CN106008802A - Preparation technology of cationic polyacrylamide water-in-oil emulsion - Google Patents
Preparation technology of cationic polyacrylamide water-in-oil emulsion Download PDFInfo
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- CN106008802A CN106008802A CN201610441065.9A CN201610441065A CN106008802A CN 106008802 A CN106008802 A CN 106008802A CN 201610441065 A CN201610441065 A CN 201610441065A CN 106008802 A CN106008802 A CN 106008802A
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- oil emulsion
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/32—Polymerisation in water-in-oil emulsions
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides a preparation technology of cationic polyacrylamide water-in-oil emulsion. The preparation technology comprises the steps that 1, an oil-soluble emulsifying agent is dissolved in oil, and an oil phase is prepared; 2, a water-soluble polymer emulsifying agent, a water-soluble cationic emulsifying agent, acrylamide, water-soluble cationic monomers, a metal ion capturing agent and deionized water are prepared into a water phase together, and the pH value is regulated to be 2 to 3; 3, the water phase is gradually added into the oil phase while stirring is conducted, stirring and emulsifying are continuously conducted, and water-in-oil emulsion is generated; 4, after nitrogen is introduced to remove oxygen, the temperature of the water-in-oil emulsion generated in the step 3 is controlled to be 10 DEG C to 90 DEG C, polymerization is initiated by adding an initiating agent, and then the water-in-oil cationic polyacrylamide emulsion is obtained. The cationic polyacrylamide water-in-oil emulsion can be used for urban domestic sewage treatment, and is especially suitable for flocculating settling of organic suspended solids in acid or weak acid sewage.
Description
Technical field
The present invention relates to water-in-oil emulsion.
Background technology
Polyacrylamide series products mainly has four kinds of forms in the market: aqueous solution, aqueous dispersions product, water in oil emulsion liquid product and solid product.Due to polyacrylamide molecular weight product generally more than million orders of magnitude, its aqueous solution often has very high viscosity, and therefore its aqueous solution or aqueous dispersions product are difficult to use with high molecular, high effective content form, and be seldom used as flocculant or oil displacement agent.Solid polypropylene amide products is a kind of product form that consumption is maximum in the market, this series products is typically by pulverizing after polymerisation in solution or using Inverse suspension copolymerization method to prepare, during polymerization, reaction monomers effective content is usually 25～35 weight %, and molecular weight of product is higher.But, solid product needs to remove large quantity of moisture in preparation process, and energy consumption is the highest, and in use there is the problem dissolving difficulty.Water-in-oil emulsion (reversed-phase emulsion) product is the series products establishing one's own system, showing unique characteristics, in preparation process reaction monomers effective content up to 40 weight % more than, wherein in aqueous phase reaction monomers concentration up to 60 weight %, super high molecular weight product can be prepared simultaneously, apply excellent effect.Water in oil emulsion liquid product is the most rapidly dissolvable by phase reversal effect during using, and substantially increases the motility in application process.Compared with solid product, water in oil emulsion liquid product still suffers from the deficiency that preparation cost is higher, but its high comprehensive performance, in a lot of application scenarios, there is higher cost performance.
Along with improving constantly of people's living standard; environmental conservation has become people's question of common concern; industrial wastewater particularly discharge to coking water is the important polluter causing environmental pollution; and country also takes compulsive measures; to the coking producer not meeting discharge standard; take pass, stop, the compulsory measure such as turn, be thus badly in need of a kind of effective coking water inorganic agent.At present for coke-oven plant's sewage water treatment method of municipal sewage particularly Cities with Coal Mines, commonly used ferrous chloride or aluminum sulfate liquid process, by domestic and international related data is retrieved coking water processing method, the most frequently used ferrous sulfate or polyaluminium chloride liquid process, above-mentioned inorganic agent treatment effect is poor, some leading indicators, such as color degree, chemical oxygen consumption (COC) (COD), the removal rate of float (SS) is relatively low, it is extremely difficult to the discharge standard of regulation, additionally the consumption of these inorganic agents is the biggest, easily produce more reluctant residue, easily cause secondary pollution.
Application publication number CN102304498A discloses a kind of method preparing cross-linked enzyme aggregate in water-in-oil emulsion, enzymatic solution is prepared including (1), (2) in enzymatic solution, addition can make the precipitant of enzyme aggregate and precipitate, the preparation dispersion phase containing enzyme, (3) dispersion phase containing enzyme is scattered in hydrophobic liquid, forming water-in-oil emulsion, (4) reclaim the steps such as the cross-linked enzyme aggregate of formation with the enzyme aggregate in cross-linking agents water-in-oil emulsion and (5).Cross-linked enzyme aggregate prepared by the inventive method is Immobilized Enzymes Without Carriers, and unit enzyme is lived high, can be used in corresponding enzymic catalytic reaction.But this water-in-oil emulsion does not have decontamination.
Summary of the invention
The shortcoming of prior art in view of the above, the present invention provides the preparation technology of a kind of PAMC water-in-oil emulsion.City domestic sewage can be used for process, be particularly well-suited to the flocculating sedimentation of the organic suspended matter of acidity or slant acidity sewage.
For achieving the above object and other relevant purposes, the present invention provides the preparation technology of a kind of PAMC water-in-oil emulsion, the steps include:
The first step, is dissolved in oil by oil soluble emulsifying agent and makes oil phase；
Second step, is together configured to water soluble polymer emulsifying agent, water-soluble cationic emulsifying agent, acrylamide, water-soluble cationic monomer and metal ion capturing agent and deionized water aqueous phase and to regulate pH value is 2-3；
3rd step, is gradually added into aqueous phase in oil phase while stirring, and continuously stirred emulsifying forms water in oil emulsion；
4th step, after logical nitrogen deoxygenation, the water in oil emulsion temperature control the 3rd step formed, to 10-90 DEG C, adds initiator and causes polymerization, obtain water-in-oil type cation polyacrylamide emulsion.
Preferably, one or more in polyvinyl alcohol, Polyethylene Glycol, vinyl pyrrolidone polymer of described water soluble polymer emulsifying agent.
Preferably, the molecular weight of described polyvinyl alcohol is 6000-120000, and degree of hydrolysis is 80-100%.
Preferably, adding enzymatic solution in the third step, described enzymatic solution is trehalose synthase solution.
Preferably, the mixing speed in the 4th step is 60-100r/min, and mixing time is 15-20r/min.
As mentioned above, a kind of preparation technology of the PAMC water-in-oil emulsion of the present invention, have the advantages that this preparation technology is simple, application process is scientific and reasonable, effective for processing coked waste water, it is possible not only to reach emission request, it is possible to become to purify water by sewage disposal, reuse doing recirculated water, saved and used water.Cation polypropylene amine water-in-oil emulsion is mainly used in city domestic sewage and processes, the Industrial Waste Water Treatments such as brewery, starch factory, food processing factory, it is particularly well-suited to the flocculating sedimentation of the organic dangerous thing of acidity or slant acidity sewage, degreaser is can be used in disposing polluted water in oil, in paper industry, it is used for making retention aid and filter, and the process of papermaking wastewater.
Detailed description of the invention
By particular specific embodiment, embodiments of the present invention being described below, those skilled in the art can be understood other advantages and effect of the present invention easily by the content disclosed by this specification.
The preparation technology of a kind of PAMC water-in-oil emulsion, the steps include:
The first step, is dissolved in oil by oil soluble emulsifying agent and makes oil phase；
Second step, is together configured to water soluble polymer emulsifying agent, water-soluble cationic emulsifying agent, acrylamide, water-soluble cationic monomer and metal ion capturing agent and deionized water aqueous phase and to regulate pH value is 2-3；
3rd step, is gradually added into aqueous phase in oil phase while stirring, and continuously stirred emulsifying forms water in oil emulsion；
4th step, after logical nitrogen deoxygenation, the water in oil emulsion temperature control the 3rd step formed, to 10-90 DEG C, adds initiator and causes polymerization, obtain water-in-oil type cation polyacrylamide emulsion.
Preferably, one or more in polyvinyl alcohol, Polyethylene Glycol, vinyl pyrrolidone polymer of described water soluble polymer emulsifying agent.
Preferably, the molecular weight of described polyvinyl alcohol is 6000-120000, and degree of hydrolysis is 80-100%.
Preferably, adding enzymatic solution in the third step, described enzymatic solution is trehalose synthase solution.
Preferably, the mixing speed in the 4th step is 60-100r/min, and mixing time is 15-20r/min.
Using method: load appropriate water in dissolving tank, opens stirring, and rotating speed reaches more than 80r/min, and emulsion is slowly injected in water, after emulsion all adds, stirs 15-20min.If using the devices such as high speed agitator, static mixer, Venturi tube to help emulsion to dissolve, emulsion can be fully contacted dispersion with water, and solute effect is more preferable, dissolution time 3-15min.
The one-level breakdown of emulsion processing method of oil-containing≤100mg/L in pending oil-polluted water: 1, first by oil-polluted water through Air Exposure, remove the oil of free state, floccule and granule, acquirement processes water A1.2, process water A1 is passed through Venturi tube, control the oil-polluted water pressure of venturi throat less than the vapour pressure of processing environment water saturation at that time, using lipophilic material to adsorb free state oil molecule again, make oil molecule assemble and form separation removal after oil droplet, acquirement processes water A2.
In sum, the present invention provides the preparation technology of a kind of PAMC water-in-oil emulsion, this preparation technology is simple, application process is scientific and reasonable, effective for processing coked waste water, it is possible not only to reach emission request, it is possible to become to purify water by sewage disposal, reuse doing recirculated water, saved and used water.Cation polypropylene amine water-in-oil emulsion is mainly used in city domestic sewage and processes, the Industrial Waste Water Treatments such as brewery, starch factory, food processing factory, it is particularly well-suited to the flocculating sedimentation of the organic dangerous thing of acidity or slant acidity sewage, degreaser is can be used in disposing polluted water in oil, in paper industry, it is used for making retention aid and filter, and the process of papermaking wastewater.So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by any person skilled in the art.Therefore, art has all equivalence modification or changes that usually intellectual is completed under without departing from disclosed spirit and technological thought such as, must be contained by the claim of the present invention.
Claims (5)
1. the preparation technology of a PAMC water-in-oil emulsion, it is characterised in that: the steps include:
The first step, is dissolved in oil by oil soluble emulsifying agent and makes oil phase；
Second step, is together configured to water soluble polymer emulsifying agent, water-soluble cationic emulsifying agent, acrylamide, water-soluble cationic monomer and metal ion capturing agent and deionized water aqueous phase and to regulate pH value is 2-3；
3rd step, is gradually added into aqueous phase in oil phase while stirring, and continuously stirred emulsifying forms water in oil emulsion；
4th step, after logical nitrogen deoxygenation, the water in oil emulsion temperature control the 3rd step formed, to 10-90 DEG C, adds initiator and causes polymerization, obtain water-in-oil type cation polyacrylamide emulsion.
The preparation technology of a kind of PAMC water-in-oil emulsion the most according to claim 1, it is characterised in that: one or more in polyvinyl alcohol, Polyethylene Glycol, vinyl pyrrolidone polymer of described water soluble polymer emulsifying agent.
The preparation technology of a kind of PAMC water-in-oil emulsion the most according to claim 1 and 2, it is characterised in that: the molecular weight of described polyvinyl alcohol is 6000-120000, and degree of hydrolysis is 80-100%.
The preparation technology of a kind of PAMC water-in-oil emulsion the most according to claim 2, it is characterised in that: adding enzymatic solution in the third step, described enzymatic solution is trehalose synthase solution.
The preparation technology of a kind of PAMC water-in-oil emulsion the most according to claim 4, it is characterised in that: the mixing speed in the 4th step is 60-100r/min, and mixing time is 15-20r/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610441065.9A CN106008802A (en) | 2016-06-20 | 2016-06-20 | Preparation technology of cationic polyacrylamide water-in-oil emulsion |
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| CN201610441065.9A CN106008802A (en) | 2016-06-20 | 2016-06-20 | Preparation technology of cationic polyacrylamide water-in-oil emulsion |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866250A (en) * | 2017-03-10 | 2017-06-20 | 江苏大唐博创再生资源开发有限公司 | A kind of method that controlled-release urea fertilizer is prepared by water-in-oil microemulsion method |
| CN111848862A (en) * | 2020-06-24 | 2020-10-30 | 爱森（中国）絮凝剂有限公司 | Preparation method of cation inverse emulsion based on high-activity emulsifier |
| WO2020257978A1 (en) * | 2019-06-24 | 2020-12-30 | Kemira Oyj | Polymeric structure and its uses |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037492A (en) * | 2007-03-28 | 2007-09-19 | 中国石油大学(华东) | Method for preparing propylene amides copolymer with regular branch structure by inverse emulsion method |
| CN101298488A (en) * | 2008-06-25 | 2008-11-05 | 山东大学 | Preparation of cationic polyacrylamide reverse microemulsion |
| CN101628953A (en) * | 2009-08-11 | 2010-01-20 | 华南师范大学 | High molecular weight cationic polyacrylamide preparation method |
| CN102206301A (en) * | 2010-03-29 | 2011-10-05 | 苏州瑞普工业助剂有限公司 | Preparation method of rapid dissolved cationic polyacrylamide emulsion of water in oil type |
| CN102304498A (en) * | 2011-09-08 | 2012-01-04 | 天津市林业果树研究所 | Cross-linked enzyme aggregate prepared in water-in-oil emulsion and preparation method thereof |
-
2016
- 2016-06-20 CN CN201610441065.9A patent/CN106008802A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037492A (en) * | 2007-03-28 | 2007-09-19 | 中国石油大学(华东) | Method for preparing propylene amides copolymer with regular branch structure by inverse emulsion method |
| CN101298488A (en) * | 2008-06-25 | 2008-11-05 | 山东大学 | Preparation of cationic polyacrylamide reverse microemulsion |
| CN101628953A (en) * | 2009-08-11 | 2010-01-20 | 华南师范大学 | High molecular weight cationic polyacrylamide preparation method |
| CN102206301A (en) * | 2010-03-29 | 2011-10-05 | 苏州瑞普工业助剂有限公司 | Preparation method of rapid dissolved cationic polyacrylamide emulsion of water in oil type |
| CN102304498A (en) * | 2011-09-08 | 2012-01-04 | 天津市林业果树研究所 | Cross-linked enzyme aggregate prepared in water-in-oil emulsion and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866250A (en) * | 2017-03-10 | 2017-06-20 | 江苏大唐博创再生资源开发有限公司 | A kind of method that controlled-release urea fertilizer is prepared by water-in-oil microemulsion method |
| WO2020257978A1 (en) * | 2019-06-24 | 2020-12-30 | Kemira Oyj | Polymeric structure and its uses |
| CN114072436A (en) * | 2019-06-24 | 2022-02-18 | 凯米拉公司 | Polymeric structures and uses thereof |
| CN114072436B (en) * | 2019-06-24 | 2023-12-08 | 凯米拉公司 | Polymeric structure and use thereof |
| CN111848862A (en) * | 2020-06-24 | 2020-10-30 | 爱森（中国）絮凝剂有限公司 | Preparation method of cation inverse emulsion based on high-activity emulsifier |
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