CN106238223B - Melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor and its preparation, application method - Google Patents
Melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor and its preparation, application method Download PDFInfo
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- CN106238223B CN106238223B CN201610955302.3A CN201610955302A CN106238223B CN 106238223 B CN106238223 B CN 106238223B CN 201610955302 A CN201610955302 A CN 201610955302A CN 106238223 B CN106238223 B CN 106238223B
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- melamine
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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
- B03D2201/06—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
- B03D2203/04—Non-sulfide ores
- B03D2203/06—Phosphate ores
Abstract
The invention discloses a kind of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor and its preparation, application methods, including using first, melamine, formaldehyde, reaction prepares six sulfonic acid of melamine to sodium pyrosulfite under alkaline condition, then melamine hexa-acetic acid is prepared, finally six sulfonic acid of melamine, melamine hexa-acetic acid and synergist OP 10 are added in reactor jointly, base substance is prepared under highly basic existence condition, is diluted with water up to inhibitor.The synthesis technology and complex process of the inhibitor are simple and practicable, reaction condition is mild, it is compounded with synergist by two kinds of melamine derivatives, Calcium magnesium minerals can be more effectively complexed in the synergistic effect of the two, the removal efficiency of magnesia during raising direct flotation, direct reverse flotation technological process is reduced to a step direct flotation flow, is of great significance to reducing collector dosage, reducing flotation cost.
Description
Technical field
The invention belongs to phosphate rock floating technical fields, and in particular to a kind of melamine derivative Compositional type phosphate rock floating calcium
Magnesium inhibitor and its preparation, application method.
Background technology
China's phosphate rock resource is abundant but grade is generally relatively low, and most of is mid-low grade collophanite ore, and gangue mineral is mostly with micro-
Fine-grained form is close mutually embedding with phosphorite so that valuable mineral and the extremely difficult monomer dissociation of gangue mineral lead to its sorting property of room temperature
Difference, ore dressing difficulty are big.Carbonate mineral was not only contained for middle-low grade calcium (magnesium) siliceous phosphorite, in gangue mineral but also had contained
Silicate mineral can generally be sorted using direct-reverse flotation technique.Usually in key player on a team's flow, contain magnesium in phosphorus concentrate
Mineral can be also enriched with, and this not only lowers phosphorus concentrate grades, the anti-dosage for selecting medicament also be will increase, to subsequent reverse flotation flowsheet
Cause larger pressure.
Therefore, a kind of efficient phosphate rock floating calcium and magnesium inhibitor is synthesized, is applied in direct flotation flow, is contained in removing
Also inhibit the magnesium-containing mineral of a part while silicon gangue mineral so that this needs to solve the problems, such as using n- anti-technique
It is only necessary to a step direct flotations, shorten flotation process.This is for improving production target, reducing cost, solution life
Producing practical problem has very great meaning.
Invention content
It is an object of the invention to solve the above problem of the existing technology, a kind of melamine derivative compounding is provided
Type phosphate rock floating calcium and magnesium inhibitor and its preparation, application method.The inhibitor utilizes the association between two kinds of melamine derivatives
Same-action greatly strengthens its complexing power, can be with Ca2+、Mg2+Plasma forms stable complex compound, has to Calcium magnesium minerals
Good rejection ability is applied to phosphorus ore direct flotation flow and the removal efficiency of MgO in direct flotation flow can be improved and can simplify
Technological process.
Used technical solution is as follows in order to solve the above problem by the present invention:
A kind of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, is prepared from the following materials:Melamine
Six sulfonic acid of amine, melamine hexa-acetic acid, synergist OP-10, highly basic and water, wherein six sulfonic acid of melamine, melamine six
Acetic acid and the mass ratio of OP-10 are 1-5:1-10:0.1-0.5.
In said program, the highly basic is sodium hydroxide solution or potassium hydroxide solution, a concentration of 0.5mol/L.
The preparation method of above-mentioned melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor is as follows:A is by melamine
It is put into reactor with formaldehyde, adjusts temperature reaction after pH to alkalinity, then adjusted pH value of solution again to alkalinity, delay into solution
Slow temperature reaction after sodium pyrosulfite saturated solution is added dropwise, obtains six sulfonic acid of melamine after product is purified;B with melamine,
Monoxone, methanol and triethylamine prepare melamine hexa-acetic acid crystal;C by six sulfonic acid of melamine, melamine hexa-acetic acid,
OP-10 is put into reactor, then a certain amount of strong base solution is slowly added dropwise thereto, stirs and temperature reaction obtains base substance;d
Base substance and water are configured to solution by a certain percentage.
According to said program, melamine in step a, formaldehyde, sodium pyrosulfite molar ratio be 1:6-10:4-6.
According to said program, pH to 9-11 first is adjusted with strong base solution in step a, solution is warming up to 50-60 DEG C of stirring
30min is reacted, then pH to 10-12 is adjusted with strong base solution, sodium pyrosulfate saturated solution is slowly added dropwise into solution and heats up
To 90 DEG C of reaction 120min.
According to said program, six sulfonic acid of melamine in step c, melamine hexa-acetic acid, OP-10 mass ratio be 1-5:
1-10:0.1-0.5, reaction temperature are 80 DEG C.
According to said program, the mass ratio of base substance and water is 1 in step d:49.
The application method of the melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, including first grind raw ore
After to certain fineness plus water is sized mixing, and sodium carbonate, waterglass, the phosphate rock floating calcium and magnesium inhibitor is then added into ore pulp successively
With collecting agent HX and stir evenly respectively, direct flotation is finally carried out in flotation cell.
According to said program, the sodium carbonate, waterglass, phosphate rock floating calcium and magnesium inhibitor and collecting agent HX addition point
It Wei not 0.3Kg/t, 0.3Kg/t, 1.2Kg/t and 1.2Kg/t.
Melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor provided by the invention has the advantages that:
(1) raw material melamine derives from a wealth of sources, cheap;(2) there is excellent sequestering power by being introduced in melamine molecule
Polar group-SO3H and-CH2COOH, can be with Ca2+、Mg2+Plasma forms complex compound, has to Calcium magnesium minerals fine
Rejection ability;(3) two kinds of melamine derivatives are compounded with synergist OP-10, the synergistic effect of the two can more have
The complexing Calcium magnesium minerals of effect effectively remove the gangue mineral in ore pulp, improve the removal efficiency of magnesia in direct flotation flow;(4)
Traditional direct-reverse flotation technological process is reduced to a step direct flotation flow, is had to reducing collector dosage, reducing flotation cost
Great meaning.
Specific implementation mode
To make those of ordinary skill in the art fully understand technical scheme of the present invention and advantageous effect, with reference to specific
Embodiment illustrates.
Embodiment 1
A kind of preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, includes the following steps:
It takes the formalin that 12.6g melamines and 64.86g mass fractions are 37% to be added in four-hole boiling flask, uses
It is 9-11 that 0.5mol/L sodium hydroxide strong base solutions, which adjust pH value of solution,.Solution is warming up to 50-60 DEG C, is reacted under moderate-speed mixer
PH value of solution is adjusted to 10-11 with 0.5mol/L sodium hydroxide strong base solutions after 30min.It is slowly added dropwise into solution containing 99.0g cokes
Solution is warming up to 90 DEG C of reaction 120min by the saturated aqueous solution of sodium sulfite after being added dropwise to complete, and reaction product is successively through revolving
Concentration, acidification, ethyl alcohol wash to obtain six sulfonic acid of melamine.
With reference to pertinent literature method, melamine hexa-acetic acid is prepared with melamine, monoxone, methanol and triethylamine.Instead
It answers product after suction filtration, pH is adjusted after filter cake priority hot water, ethyl alcohol are washed to acidity, standing crystallizes for 24 hours, and gained crystal is
For melamine hexa-acetic acid.
Six sulfonic acid of 1.0g melamines, 5.0g melamine hexa-acetic acids and 0.2g synergist OP-10 are put into reactor, to
The strong base solution of a concentration of 0.5mol/L sodium hydroxides is wherein slowly added dropwise, stirring and heating makes solution temperature rise to 80 DEG C, protects
A period of time is held up to base substance.By base substance and water in mass ratio 1:49 carry out mixing to obtain the inhibition of phosphate rock floating calcium and magnesium
Agent.It is noted that controlling the proportioning of several substances during preparing inhibitor, the unsuitable too low or mistake of molar concentration of strong base solution
Height, temperature is also unsuitable excessively high, is otherwise easy to cause and becomes turbid and make formula failure.
To evaluate the practical effect of the inhibitor, we select to put three layers of Mashan phosphorus ore for sample ore carried out it is single just
Flotation experiments.The sample ore raw ore chemical composition is following (mass percent %):
The application method of above-mentioned phosphate rock floating calcium and magnesium inhibitor is as follows:
(1) ore pre-treatment:To raw ore muck, mog accounts for 95.12% less than -200 purposes.
(2) direct flotation demagging:166g raw ores are added into flotation cell, is subsequently added into a certain amount of tap water and sizes mixing.Fully
After stirring evenly, pH regulator sodium carbonate (concentration 10wt%) 3kg/t is added into slurry, stirs 2min;Add inhibitor water glass
Glass (concentration 5wt%) 6kg/t stirs 2min;It is subsequently added into inhibitor 1.2kg/t made from the present embodiment, stirs 2min;Finally
Collecting agent HX 1.2kg/t are added, stir 4min.After inflation is bubbled, room temperature direct flotation removes carbonate gangue mineral, when scraper plate
Between be 5min.
With obtained by embodiment 1 inhibitor and its single direct floatation process condition, three layers of Mashan phosphorus ore is put to this
(P2O514.96%, MgO5.88%) raw ore carry out direct flotation after, reach concentrate P2O517.81%, the rate of recovery 91.22%, MgO
The good flotation effect of removal efficiency 14.28%.
Embodiment 2
A kind of preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, includes the following steps:
It takes the formalin that 12.6g melamines and 81.0g mass fractions are 37% to be added in four-hole boiling flask, uses
It is 9-11 that 0.5mol/L sodium hydroxide strong base solutions, which adjust pH value of solution,.Solution is warming up to 50-60 DEG C, is reacted under moderate-speed mixer
PH value of solution is adjusted to 11-12 with 0.5mol/L sodium hydroxide strong base solutions after 30min.It is slowly added dropwise into solution containing 76.0g cokes
The saturated solution of sodium sulfite, 90 DEG C of reaction 120min are warming up to after being added dropwise to complete by solution, and reaction product is dense through rotating successively
Contracting, acidification, ethyl alcohol wash to obtain six sulfonic acid of melamine.
Melamine hexa-acetic acid is prepared with melamine, monoxone, methanol and triethylamine.Reaction product, will after suction filtration
Filter cake adjusts pH to acidity after successively hot water, ethyl alcohol wash, and standing crystallizes for 24 hours, and gained crystal is melamine hexa-acetic acid.
Six sulfonic acid of 2.0g melamines, 8.0g melamine hexa-acetic acids and 0.3g synergist OP-10 are put into reactor, to
The strong base solution of a concentration of 0.5mol/L sodium hydroxides is wherein slowly added dropwise, stirring and heating makes solution temperature rise to 80 DEG C, protects
A period of time is held up to base substance.By base substance and water in mass ratio 1:49 carry out mixing to obtain the inhibition of phosphate rock floating calcium and magnesium
Agent.
To evaluate the practical effect of the inhibitor, we select three layers of big exit of valley phosphorus ore for sample ore carried out it is single just
Flotation experiments.The sample ore raw ore chemical composition is following (mass percent %):
The application method of above-mentioned phosphate rock floating calcium and magnesium inhibitor is as follows:
(1) ore pre-treatment:To raw ore muck, mog accounts for 97.12% less than -200 purposes.
(2) direct flotation demagging:166g raw ores are added into flotation cell, is subsequently added into a certain amount of tap water and sizes mixing.Fully
After stirring evenly, pH regulator sodium carbonate (concentration 10wt%) 3kg/t is added into slurry, stirs 2min;Add inhibitor water glass
Glass (concentration 5wt%) 6kg/t stirs 2min;It is subsequently added into inhibitor 1.2kg/t made from the present embodiment, stirs 2min;Finally
Collecting agent HX1.2kg/t is added, stirs 4min.After inflation is bubbled, room temperature direct flotation removes carbonate gangue mineral, scraper plate time
For 5min.
With obtained by embodiment 2 inhibitor and its single direct floatation process condition, three layers of Mashan phosphorus ore is put to this
(P2O517.09%, MgO5.825%) raw ore carry out direct flotation after, reach concentrate P2O522.15%, the rate of recovery 89.72%, MgO
The good flotation effect of removal efficiency 18.32%.
Embodiment 3
A kind of preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, includes the following steps:
It takes the formalin that 12.6g melamines and 48.65g mass fractions are 37% to be added in four-hole boiling flask, uses
It is 10 that 0.5mol/L sodium hydroxide strong base solutions, which adjust pH value of solution,.Solution is warming up to 55 DEG C, reacts 30min under moderate-speed mixer
0.5mol/L sodium hydroxide strong base solutions are used to adjust pH value of solution to 11 afterwards.The sodium pyrosulfite containing 114g is slowly added dropwise into solution
Solution is warming up to 90 DEG C of reaction 120min by saturated solution after being added dropwise to complete, and reaction product is successively through concentrated by rotary evaporation, acidification, second
Alcohol washs to obtain six sulfonic acid of melamine.
Melamine hexa-acetic acid is prepared with melamine, monoxone, methanol and triethylamine.Reaction product, will after suction filtration
Filter cake adjusts pH to acidity after successively hot water, ethyl alcohol wash, and standing crystallizes for 24 hours, and gained crystal is melamine hexa-acetic acid.
Six sulfonic acid of 5.0g melamines, 10.0g melamine hexa-acetic acids and 0.5g synergist OP-10 are put into reactor,
The strong base solution of a concentration of 0.5mol/L sodium hydroxides is slowly added dropwise thereto, stirring and heating makes solution temperature rise to 80 DEG C,
Kept for a period of time up to base substance.By base substance and water in mass ratio 1:49 carry out mixing to obtain the inhibition of phosphate rock floating calcium and magnesium
Agent.The application method of the phosphate rock floating calcium and magnesium inhibitor is same as above.
Embodiment 4
A kind of preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, includes the following steps:
It takes the formalin that 12.6g melamines and 81g mass fractions are 37% to be added in four-hole boiling flask, uses
It is 9-11 that 0.5mol/L sodium hydroxide strong base solutions, which adjust pH value of solution,.Solution is warming up to 55 DEG C, is reacted under moderate-speed mixer
PH value of solution is adjusted to 10-12 with 0.5mol/L sodium hydroxide strong base solutions after 30min.It is slowly added dropwise into solution burnt sub- containing 95g
The saturated solution of sodium sulphate, after being added dropwise to complete by solution be warming up to 90 DEG C reaction 120min, reaction product successively through concentrated by rotary evaporation,
Acidification, ethyl alcohol wash to obtain six sulfonic acid of melamine.
Melamine hexa-acetic acid is prepared with melamine, monoxone, methanol and triethylamine.Reaction product, will after suction filtration
Filter cake adjusts pH to acidity after successively hot water, ethyl alcohol wash, and standing crystallizes for 24 hours, and gained crystal is melamine hexa-acetic acid.
Six sulfonic acid of 2.0g melamines, 1.0g melamine hexa-acetic acids and 0.1g synergist OP-10 are put into reactor, to
The strong base solution of a concentration of 0.5mol/L sodium hydroxides is wherein slowly added dropwise, stirring and heating makes solution temperature rise to 80 DEG C, protects
A period of time is held up to base substance.By base substance and water in mass ratio 1:49 carry out mixing to obtain the inhibition of phosphate rock floating calcium and magnesium
Agent.The application method of the phosphate rock floating calcium and magnesium inhibitor is same as above.
Claims (9)
1. a kind of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, which is characterized in that prepared by following raw material and
At:Six sulfonic acid of melamine, melamine hexa-acetic acid, synergist OP-10, highly basic and water, wherein six sulfonic acid of melamine, three
The mass ratio of paracyanogen hexaacetic acid and OP-10 are 1-5:1-10:0.1-0.5, by six sulfonic acid of melamine, melamine when preparation
Six acetic acid, OP-10 are put into reactor, then a certain amount of strong base solution is slowly added dropwise thereto, stir and temperature reaction obtains base
Then base substance and water are configured to solution by this substance by a certain percentage.
2. melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor as described in claim 1, it is characterised in that:It is described
Highly basic is sodium hydroxide solution or potassium hydroxide solution, a concentration of 0.5mol/L.
3. the preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, feature described in claim 1 exist
In including the following steps:A adjusts temperature reaction after pH to alkalinity, then again by melamine and formaldehyde input reactor
PH value of solution is adjusted to alkalinity, sodium pyrosulfite saturated solution and temperature reaction are slowly added dropwise into solution, product is purified to obtain three
Six sulfonic acid of poly cyanamid;B prepares melamine hexa-acetic acid crystal;C throws six sulfonic acid of melamine, melamine hexa-acetic acid, OP-10
Enter into reactor, then a certain amount of strong base solution is slowly added dropwise thereto, stirs and temperature reaction obtains base substance;D will be basic
Substance is configured to solution by a certain percentage with water.
4. the preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor as claimed in claim 3, special
Sign is:Melamine in step a, formaldehyde, sodium pyrosulfite molar ratio be 1:6-10:4-6.
5. the preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor as claimed in claim 3, special
Sign is:PH to 9-11 first is adjusted with strong base solution in step a, solution is warming up to 50-60 DEG C and is stirred to react 30min, then
PH to 10-12 is adjusted with strong base solution, sodium pyrosulfate saturated solution is slowly added dropwise into solution and is warming up to 90 DEG C of reactions
120min。
6. the preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor as claimed in claim 3, special
Sign is:Reaction temperature is 80 DEG C in step c.
7. the preparation method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor as claimed in claim 3, special
Sign is:The mass ratio of base substance and water is 1 in step d:49.
8. the application method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor, feature described in claim 1 exist
In including the following steps:Raw ore is milled to after certain fineness first plus water is sized mixing, sodium carbonate, water is then added into ore pulp successively
Glass, phosphate rock floating calcium and magnesium inhibitor and collecting agent HX are simultaneously stirred evenly respectively, and direct flotation is finally carried out in flotation cell.
9. the application method of melamine derivative Compositional type phosphate rock floating calcium and magnesium inhibitor as claimed in claim 8, special
Sign is:The sodium carbonate, waterglass, phosphate rock floating calcium and magnesium inhibitor and collecting agent HX addition be respectively 0.3kg/t,
0.3kg/t, 1.2kg/t and 1.2kg/t.
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CN111036413B (en) * | 2019-11-27 | 2021-01-26 | 东北大学 | Application of inhibitor AA/AMPS in positive flotation and magnesium removal of phosphate ore |
CN112430219A (en) * | 2020-11-23 | 2021-03-02 | 武汉工程大学 | Melamine derivative heavy metal chelating agent and preparation method thereof |
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US4720339A (en) * | 1985-03-15 | 1988-01-19 | American Cyanamid Company | Flotation beneficiation process for non-sulfide minerals |
CN87101820A (en) * | 1987-03-07 | 1988-09-21 | 化学工业部化工矿山设计研究院 | A kind of preparation method who is used for the new dolomite inhibitor sulfomethylated derivative of calcium lignosulfonate of phosphate rock floating |
CN1443607A (en) * | 2003-04-22 | 2003-09-24 | 武汉化工学院 | Phosphate mineral inhibitor, its application in reverse floatation of phosphorus ore and preparation method |
CN103056035A (en) * | 2012-11-15 | 2013-04-24 | 中国海洋石油总公司 | Carbonate inhibitor and preparation method and application thereof |
CN103909018A (en) * | 2014-04-18 | 2014-07-09 | 武汉工程大学 | Collophanite reverse flotation depressing agent and application thereof |
CN104259012A (en) * | 2014-08-05 | 2015-01-07 | 云南红富化肥有限公司 | Composite inhibitor and direct flotation method for low-grade refractory phosphate |
-
2016
- 2016-10-27 CN CN201610955302.3A patent/CN106238223B/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4720339A (en) * | 1985-03-15 | 1988-01-19 | American Cyanamid Company | Flotation beneficiation process for non-sulfide minerals |
CN87101820A (en) * | 1987-03-07 | 1988-09-21 | 化学工业部化工矿山设计研究院 | A kind of preparation method who is used for the new dolomite inhibitor sulfomethylated derivative of calcium lignosulfonate of phosphate rock floating |
CN1443607A (en) * | 2003-04-22 | 2003-09-24 | 武汉化工学院 | Phosphate mineral inhibitor, its application in reverse floatation of phosphorus ore and preparation method |
CN103056035A (en) * | 2012-11-15 | 2013-04-24 | 中国海洋石油总公司 | Carbonate inhibitor and preparation method and application thereof |
CN103909018A (en) * | 2014-04-18 | 2014-07-09 | 武汉工程大学 | Collophanite reverse flotation depressing agent and application thereof |
CN104259012A (en) * | 2014-08-05 | 2015-01-07 | 云南红富化肥有限公司 | Composite inhibitor and direct flotation method for low-grade refractory phosphate |
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