CN103242489A - Preparation method of settling separation agent for red mud in aluminium ores - Google Patents
Preparation method of settling separation agent for red mud in aluminium ores Download PDFInfo
- Publication number
- CN103242489A CN103242489A CN2013101865875A CN201310186587A CN103242489A CN 103242489 A CN103242489 A CN 103242489A CN 2013101865875 A CN2013101865875 A CN 2013101865875A CN 201310186587 A CN201310186587 A CN 201310186587A CN 103242489 A CN103242489 A CN 103242489A
- Authority
- CN
- China
- Prior art keywords
- oil
- emulsion
- preparation
- water
- separating agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a preparation method of a settling separation agent for red mud in aluminium ores, which comprises the following steps: 1) uniformly mixing liquid oil and a low-HLB-value surfactant to obtain an oil phase; 2) mixing a polymerization monomer and the oil phase, and carrying out emulsification on the obtained mixture under the stirring of an emulsification pump so as to form a stable water-in-oil emulsion; 3) feeding nitrogen into the water-in-oil emulsion obtained in the step 2) so as to expel oxygen for protection, and adding an initiator into the obtained product for mixing and reacting so as to obtain a polymerized emulsion; 4) mixing modified salt and the oil phase obtained in the step 1), and carrying out emulsification on the obtained mixture so as to form a stable water-in-oil emulsion; 5) mixing the polymerized emulsion and the water-in-oil emulsion obtained in the step 4), and carrying out modification on the obtained mixture so as to a mixed emulsion; and 6) carrying out reduced pressure distillation on the modified mixed emulsion so as to obtain a finished product with a solid content of 45-55%. Through the addition of a reduced pressure distillation process, the polymerization active components are improved; and because the oil phase adopts non-volatile and biodegradable liquid oil, the process is simple, and obtained polymers are safer to the human body and the environment.
Description
Technical field
The present invention relates to the preparation technology of organic high molecular compound, specifically, relate to the synthesis technique that a kind of aluminium ore is used separating agent.
Background technology
In alumina producing, can produce a large amount of red muds, the settlement separate of red mud is important link of aluminium industry, red-mud settlement need use special-purpose settlement separate dose of aluminium ore when separating, existing aluminium ore adopts the solution polymerization mode to prepare for special-purpose settlement separate dose, this method preparation process viscosity increases fast, heat conduction is difficulty, so product can only be controlled low-solid content, its value has only 20～30%, because the difficult control of this method preparation process temperature is so easily produce cross-linked material, the back is poorly soluble and viscosity is low so this product comes out, and causes existing consumption big when the red-mud settlement separating treatment, floc sedimentation is little, the shortcoming of mud-water separation weak effect; Existing preparation method adopts low boiling point organic solvent, and the polymkeric substance that makes pollutes human body and environment.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of aluminium ore red-mud settlement separating agent, this method makes the solid content of product up to 45～55%, solvability and viscosity all increase, and simultaneously, do not contain the organic solvent that environment and operator are polluted in production process and the product.
The objective of the invention is to be achieved by the following technical programs, a kind of preparation method of aluminium ore red-mud settlement separating agent may further comprise the steps:
(1) with liquid fat and low HLB value tensio-active agent by mass ratio (5～20): 1 mixes the back uses as oil phase;
(2) oil phase that polymerization single polymerization monomer and step (1) are obtained is by mass ratio (1～3): 1 mixes, and carries out emulsification under emulsification pump stirs, and forms stable water-in-oil emulsion;
(3) feed nitrogen in the water-in-oil emulsion that obtains to step (2) and drive the oxygen protection, the initiator that adds this water-in-oil emulsion quality 0.1% simultaneously carries out hybrid reaction and makes polymerized emulsion;
(4) oil phase that modified-salt and step (1) are obtained is by mass ratio (1～4): 1 mixes, and carries out emulsification under emulsification pump stirs, and forms stable water-in-oil emulsion;
(5) water-in-oil emulsion that makes of the polymerized emulsion that makes of step (3) and step (4) is by mass ratio 1:(1～2) mix and carry out modification and obtain mixed emulsion;
(6) mixed emulsion after the modification makes solid content through underpressure distillation and reaches 45～55% finished product.
Described low HLB value tensio-active agent is one or more mixing in sorbitan fatty acid ester, glyceryl stearate, fatty alcohol aliphatic ester, the polyoxyethylene fatty acid ester.
Described polymerization single polymerization monomer refers to acrylamide, vinylformic acid, acrylate or their sodium salt, sylvite; The pH value of polymerization single polymerization monomer is 8～14.
Described liquid fat is Vegetable oil lipoprotein, animal grease or mineral grease.
Described initiator is oil-soluble initiator or water soluble starter.
Modified-salt is sodium acrylate or potassium acrylate in the described step (4).
The viscosity of water-in-oil emulsion is 100cp～500cp in described step (2) and (4).
The modification temperature of described step (5) is 40～90 ℃, and pH value 10～14, modification time are 3～48 hours.
The vacuum tightness of described step (6) underpressure distillation is 0.01MP～0.05MP, distillation time 3～48 hours.
Described oil-soluble initiator is azo two cyanogen in different heptan, and water soluble starter is ammonium persulphate or Sodium Persulfate.
Beneficial effect: the present invention adopts polymerized emulsion and modified emulsion directly to mix, and with respect to traditional oil phase and the slow drop-method of salt solution, saves a large amount of reaction times, enhances productivity, and mixes back dissolving homogeneous; Oil phase adopt can not volatilize, can biodegradable liquid fat, the finished product do not contain organic solvent, reach environmental requirement, safer to environment and operator, reduced pressure distillation process obviously improves solid content height, solvability and the viscosity of product, process steams moisture can recycle, cuts the waste, and product settlement separate effect in the aluminium ore red mud is used improves obvious especially.
Embodiment
Embodiment 1
(1), rape oil and glyceryl stearate are under agitation evenly mixed in the ratio of 5:1, temperature is controlled at 30 ℃, and stirring velocity is 60 rev/mins;
(2), under condition of stirring, vinylformic acid is added in the oil phase, vinylformic acid is 1:1 with the ratio of oil, temperature is controlled at 30～40 ℃, 300 rev/mins of emulsification rotating speeds form stable water-in-oil emulsion;
(3), under condition of stirring, logical nitrogen 2 minutes adds the initiator ammonium persulfate of water-in-oil emulsion quality 0.1%, stirring velocity is at 100 rev/mins, temperature is controlled at 40～45 ℃, stirs 5 minutes;
(4), namely obtain polymerized emulsion after reaction is finished;
(5), rape oil and glyceryl stearate pressed 5:1 under agitation evenly mix, temperature is controlled at 30 ℃, stirring velocity is 60 rev/mins;
(6), under condition of stirring, the modified-salt sodium acrylate is added in the oil phase, sodium acrylate is 1:1 with the ratio of oil, temperature is controlled at 32 ℃, 300 rev/mins of emulsification rotating speeds form stable modification water-in-oil emulsion;
(7), under condition of stirring, polymerized emulsion and modification water-in-oil emulsion are pressed mass ratio 1:1 mix, 400 rev/mins of stirring velocitys, 40 ℃ of modifications 5 hours;
(8), mixed emulsion under vacuum tightness 0.04MP, underpressure distillation 48 hours;
(9), the solid content that obtains finished product after the underpressure distillation is 52%, solvability is molten entirely in five minutes, apparent viscosity is 510cps.
Embodiment 2
(1), be that the ratio of 10:1 is under agitation evenly mixed in proportion with food grade white mineral oil and glyceryl stearate, temperature is controlled at 35 ℃, stirring velocity is 80 rev/mins;
(2), under condition of stirring, vinylformic acid is added in the oil phase, vinylformic acid is that 2:1 mixes with the ratio of oil phase, temperature is controlled at 33 ℃, 100 rev/mins of emulsification rotating speeds form stable water-in-oil emulsion;
(3), under condition of stirring, logical nitrogen 3 minutes adds the initiator Sodium Persulfate of water-in-oil emulsion quality 0.1%, stirring velocity is at 250 rev/mins, temperature is controlled at 50 ℃, stirs 5 minutes;
(4), namely obtain polymerized emulsion after reaction is finished;
(5), be that the ratio of 10:1 is under agitation evenly mixed in proportion with food grade white mineral oil and glyceryl stearate, temperature is controlled at 35 ℃, stirring velocity is 80 rev/mins;
(6), the modified-salt sodium acrylate adds in the oil phase, the ratio of sodium acrylate and oil phase is 2:1, temperature is controlled at 40 ℃, stirring velocity is 80 rev/mins, forms stable modification water-in-oil emulsion;
(7), under condition of stirring, polymerized emulsion and modification water-in-oil emulsion are pressed mass ratio 1:1.5 mix, 380 rev/mins of stirring velocitys, 30 ℃ of modifications 6 hours;
(8), mixed emulsion under vacuum tightness 0.03MP, underpressure distillation 46 hours;
(9), the solid content that obtains finished product after the underpressure distillation is 51%, solvability is molten entirely in five minutes, apparent viscosity is 530cps.
Embodiment 3
(1), be that 12:1 under agitation evenly mixes in proportion with soya-bean oil and sorbitan sesquioleate, temperature is controlled at 40 ℃, stirring velocity is 100 rev/mins;
(2), under condition of stirring, polymerization single polymerization monomer vinylformic acid is added in the oil phase, the ratio of vinylformic acid and oil phase is 2:1, temperature is controlled at 45 ℃, 300 rev/mins of emulsification rotating speeds form stable water-in-oil emulsion;
(3), under condition of stirring, logical nitrogen 3 minutes adds the initiator Sodium Persulfate of water-in-oil emulsion quality 0.1%, stirring velocity is at 280 rev/mins, temperature is controlled at 60 ℃, stirs 5 minutes;
(4), namely obtain polymerized emulsion after reaction is finished;
(5), be that 12:1 under agitation evenly mixes in proportion with soya-bean oil and sorbitan sesquioleate, temperature is controlled at 40 ℃, stirring velocity is 100 rev/mins;
(6), under condition of stirring, the modified-salt sodium acrylate is added in the oil phase, sodium acrylate is 3:1 with the ratio of oil, temperature is controlled at 40 ℃, 450 rev/mins of emulsification rotating speeds form stable modification water-in-oil emulsion;
(7), under condition of stirring, polymerized emulsion and modification water-in-oil emulsion are pressed mass ratio 1:2 mix, 100 rev/mins of stirring velocitys, 36 ℃ of modifications 3 hours;
(8), mixed emulsion under vacuum tightness 0.02MP, underpressure distillation 40 hours;
(9), the solid content that obtains finished product after the underpressure distillation is 53%, solvability is molten entirely in five minutes, apparent viscosity is 550cps.
Embodiment 4
(1), with butter and sorbitan sesquioleate 15:1 in proportion, under agitation evenly mix, temperature is controlled at 60 ℃, stirring velocity is 70 rev/mins;
(2), under condition of stirring, polymerization single polymerization monomer vinylformic acid is added in the oil phase, the ratio of vinylformic acid and oil phase is 2:1, temperature is controlled at 55 ℃, 200 rev/mins of emulsification rotating speeds form stable water-in-oil emulsion;
(3), under condition of stirring, logical nitrogen 4 minutes adds the initiator Sodium Persulfate of water-in-oil emulsion quality 0.1%, stirring velocity is at 280 rev/mins, temperature is controlled at 30 ℃, stirs 5 minutes;
(4), namely obtain polymerized emulsion after reaction is finished;
(5), with butter and sorbitan sesquioleate 15:1 in proportion, under agitation evenly mix, temperature is controlled at 60 ℃, stirring velocity is 70 rev/mins;
(6), under condition of stirring, sodium acrylate is added in the oil phase, the ratio of sodium acrylate and oil phase for 3:1 temperature control at 40 ℃, 150 rev/mins of emulsification rotating speeds form stable modification water-in-oil emulsion;
(7), under condition of stirring, polymerized emulsion and modification water-in-oil emulsion are pressed mass ratio 1:1 mix, 100 rev/mins of stirring velocitys, 30 ℃ of modifications 3 hours;
(8), mixed emulsion under vacuum tightness 0.01MP, underpressure distillation 40 hours;
(9), the solid content that obtains finished product after the underpressure distillation is 55%, solvability is molten entirely in five minutes, apparent viscosity is 540cps.
Embodiment 5
(1), with beans sheep oil and polyoxyethylene fatty acid ester in proportion 20:1 under agitation evenly mix, temperature is controlled at 35 ℃, stirring velocity is 80 rev/mins;
(2), under condition of stirring, vinylformic acid is added in the oil phase, the ratio of vinylformic acid and oil phase is 3:1, temperature is controlled at 45 ℃, 400 rev/mins of emulsification rotating speeds form stable water-in-oil emulsion;
(3), under condition of stirring, logical nitrogen 5 minutes adds the initiator Sodium Persulfate of water-in-oil emulsion quality 0.1%, stirring velocity is at 280 rev/mins, temperature is controlled at 70 ℃, stirs 5 minutes;
(4), namely obtain polymerized emulsion after reaction is finished;
(5), with sheep oil and polyoxyethylene fatty acid ester 20:1 in proportion, under agitation evenly mix, temperature is controlled at 35 ℃, stirring velocity is 80 rev/mins;
(6), under condition of stirring, sodium acrylate is added in the oil phase, the ratio of sodium acrylate and oil phase is 3:1, temperature is controlled at 40 ℃, 150 rev/mins of emulsification rotating speeds form stable modification water-in-oil emulsion;
(7), under condition of stirring, polymerized emulsion and modification water-in-oil emulsion are pressed mass ratio 1:1 mix, 200 rev/mins of stirring velocitys, 40 ℃ of modifications 3 hours;
(8), mixed emulsion under vacuum tightness 0.02MP, underpressure distillation 40 hours;
(9), the solid content that obtains finished product after the underpressure distillation is 53%, solvability is molten entirely in five minutes, apparent viscosity is 520cps.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Any those of ordinary skill in the art, do not breaking away under the technical solution of the present invention scope situation, all can utilize method and the technology contents of above-mentioned announcement that technical solution of the present invention is made many possible changes and modification, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical solution of the present invention, any simple modification of above embodiment being done according to technical spirit of the present invention, be equal to replacements, equivalence changes and modify, all still belong in the scope that technical solution of the present invention protects.
Claims (10)
1. the preparation method of an aluminium ore red-mud settlement separating agent is characterized in that, may further comprise the steps:
(1) with liquid fat and low HLB value tensio-active agent by mass ratio (5～20): 1 mixes the back uses as oil phase;
(2) oil phase that polymerization single polymerization monomer and step (1) are obtained is by mass ratio (1～3): 1 mixes, and carries out emulsification under emulsification pump stirs, and forms stable water-in-oil emulsion;
(3) feed nitrogen in the water-in-oil emulsion that obtains to step (2) and drive the oxygen protection, the initiator that adds this water-in-oil emulsion quality 0.1% simultaneously carries out hybrid reaction and makes polymerized emulsion;
(4) oil phase that modified-salt and step (1) are obtained is by mass ratio (1～4): 1 mixes, and carries out emulsification under emulsification pump stirs, and forms stable water-in-oil emulsion;
(5) water-in-oil emulsion that makes of the polymerized emulsion that makes of step (3) and step (4) is by mass ratio 1:(1～2) mix and carry out modification and obtain mixed emulsion;
(6) mixed emulsion after the modification makes solid content through underpressure distillation and reaches 45～55% finished product.
2. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1, it is characterized in that described low HLB value tensio-active agent is one or more mixing in sorbitan fatty acid ester, glyceryl stearate, fatty alcohol aliphatic ester, the polyoxyethylene fatty acid ester.
3. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1 is characterized in that, described polymerization single polymerization monomer refers to acrylamide, vinylformic acid, acrylate or their sodium salt, sylvite; The pH value of polymerization single polymerization monomer is 8～14.
4. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1 is characterized in that, described liquid fat is Vegetable oil lipoprotein, animal grease or mineral grease.
5. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1 is characterized in that, described initiator is oil-soluble initiator or water soluble starter.
6. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1 is characterized in that, modified-salt is sodium acrylate or potassium acrylate in the described step (4).
7. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1 is characterized in that, the viscosity of water-in-oil emulsion is 100cp～500cp in described step (2) and (4).
8. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1 is characterized in that, the modification temperature of described step (5) is 40～90 ℃, and pH value 10～14, modification time are 3～48 hours.
9. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 1 is characterized in that, the vacuum tightness of described step (6) underpressure distillation is 0.01MP～0.05MP, distillation time 3～48 hours.
10. the preparation method of a kind of aluminium ore red-mud settlement separating agent according to claim 5 is characterized in that, described oil-soluble initiator is azo two cyanogen in different heptan, and water soluble starter is ammonium persulphate or Sodium Persulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101865875A CN103242489A (en) | 2013-05-20 | 2013-05-20 | Preparation method of settling separation agent for red mud in aluminium ores |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101865875A CN103242489A (en) | 2013-05-20 | 2013-05-20 | Preparation method of settling separation agent for red mud in aluminium ores |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103242489A true CN103242489A (en) | 2013-08-14 |
Family
ID=48922389
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101865875A Pending CN103242489A (en) | 2013-05-20 | 2013-05-20 | Preparation method of settling separation agent for red mud in aluminium ores |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103242489A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199036A (en) * | 2015-10-13 | 2015-12-30 | 扬州大学 | Ammonium acrylate/acrylamide copolymerized emulsion flocculant and preparation method thereof |
| CN106632802A (en) * | 2016-12-09 | 2017-05-10 | 安徽天润化学工业股份有限公司 | Preparation method of aluminum ore red mud sedimentation flocculating agent |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220104A (en) * | 2007-12-07 | 2008-07-16 | 山东大学 | Preparation method for oxygen-containing nitrolic acid structure polyalcohol inphase opposition emulsions |
| CN101591415A (en) * | 2009-07-13 | 2009-12-02 | 湖北同一石油化工有限公司 | Iso-hydroxamic modified polyacrylamide and preparation method thereof |
| CN101735376A (en) * | 2009-12-13 | 2010-06-16 | 安徽省天润功能高分子工程研究有限公司 | Preparation method of red mud sinking agent |
| CN101747472A (en) * | 2008-12-15 | 2010-06-23 | 安徽省天润功能高分子工程研究有限公司 | Method for preparing high molecular weight instant cationic flocculant |
-
2013
- 2013-05-20 CN CN2013101865875A patent/CN103242489A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220104A (en) * | 2007-12-07 | 2008-07-16 | 山东大学 | Preparation method for oxygen-containing nitrolic acid structure polyalcohol inphase opposition emulsions |
| CN101747472A (en) * | 2008-12-15 | 2010-06-23 | 安徽省天润功能高分子工程研究有限公司 | Method for preparing high molecular weight instant cationic flocculant |
| CN101591415A (en) * | 2009-07-13 | 2009-12-02 | 湖北同一石油化工有限公司 | Iso-hydroxamic modified polyacrylamide and preparation method thereof |
| CN101735376A (en) * | 2009-12-13 | 2010-06-16 | 安徽省天润功能高分子工程研究有限公司 | Preparation method of red mud sinking agent |
Non-Patent Citations (1)
| Title |
|---|
| 方道斌等: "《丙烯酰胺聚合物》", 30 April 2006, 化学工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199036A (en) * | 2015-10-13 | 2015-12-30 | 扬州大学 | Ammonium acrylate/acrylamide copolymerized emulsion flocculant and preparation method thereof |
| CN106632802A (en) * | 2016-12-09 | 2017-05-10 | 安徽天润化学工业股份有限公司 | Preparation method of aluminum ore red mud sedimentation flocculating agent |
| CN106632802B (en) * | 2016-12-09 | 2019-03-05 | 安徽天润化学工业股份有限公司 | A kind of preparation method of aluminium ore flocculating agent for red mud precipitation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105254792B (en) | A kind of modified Cardanol derivative water reducer and preparation method thereof | |
| CN101704928B (en) | Preparation method of starch grafted acrylamide flocculating agent | |
| CN101613433B (en) | Method for synthesizing electrolyte-resistant thickener by using inverse emulsion | |
| FR2710342A1 (en) | Superabsorbent acrylic polymers with improved properties and process for obtaining them. | |
| CN103524757A (en) | Preparation method of hydroxamic acid modified polyacrylamide emulsion flocculant | |
| CN103242489A (en) | Preparation method of settling separation agent for red mud in aluminium ores | |
| CN102320699B (en) | Method for destabilization coagulating treatment of well drilling waste liquid | |
| JP4334279B2 (en) | Method for producing emulsion polymer | |
| CN103242471A (en) | Method for preparing non-ionic polyacrylamide emulsion and prepared emulsion | |
| CN102887806A (en) | One-pass charge for plain detonator | |
| CN102633921B (en) | Preparation method of aqueous emulsion type polyvinyl chloride resin non-toxic terminator | |
| CN104672377A (en) | Preparation method for high-solid-content cationic polyacrylamide inverse emulsion | |
| CN101323657B (en) | Preparing methods ofbutyl cyanide rubber emulsion and butyl cyanide rubber | |
| RU2489446C2 (en) | Method of separating emulsion polymerisation synthetic rubber from latex | |
| CN101293829A (en) | Method for preparing polydiallyl itaconate and dimer acid | |
| CN102219879B (en) | Method for producing polyacrylamide emulsion | |
| CN105419766A (en) | Technology method of synthesizing heavy oil sulfonate surfactant with sulfonation promoter | |
| RU2448121C1 (en) | Method of extracting synthetic rubber | |
| CN104497203B (en) | Preparation method of turbidity reducing agent | |
| CN1670048A (en) | Method for preparing carboxylated NBR latex | |
| CN106699936A (en) | Preparation method of sodium polyacrylate with high molecular weight | |
| RU2803745C1 (en) | Composition for latex stabilization and method for its production | |
| CN101570715A (en) | Oil and fat refining method and device thereof | |
| RU2516640C2 (en) | Method of obtaining filled butadiene styrene rubber | |
| CN105859946B (en) | A kind of preparation method of aluminum oxide flocculation agent reverse micro emulsion |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130814 |