ 99 times of step 1) gains gross weight water in, water-bath be sufficiently stirred to get.
It should be pointed out that when preparing collecting agent of the present invention, to bath temperature, mixing time without particular/special requirement, only
It needs each component being dissolved in water.
It is another object of the present invention to provide above-mentioned collecting agent answering in the silicate impurities such as flotation removing quartz
With.For from Selective Separation silicate in silicon calcium quality ore and phosphate, the effect of collecting agent of the invention is more aobvious
It writes.Collecting agent of the present invention can use under conditions of 10 ~ 25 DEG C, the rock phosphate in powder big suitable for clay content, in conjunction with matched flotation
Technique, collector dosage are generally 300 ~ 500g/t raw ore, can obtain the effect that efficient selective excludes silicate impurity.
Beneficial effects of the present invention:
1) combined capturing and collecting agent raw material sources of the invention are extensive, economic and environment-friendly；
2) combined capturing and collecting agent of the invention is selectively good, collecting ability is strong, resistance to hard water, bubble mobility are good；
3) combined capturing and collecting agent of the invention configuration is simple, applied widely, Ke Yi good with anionic surfactant compatibility
The silicate impurities such as efficient removal quartz under low temperature environment of mining area and under wider ore pulp pH value of solution environment.
4) combined capturing and collecting agent of the invention using Mr. Yu's low-grade silicon calcium quality ore flotation when there are good floatation indicators
And required concentration times are only 2 times when reaching above-mentioned floatation indicators, the present invention can save the dosing of one third.Simultaneously originally
Invention collecting agent is of less demanding to flotation conditions, control easy to implement.
Detailed description of the invention
Fig. 1 is flotation process figure of the invention.
Specific embodiment
The present invention is specifically described by embodiment referring to Fig. 1, it is necessary to which indicated herein is following implementation
Example is only intended to that the present invention is further detailed, and should not be understood as limiting the scope of the invention, the field
Some nonessential modifications and adaptations that professional technician is made according to foregoing invention content, still fall within protection of the invention
Range.
Embodiment 1
By 20 parts of the mixture of eight alkyl dimethyl tertiary amide acetate and Dodecyl Dimethyl Amine acetate 1:1(w/w), ten
20 parts of 30 parts of zephiran, 30 parts of lauryl sodium sulfate (SDS), n-octyl alcohol addition weight are above-mentioned substance
In the water that 49 times of gross weight, then under the conditions of 50 DEG C of constant temperature water bath, it is 2.0% that mass percentage concentration, which is made, in stirring after twenty minutes
Desiliconization combined capturing and collecting agent.
For the low-grade silicon calcium quality ore in Guizhou, raw ore P2O5Grade 17.11%, MgO grade 7.21%, SiO2Grade
16.16%.Crushing raw ore accounts for 70% through rod milling to -0.074mm again to -1mm, and sizing mixing to mass concentration is 28%.One section of roughing de-magging
When, ore pulp solution ph is first adjusted to 5.0 with industrial acidic wastewater WFS, then add conventional anion collecting agent WF-01 dosage
400g/t obtains high silicon rough concentrate (P through one roughing de-magging2O5Grade 24.87%, SiO2Grade 27.87%)；Rough concentrate is through two
Solution is first adjusted to pH=6.0 with sodium carbonate by Duan Jingxuan desiliconization, and combined capturing and collecting agent of the invention is added in selected desiliconization for the first time
200g/t, second of addition 100g/t, whole system temperature maintain 15 DEG C.It, can be with through the one thick two single-minded closed circuit flow swept
Obtain P2O5Grade 31.97%, MgO grade 0.81%, SiO2Grade 12.63%, the phosphorus concentrate of the rate of recovery 77.43%.
Embodiment 2
By ten alkyl dimethyl tertiary amide acetate and dodecyldimethylamine base tertiary amine acetate 1:1(w/w) 25 parts of mixture, ten
15 parts of 35 parts of dialkyl dimethyl benzyl ammonium chloride, 25 parts of lauryl sodium sulfate (SDS), tetradecyl alchohol addition weight are above-mentioned object
In the water that 99 times of matter gross weight, then under the conditions of 60 DEG C of constant temperature water bath, mass percentage concentration, which is made, after stirring 30 minutes is
1.0% desiliconization combined capturing and collecting agent.
Obtain high silicon rough concentrate by one roughing de-magging technique in above-described embodiment 1, rough concentrate again through two sections of selected desiliconizations,
Solution is first adjusted to pH=7.0 with sodium carbonate, combined capturing and collecting agent 250g/t of the invention is added in selected desiliconization for the first time, and second
150g/t is added, whole system temperature maintains 19 DEG C, through the one thick two single-minded closed circuit flow swept, can obtain P2O5Grade
32.79%, MgO grade 0.74%, SiO2Grade 11.30%, the phosphorus concentrate of the rate of recovery 75.58%.
Embodiment 3
By 30 parts of the mixture of ten alkyl dimethyl tertiary amide acetate and Dodecyl Dimethyl Amine acetate 1:1(w/w), ten
20 parts of 30 parts of tetraalkyl dimethyl benzyl ammonium chloride, 20 parts of lauryl sodium sulfate (SDS), octadecyl alcolol addition weight are above-mentioned object
In the water that 79 times of matter gross weight, then under the conditions of 70 DEG C of constant temperature water bath, mass percentage concentration, which is made, after stirring 25 minutes is
1.25% desiliconization combined capturing and collecting agent.
Obtain high silicon rough concentrate by one roughing de-magging technique in above-described embodiment 1, rough concentrate again through two sections of selected desiliconizations,
Solution is first adjusted to pH=8.0 with sodium carbonate, combined capturing and collecting agent 300g/t of the invention is added in selected desiliconization for the first time, and second
200g/t is added, whole system temperature maintains 22 DEG C, through the one thick two single-minded closed circuit flow swept, can obtain P2O5Grade
33.79%, MgO grade 0.52%, SiO2Grade 10.70%, the phosphorus concentrate of the rate of recovery 74.19%.
Embodiment 4
By Dodecyl Dimethyl Amine acetate and dodecyldimethylamine base tertiary amine acetate 1:1(w/w) 30 parts of mixture,
25 parts of 35 parts of dodecyl benzyl dimethyl ammonium chloride, 20 parts of lauryl sodium sulfate (SDS), polyethylene glycol addition weight are upper
It states in 49 times of substance gross weight of water, then under the conditions of 55 DEG C of constant temperature water bath, mass percentage concentration is made in stirring after twenty minutes
For 2.0% desiliconization combined capturing and collecting agent.
Obtain high silicon rough concentrate by one roughing de-magging technique in above-described embodiment 1, rough concentrate again through two sections of selected desiliconizations,
Solution is first adjusted to pH=9.0 with sodium carbonate, combined capturing and collecting agent 200g/t of the invention is added in selected desiliconization for the first time, and second
150g/t is added, whole system temperature maintains 25 DEG C, through the one thick two single-minded closed circuit flow swept, can obtain P2O5Grade
32.01%, MgO grade 0.79%, SiO2Grade 12.37%, the phosphorus concentrate of the rate of recovery 76.24%.
From case study on implementation 1 ~ 4 it is found that combined capturing and collecting agent of the present invention can obtain outstanding ore dressing in flotation silico-calcium phosphorus ore refers to
Mark, P2O5Grade is all larger than 32%, MgO grade and is respectively less than 1%, and the rate of recovery is all larger than 75%, has reached industrial acid making fertilizer to one kind
The index request of phosphorus concentrate.It is low that it is also shown dosing when collecting agent of the present invention uses high silicon de-magging concentrate simultaneously, to low product
The rock phosphate in powder sorting of the more impurity compositions in position has good adaptability.
Claims (9)
- The combined capturing and collecting agent 1. a kind of silicon calcium quality ore Counterfloatating desiliconization cleans, which is characterized in that by weight, the collecting agent Including 20 ~ 30 parts of tertiary amine acetate, 30 ~ 40 parts of quaternary ammonium salts, 15 ~ 30 parts of lauryl sodium sulfate (SDS), 10 ~ 25 parts of alcohols bubbles Foam regulator.
- 2. collecting agent according to claim 1, which is characterized in that the tertiary amine acetate is eight alkyl dimethyl tertiary amide vinegar Hydrochlorate, ten alkyl dimethyl tertiary amide acetate, Dodecyl Dimethyl Amine acetate, dodecyldimethylamine base tertiary amine acetate In any two kinds.
- 3. collecting agent according to claim 2, which is characterized in that the tertiary amine acetate is eight alkyl dimethyl tertiary amide vinegar Hydrochlorate, ten alkyl dimethyl tertiary amide acetate, Dodecyl Dimethyl Amine acetate, dodecyldimethylamine base tertiary amine acetate Any two kinds of substances, the mass ratioes of any two kinds of substances is 1:1.
- 4. collecting agent according to claim 1, which is characterized in that the quaternary ammonium salt is ten alkyldimethylbenzylammonium chlorinations Ammonium or dodecyl benzyl dimethyl ammonium chloride or myristyl benzyl dimethyl ammonium chloride.
- 5. collecting agent according to claim 1, which is characterized in that the alcohols froth modifier is n-octyl alcohol, the positive last of the ten Heavenly stems Alcohol, tetradecyl alchohol, octadecyl alcolol, any one in polyethylene glycol.
- 6. such as the preparation method of claim 1 ~ 5 collecting agent, which is characterized in that the preparation method includes the following steps:1) by weight, 20 ~ 30 parts of tertiary amine acetate, 30 ~ 40 parts of quaternary ammonium salts, 15 ~ 30 parts of lauryl sodium sulfate (SDS), 10 ~ 25 parts of alcohols froth modifiers, mixing；2) be added weight be 49 ~ 99 times of step 1) gains gross weight water in, water-bath be sufficiently stirred to get.
- 7. method according to claim 6, which is characterized in that temperature is 50 ~ 70 DEG C when water-bath in step 2, and mixing time is 20~30min。
- 8. combined capturing and collecting agent as described in claim 1 ~ 5 or the combination collecting that method is prepared according to claim 6 Application of the agent in terms of the low-grade silicon calcium quality ore of flotation.
- 9. application according to claim 8, which is characterized in that in application, the pH range of flotation pulp solution be 6.0 ~ 9.0, flotation temperature is 10 ~ 25 DEG C, and combined capturing and collecting agent dosage is 300 ~ 500g/t raw ore.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111570082A (en) * | 2020-06-03 | 2020-08-25 | 瓮福（集团）有限责任公司 | Combined separation process for high-sesqui medium-low grade silico-calcic phosphorite |
| CN111617885A (en) * | 2020-05-18 | 2020-09-04 | 宜都兴发化工有限公司 | Synchronous reverse flotation process for low-magnesium high-sesqui collophanite |
| CN113617533A (en) * | 2021-08-10 | 2021-11-09 | 河北瓮福正昌工贸有限公司 | Phosphorite ore reverse flotation collecting agent and using method thereof |
| CN113695085A (en) * | 2021-06-29 | 2021-11-26 | 郑州大学 | Phosphogypsum desiliconization and decarbonization combined collecting agent and solution preparation method and application thereof |
| CN114653480A (en) * | 2022-03-29 | 2022-06-24 | 武汉工程大学 | Reverse flotation process for synchronously removing silicon and magnesium impurities from collophanite and collecting agent thereof |
| CN114653480B (en) * | 2022-03-29 | 2024-06-25 | 武汉工程大学 | Reverse flotation process for synchronously removing silicon-magnesium impurities from collophanite and collecting agent thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111617885A (en) * | 2020-05-18 | 2020-09-04 | 宜都兴发化工有限公司 | Synchronous reverse flotation process for low-magnesium high-sesqui collophanite |
| CN111617885B (en) * | 2020-05-18 | 2022-09-16 | 宜都兴发化工有限公司 | Synchronous reverse flotation process for low-magnesium high-sesqui collophanite |
| CN111570082A (en) * | 2020-06-03 | 2020-08-25 | 瓮福（集团）有限责任公司 | Combined separation process for high-sesqui medium-low grade silico-calcic phosphorite |
| CN111570082B (en) * | 2020-06-03 | 2022-03-08 | 瓮福（集团）有限责任公司 | Combined separation process for high-sesqui medium-low grade silico-calcic phosphorite |
| CN113695085A (en) * | 2021-06-29 | 2021-11-26 | 郑州大学 | Phosphogypsum desiliconization and decarbonization combined collecting agent and solution preparation method and application thereof |
| CN113617533A (en) * | 2021-08-10 | 2021-11-09 | 河北瓮福正昌工贸有限公司 | Phosphorite ore reverse flotation collecting agent and using method thereof |
| CN113617533B (en) * | 2021-08-10 | 2023-04-25 | 瓮福（集团）有限责任公司 | Phosphorite ore reverse flotation collector and use method thereof |
| CN114653480A (en) * | 2022-03-29 | 2022-06-24 | 武汉工程大学 | Reverse flotation process for synchronously removing silicon and magnesium impurities from collophanite and collecting agent thereof |
| CN114653480B (en) * | 2022-03-29 | 2024-06-25 | 武汉工程大学 | Reverse flotation process for synchronously removing silicon-magnesium impurities from collophanite and collecting agent thereof |
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Application publication date: 20190823 |