CN104761678A - Method for preparing flocculating agent for dry discharge of tailings - Google Patents
Method for preparing flocculating agent for dry discharge of tailings Download PDFInfo
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- CN104761678A CN104761678A CN201510168210.6A CN201510168210A CN104761678A CN 104761678 A CN104761678 A CN 104761678A CN 201510168210 A CN201510168210 A CN 201510168210A CN 104761678 A CN104761678 A CN 104761678A
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Abstract
The invention relates to a method for preparing a flocculating agent for dry discharge of tailings. The flocculating agent contains acrylamide, acrylic acid, 2-acrylamido-2-methyl propane sulfonic acid and dodecyl acrylate; an organic polymer flocculating agent for dry discharge of tailings is obtained by polymerization reaction of a low-temperature compound initiating system, curing, pelleting, drying and crushing treatment; and the ratio of various functional monomers can be adjusted according to the property of tailings materials, so as to obtain the product which is relatively suitable for field application. Compared with a traditional polyacrylamide flocculating agent, the flocculating agent provided by the invention can adapt to field application of dry discharge of the tailings, and is an efficient flocculating agent for dry discharge of tailings. The flocculating agent is white or light yellow granules, has the advantages of being good in solubility, good in stability, easy to store, and good in flocculating effect, and is a flocculating agent for dry discharge of tailings with good performance.
Description
Technical field
This patent relates to a kind of making method of flocculation agent, is specifically related to a kind of making method of tailing dry row flocculation agent.
Background technology
China is ore dressing mining big country, is very widely, is mainly concerned with the mineral courses of processing such as mining, ore dressing, metallurgy in the use of mining and metallurgy field flocculation agent.Need to use a large amount of water in these processes, need effectively to isolate solid mineral from the aqueous solution.Use suitable flocculation agent, concentrating and improving filtration efficiency of fine can be accelerated, thus reach very high separating effect and improve the throughput of equipment, the loss reducing valuable mineral, raising productive rate, accelerate the objects such as the reuse of mine tailing wastewater.
Along with the exploitation of Mineral resources are developed in depth and breadth, how to enhance productivity, save energy, reduction consumption, maximally utilise limited Mineral resources, cut the waste the target becoming and pursue in current mining industry field.Flocculant product has greatly promoted rational development and utilization of mineral resources in the reasonable application in this field.
Need to use a large amount of water in these processes in ore dressing field such as iron, nickel, gold and silver, copper, aluminium, lead, zinc at present, effectively mineral solids is isolated from the aqueous solution, use flocculation agent that solid mineral can be impelled to sink very soon, therefore Hhigh-efficient thickener is able to apply in the concentrate and tailings system of a large amount of mineral treatment process, the use of flocculation agent can be accelerated the concentrated of fine and improve filtration efficiency, thus improve mineral and water separating effect, enhance productivity, reduce tailing stream and become estranged and reduce production run cost.
Therefore, developing the mining industry Chemical Industry of China rapidly, develop the product of suitable for China, and be applied to production in time, is the key of dealing with problems.And in many mining industry chemical, flocculation agent will play vital impact.
Summary of the invention
This patent object is to provide a kind of production method of tailing dry row flocculation agent.This flocculation agent is a kind of white or faint yellow particle, has that solvability is good, good stability, applied widely, easy storage, the features such as flocculating effect is good, solid-liquid separation superior performance, more can adapt to tailing dry row rig-site utilization, be a kind of tailing dry row flocculation agent efficiently.
This flocculation agent is polymerized by acrylamide, vinylformic acid, 2-acrylamide-2-methylpro panesulfonic acid, dodecylacrylate the multipolymer obtained by low temperature composite initiation system.The basis of traditional acrylamide monomer introduces three kinds of function monomers, strengthen the effect that complicated mine tailing recirculated water tackled by flocculation agent, wherein acrylic acid wetting ability introducing increase multipolymer, because the hydrophilicity of hydroxy-acid group is superior, the solubility property of high molecular polymer product can be improved, this flocculation agent is made just can be all dissolved in water, than the efficiency that traditional flocculant is doubled being less than 30 minutes; Containing sulfonic acid group on copolymer molecule chain, this group is strong polar group, it is better water-soluble that its very strong hydrophilic interaction and electrostatic repulsion forces make multipolymer have, greatly increase the hydrodynamic volume of molecular chain, add molecule chain rigidity, and hydrodynamic volume does not change with pH substantially.The more important thing is that multipolymer has outstanding heat and salt resistance, with divalent cation Ca
2+, Mg
2+can not generate precipitation, can tackle complicated mine tailing circulating water system, the impurity in recirculated water can not have an impact to flocculation agent, keeps the flocculating effect of flocculant product; Long-chain alkyl groups in multipolymer is that hydrophobic grouping introduces hydrophobic grouping in Macroscopic single crystal, is improved the temperature and shearing sustainability of polymkeric substance by the heat resistance and salt tolerance of hydrophobic grouping.Water-soluble polymers containing hydrophobic grouping is close with the water medium viscosity effect containing high salinity at fresh water, and molecular weight does not lose, and ensures the flocculating polymer bridging action effect of polymeric flocculant.
In order to synthesize this flocculation agent, adopt following technical scheme:
1. first four kinds of comonomers A, B, C, D are proportionally configured to reaction solution, the water-content of reaction solution is 65%, and comonomer total amount is 35%.The ratio of components of each copolymerize monomer is:
40%-85% comonomer A
5%-40% comonomer B
5%-35% comonomer C
1%-3% comonomer D
Above content is all weight percentage
Wherein comonomer A is the vinyl monomer containing amide group and unsaturated double-bond.Such as: acrylamide, Methacrylamide.Preferred acrylamide;
Comonomer B is the vinyl monomer containing hydrophilic carboxylic acid's group and unsaturated double-bond, such as: vinylformic acid, methacrylic acid, Propylene glycol monoacrylate.Preferred vinylformic acid;
Comonomer C is the vinyl monomer containing sulfonic acid group and unsaturated double-bond, such as: 2-acrylamide-2-methylpro panesulfonic acid, and sodium allylsulfonate, Sodium styrene sulfonate, methylpropene sodium sulfonate.Preferred 2-acrylamide-2-methylpro panesulfonic acid;
Comonomer D is the vinyl monomer containing long chain hydrophobic group and unsaturated double-bond, such as: dodecylacrylate, aliphatic acrylate, octadecyl acrylate.Preferred dodecylacrylate;
2. the reaction solution configured is adjusted between pH value to 7.0 ~ 7.5, be then cooled to zero degree;
3. the reaction solution of the 2nd step is poured in reactor, logical nitrogen deoxygenation 30 minutes;
4. add low temperature composite initiator, add initiator, treat the thickness that solution becomes, stop logical nitrogen, sealing, insulation;
5. wait until temperature not when rising, reaction terminates, and now solution is reacted into blob of viscose, takes out blob of viscose, granulation, dries, and pulverizes, obtains finished product tailing dry row flocculation agent.
The fracturing liquid nanometer that this patent relates to is fallen filtering agent and is compared with prior art had following advantage:
(1) flocculating effect is good, is more conducive to solid-liquid separation effect during tailing dry row;
(2) dissolution rate is fast, in timely northerly winter, within 30 minutes, can dissolve completely;
(3) applied widely, the tailing dry row that can tackle the complicated ore dressing field such as iron, nickel, gold and silver, copper, aluminium, lead, zinc uses;
(4) working substance content is high, and onsite application amount is few, is convenient to transport.
Embodiment
Below by specific examples, this patent building-up process is described in detail.
Embodiment 1
Raw material prepares: acrylamide, vinylformic acid, 2-acrylamide-2-methylpro panesulfonic acid, dodecylacrylate.
Solution preparation: weigh 650g deionized water, under whipped state, add 245g acrylamide, 70g vinylformic acid, 31.5g 2-acrylamide-2-methylpro panesulfonic acid, 3.5g dodecylacrylate, be stirred to and dissolve completely.
The adjustment of solution: the reaction solution sodium hydroxide prepared is regulated PH to 7 ~ 7.5, is cooled to 0 DEG C.
The preparation of flocculation agent: pour in reactor by 1000g reaction solution, passes into high pure nitrogen 30 minutes, adds 20mg initiator V50 in order, 30mg sodium formiate, 30mg tertbutyl peroxide, 20mg ferrous sulfate, after adding ferrous sulfate, reaction solution becomes sticky thick, stops logical nitrogen, sealing.
The aftertreatment of flocculation agent: taken out by completely reacted flocculation agent colloid, pelletizing, is cut into the little micelle of 3mm ~ 5mm, puts into the oven for drying 4 hours of 60 DEG C, takes out drying object, pulverizes with pulverizer, and screening, obtains tailing dry row and use flocculation agent finished product.
Embodiment 2
Raw material prepares: acrylamide, vinylformic acid, 2-acrylamide-2-methylpro panesulfonic acid, dodecylacrylate.
Solution preparation: weigh 650g deionized water, under whipped state, add 175g acrylamide, 45.5g vinylformic acid, 122.5g 2-acrylamide-2-methylpro panesulfonic acid, 7g dodecylacrylate, be stirred to and dissolve completely.
The adjustment of solution: the reaction solution sodium hydroxide prepared is regulated PH to 7 ~ 7.5, is cooled to 0 DEG C.
The preparation of flocculation agent: pour in reactor by 1000g reaction solution, passes into high pure nitrogen 30 minutes, adds 20mg initiator V50 in order, 30mg sodium formiate, 30mg tertbutyl peroxide, 20mg ferrous sulfate, after adding ferrous sulfate, reaction solution becomes sticky thick, stops logical nitrogen, sealing.
The aftertreatment of flocculation agent: taken out by completely reacted flocculation agent colloid, pelletizing, is cut into the little micelle of 3mm ~ 5mm, puts into the oven for drying 4 hours of 60 degree, takes out drying object, pulverizes with pulverizer, and screening, obtains tailing dry row and use flocculation agent finished product.
Embodiment 3
Raw material prepares: acrylamide, vinylformic acid, 2-acrylamide-2-methylpro panesulfonic acid, dodecylacrylate.
Solution preparation: weigh 650g deionized water, under whipped state, add 210g acrylamide, 98g vinylformic acid, 35g 2-acrylamide-2-methylpro panesulfonic acid, 7g dodecylacrylate, be stirred to and dissolve completely.
The adjustment of solution: the reaction solution sodium hydroxide prepared is regulated PH to 7 ~ 7.5, is cooled to 0 DEG C.
The preparation of flocculation agent: pour in reactor by 1000g reaction solution, passes into high pure nitrogen 30 minutes, adds 20mg initiator V50 in order, 30mg sodium formiate, 30mg tertbutyl peroxide, 20mg ferrous sulfate, after adding ferrous sulfate, reaction solution becomes sticky thick, stops logical nitrogen, sealing.
The aftertreatment of flocculation agent: taken out by completely reacted flocculation agent colloid, pelletizing, is cut into the little micelle of 3mm ~ 5mm, puts into the oven for drying 4 hours of 60 degree, takes out drying object, pulverizes with pulverizer, and screening, obtains tailing dry row and use flocculation agent finished product.
Embodiment 4
Raw material prepares: acrylamide, vinylformic acid, 2-acrylamide-2-methylpro panesulfonic acid, dodecylacrylate.
Solution preparation: weigh 650g deionized water, under whipped state, add 140g acrylamide, 122g vinylformic acid, 84g 2-acrylamide-2-methylpro panesulfonic acid, 4g dodecylacrylate, be stirred to and dissolve completely.
The adjustment of solution: the reaction solution sodium hydroxide prepared is regulated PH to 7 ~ 7.5, is cooled to 0 DEG C.
The preparation of flocculation agent: pour in reactor by 1000g reaction solution, passes into high pure nitrogen 30 minutes, adds 20mg initiator V50 in order, 30mg sodium formiate, 30mg tertbutyl peroxide, 20mg ferrous sulfate, after adding ferrous sulfate, reaction solution becomes sticky thick, stops logical nitrogen, sealing.
The aftertreatment of flocculation agent: taken out by completely reacted flocculation agent colloid, pelletizing, is cut into the little micelle of 3mm ~ 5mm, puts into the oven for drying 4 hours of 60 degree, takes out drying object, pulverizes with pulverizer, and screening, obtains tailing dry row and use flocculation agent finished product.
Claims (3)
1. a making method for tailing dry row flocculation agent, is characterized in that, comprises the following steps:
A, first four kinds of comonomers A, B, C, D are proportionally configured to reaction solution, the water-content of reaction solution is 65%, and comonomer total amount is 35%, and wherein the ratio of components of each copolymerize monomer is:
40%-85% comonomer A;
5%-40% comonomer B;
5%-35% comonomer C;
1%-3% comonomer D;
Above content is all weight percentage;
Wherein comonomer A is acrylamide;
Comonomer B is vinylformic acid;
Comonomer C is 2-acrylamide-2-methylpro panesulfonic acid;
Comonomer D is dodecylacrylate;
B, by configure reaction solution sodium hydroxide adjustment pH value to 7.0 ~ 7.5 between, be then cooled to zero degree;
C, reaction solution is poured in reactor, logical nitrogen deoxygenation 30 minutes;
D, add composite initiator, add initiator, treat the thickness that solution becomes, stop logical nitrogen, sealing, insulation;
E, by the time temperature be not when rising, and reaction terminates, and solution reaction becomes blob of viscose, takes out blob of viscose, granulation, dries, and pulverizes, obtain finished product tailing dry row flocculation agent.
2. the making method of a kind of tailing dry row flocculation agent as claimed in claim 1, is characterized in that composite initiator is initiator V50,30 weight part sodium formiates, the 30 weight part tertiary butyls, 20 parts by weight of ferrous sulfate of 20 weight parts.
3. the making method of a kind of tailing dry row flocculation agent as claimed in claim 1, is characterized in that the blob of viscose taken out is cut into the little micelle of square of 3mm ~ 5mm, puts into the oven for drying 4 hours of 60 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131160A (en) * | 2015-09-22 | 2015-12-09 | 焦作市宏达力生物化工有限公司 | Method for synthesizing amine polyacrylate phase inverse emulsion flocculating agent |
| CN114620818A (en) * | 2022-03-24 | 2022-06-14 | 四川禾创智源新材料有限公司 | A kind of flocculant and preparation method thereof |
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| US3658772A (en) * | 1966-10-20 | 1972-04-25 | Dow Chemical Co | Acrylic acid polymers |
| CN1542031A (en) * | 2003-11-07 | 2004-11-03 | 四川大学 | High viscosity-increasing hydrophobic association water-soluble copolymer and its preparation method and use |
| CN1884321A (en) * | 2006-05-23 | 2006-12-27 | 青岛科技大学 | AMPS analog anion copolymer water dispersoid preparation method |
| WO2009074447A1 (en) * | 2007-12-12 | 2009-06-18 | Basf Se | Copolymer based on a compound comprising sulfonic acid |
| CN101649022A (en) * | 2009-07-01 | 2010-02-17 | 山东宝莫生物化工股份有限公司 | Preparing method of lowering residual monomer content of ultra high molecular weight anion-type polyacrylamide |
| CN101845115A (en) * | 2010-04-28 | 2010-09-29 | 北京化工大学 | Preparation method and application of water-based polyacrylamide composite dispersion liquid |
| CN101899129A (en) * | 2010-07-22 | 2010-12-01 | 江苏江达生态科技有限公司 | Preparation method of hydrophobic anion flocculant |
| CN103641950A (en) * | 2013-11-29 | 2014-03-19 | 成都理工大学 | Anionic hydrophobic association partially hydrolyzed polyacrylamide and preparation method and application thereof |
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2015
- 2015-04-11 CN CN201510168210.6A patent/CN104761678A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3658772A (en) * | 1966-10-20 | 1972-04-25 | Dow Chemical Co | Acrylic acid polymers |
| CN1542031A (en) * | 2003-11-07 | 2004-11-03 | 四川大学 | High viscosity-increasing hydrophobic association water-soluble copolymer and its preparation method and use |
| CN1884321A (en) * | 2006-05-23 | 2006-12-27 | 青岛科技大学 | AMPS analog anion copolymer water dispersoid preparation method |
| WO2009074447A1 (en) * | 2007-12-12 | 2009-06-18 | Basf Se | Copolymer based on a compound comprising sulfonic acid |
| CN101649022A (en) * | 2009-07-01 | 2010-02-17 | 山东宝莫生物化工股份有限公司 | Preparing method of lowering residual monomer content of ultra high molecular weight anion-type polyacrylamide |
| CN101845115A (en) * | 2010-04-28 | 2010-09-29 | 北京化工大学 | Preparation method and application of water-based polyacrylamide composite dispersion liquid |
| CN101899129A (en) * | 2010-07-22 | 2010-12-01 | 江苏江达生态科技有限公司 | Preparation method of hydrophobic anion flocculant |
| CN103641950A (en) * | 2013-11-29 | 2014-03-19 | 成都理工大学 | Anionic hydrophobic association partially hydrolyzed polyacrylamide and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131160A (en) * | 2015-09-22 | 2015-12-09 | 焦作市宏达力生物化工有限公司 | Method for synthesizing amine polyacrylate phase inverse emulsion flocculating agent |
| CN114620818A (en) * | 2022-03-24 | 2022-06-14 | 四川禾创智源新材料有限公司 | A kind of flocculant and preparation method thereof |
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Application publication date: 20150708 |