CN1709935A - Preparation for starch grafted polyacrylamide and its derivative reversed-phase emulsion - Google Patents
Preparation for starch grafted polyacrylamide and its derivative reversed-phase emulsion Download PDFInfo
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- CN1709935A CN1709935A CN 200510013857 CN200510013857A CN1709935A CN 1709935 A CN1709935 A CN 1709935A CN 200510013857 CN200510013857 CN 200510013857 CN 200510013857 A CN200510013857 A CN 200510013857A CN 1709935 A CN1709935 A CN 1709935A
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Abstract
The invention discloses the preparation of a kind of starch grafting polyacrylamide (PAM) and its ramification, belonging to the preparation technology of water-soluble macromolecule materials. The method includes following process: add dehydrated sorbitol oleate, dehydrated sorbitol stearin and octylphenol polyoxyethylene ether (OPEO) into paraffin oil according to weight proportion, to prepare the continuous phase of emulsifier oil solution; mix starch and acrylamide (AM) or starch and AM and its ramification according to weight proportion, and dissolve them with water, to prepare the dispersed phase of solid shares of solution; add ammonium persulfate and urea, and add the dispersed phase into the continuous phase, then adjust pH by adding sodium hydroxide or ammonia; under nitrogen protection, mill to initiate polymerization at 5 - 30 Deg. C; then increase temperature to 45 - 60 Deg. C, react when keep the temperature; finally through hydrolyzing and purifying to prepare the inverse rubber latex of starch stem grafting polyacrylamide (PAM) and its ramification. The advantages of the invention are: the molecular structure of the prepared product has reasonable components, high and adjustable molecular weight; it's easy to operate, and has high conversion rate; the product has good dispersivity and high dissolving speed.
Description
Technical field
The present invention relates to the preparation method of a kind of starch grafted polyacrylamide and derivative thereof, belong to the technology of preparing of water-soluble high-molecular material.
Background technology
The polymkeric substance of starch graft acrylamide and derivative thereof is a class water-solubility function macromolecule product and since it have the molecular weight height, easily form hydrogen bond, can carry out number of chemical reaction, therefore all be applied in a lot of fields, develop extremely rapid.Product category is many, and the product of yin, yang, non-and four kinds of ion formulations of both sexes is arranged.Product mostly is 8～10% aqueous solution and pulvis.Water-sol product polymer content is low, use and store inconvenience; The powder product indissoluble, and need huge dissolution equipment.The present invention avoids above-mentioned the deficiencies in the prior art, is conceived to be improved on polymerisation process.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing inverse emulsion polymerization to prepare the method for instant type starch grafted polyacrylamide and derivant material thereof, use the starch grafted polyacrylamide of this method preparation and derivative inverse latex thereof to have the characteristics of solid content height, molecular weight height and narrowly distributing, instant and applied range.
The present invention is realized by following technical proposals, the preparation method of a kind of starch grafted polyacrylamide and derivative reversed-phase emulsion thereof, its characteristics are to comprise following process, selecting the volume ratio of disperse phase and external phase is 1/1～1.8, is in 6～9/4～6/1～2 adding paraffin oils with emulsifying agent sorbitan monooleate (span-80), Span60 (span-60), polyoxyethylene octylphenol ether (op-4) by mass ratio, be made into mass concentration and be 5～10% emulsifying agent oil solution (external phase), stirring and dissolving and logical N
2Reach 10-40min.Mixture with starch and acrylamide or starch and acrylamide and derivative thereof mixes and adds the gauge water dissolving by 10～40/20～40 or 10～40/15～30/5～10 quality proportioning in addition, be made into mass concentration and be solid part solution (disperse phase) of 40～60%, logical N
2After reaching 10-30min; it is 0.01～0.1% ammonium persulphate, 0.1～0.9% urea that adding accounts for monomer mass; hydro-oxidation sodium solution or ammonia soln are regulated pH value to 8～10, under nitrogen protection, stir and are warming up to 5～30 ℃ of initiated polymerizations; react and reached Wen Fenghou in 1～2 hour; insulation reaction 2～4 hours rises to temperature 45～60 ℃ again, insulation reaction 2～4 hours; again through hydrolysis, carry densely, promptly obtain starch grafted polyacrylamide and derivative inverse latex thereof.
Above-mentioned acrylamide derivative is vinylformic acid and (methyl) acrylyl oxy-ethyl-trimethyl salmiac.
The invention has the advantages that: products molecule structure that (1) makes is formed rationally, molecular weight is high and can adjust according to service orientation; (2) adopt combined oxidation-reduction initiating system, reaction activity is low, and reaction is easy to carry out, reacting balance, safety, transformation efficiency height, and residual monomer content is low; (3) production technique is simple, and the reaction conditions gentleness, energy consumption is low and the three-waste free pollution problem; (4) good product dispersibility, dissolution rate is fast, and is less than 5min, easy to use.
Embodiment
Embodiment 1
In having the 1000ml four-hole bottle of agitator, temperature regulator, reflux exchanger, add the 300g paraffin oil earlier, add span-80 10g, span-60 7g, op-4 2g again, stirring and dissolving and logical N
220min; Take by weighing starch 65g and acrylamide 50 in addition, add 140g water stirring and dissolving after the mixing, logical N
2Behind the 10min; add ammonium persulphate 0.15g, urea 0.3g, mix the back and add in the oil phase, add ammonia soln under the whipped state and regulate pH value to 8.5; under nitrogen protection; stirring is warming up to 10 ℃ of initiated polymerizations, reacts to reach Wen Fenghou, insulation reaction 2 hours in 1 hour; temperature is risen to 60 ℃ again; insulation reaction 4 hours, again through hydrolysis, carry densely, promptly obtain anionic starch grafted polyacrylamide inverse latex.This product is the thick latex of oyster white, and molecular weight is 400-700 ten thousand, solid content 〉=30%, and dissolution rate≤5min is as the mud conditioner in oil field and the water conditioner in the environment-protecting industrial.
Embodiment 2
In having the 1000ml four-hole bottle of agitator, temperature regulator, reflux exchanger, add the 300g paraffin oil earlier, add span-80 12g, span-60 8g, op-4 3g again, stirring and dissolving and logical N
220min; Take by weighing starch 65g and acrylamide 45 and vinylformic acid 10g in addition, add 150g water stirring and dissolving after the mixing, and regulate pH value to 8.5, logical N with aqueous sodium hydroxide solution
2Behind the 10min; add ammonium persulphate 0.15g, urea 0.3g; mix the back and add in the oil phase, under nitrogen protection, stir and be warming up to 10 ℃ of initiated polymerizations; react and reached Wen Fenghou in 1 hour; insulation reaction 2 hours rises to temperature 60 ℃ again, insulation reaction 4 hours; again through hydrolysis, carry densely, promptly obtain anionic starch grafted polyacrylamide inverse latex.This product is the thick latex of oyster white, and molecular weight is 400-700 ten thousand, solid content 〉=30%, and dissolution rate≤5min is as the mud conditioner in oil field and the water conditioner in the environment-protecting industrial.
Embodiment 3
In having the 1000ml four-hole bottle of agitator, temperature regulator, reflux exchanger, add the 300g paraffin oil earlier, add span-80 12g, span-60 8g, op-4 2g again, stirring and dissolving and logical N
220min; Take by weighing starch 60g and acrylamide 50 and (methyl) acrylyl oxy-ethyl-trimethyl salmiac 10g in addition, add 143g water stirring and dissolving after the mixing, and regulate pH value to 9.0, logical N with aqueous sodium hydroxide solution
2Behind the 10min; add ammonium persulphate 0.15g, urea 0.3g; mix the back and add in the oil phase, under nitrogen protection, stir and be warming up to 18 ℃ of initiated polymerizations; react and reached Wen Fenghou in 1.5 hours; insulation reaction 2 hours rises to temperature 60 ℃ again, insulation reaction 4 hours; again through hydrolysis, carry densely, promptly obtain cationic starch grafted polyacrylamide inverse latex.This product is the thick latex of oyster white, and molecular weight is 300-600 ten thousand, solid content 〉=30%, and dissolution rate≤5min is as paper retention and filter aid.
Claims (2)
1. the preparation method of starch grafted polyacrylamide and derivative reversed-phase emulsion thereof, its characteristics are to comprise following process: selecting the volume ratio of disperse phase and external phase is 1/1～1.8, is in 6～9/4～6/1～2 adding paraffin oils with emulsifying agent sorbitan monooleate, Span60, polyoxyethylene octylphenol ether by mass ratio, be made into mass concentration and be the external phase of 5～10% emulsifying agent oil solution, stirring and dissolving and logical N
2Reach 10-40min, in addition the mixture of starch and acrylamide or starch and acrylamide and derivative thereof is mixed by 10～40/20～40 quality proportioning and be dissolved in water, be made into mass concentration and be the disperse phase of solid part solution of 40～60%, logical N
2After reaching 10-30min; it is 0.01～0.1% ammonium persulphate, 0.1～0.9% urea that adding accounts for monomer mass; hydro-oxidation sodium solution or ammonia soln are regulated pH value to 8～10, under nitrogen protection, stir and are warming up to 5～30 ℃ of initiated polymerizations; react and reached Wen Fenghou in 1～2 hour; insulation reaction 2～4 hours rises to temperature 45～60 ℃ again, insulation reaction 2～4 hours; again through hydrolysis, carry densely, promptly obtain starch grafted polyacrylamide and derivative inverse latex thereof.
2. by the preparation method of described starch grafted polyacrylamide of claim 1 and derivative reversed-phase emulsion thereof, its characteristics are: acrylamide derivative is vinylformic acid and (methyl) acrylyl oxy-ethyl-trimethyl salmiac.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510013857 CN1709935A (en) | 2005-06-17 | 2005-06-17 | Preparation for starch grafted polyacrylamide and its derivative reversed-phase emulsion |
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| CN 200510013857 CN1709935A (en) | 2005-06-17 | 2005-06-17 | Preparation for starch grafted polyacrylamide and its derivative reversed-phase emulsion |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113524A (en) * | 2013-02-16 | 2013-05-22 | 中国石油化工股份有限公司 | Preparation method of starch grafted copolymer inverse emulsion for drilling fluid |
| CN104470975A (en) * | 2012-03-02 | 2015-03-25 | 多伦多大学董事局 | Polymeric nanoparticles useful in theranostics |
| CN106543364A (en) * | 2015-09-18 | 2017-03-29 | 上海东升新材料有限公司 | A kind of method for preparing acrylamide graft guar gum and its application |
-
2005
- 2005-06-17 CN CN 200510013857 patent/CN1709935A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104470975A (en) * | 2012-03-02 | 2015-03-25 | 多伦多大学董事局 | Polymeric nanoparticles useful in theranostics |
| CN104470975B (en) * | 2012-03-02 | 2018-02-27 | 多伦多大学董事局 | Polymer/nanoparticle available for treatment diagnostics |
| CN103113524A (en) * | 2013-02-16 | 2013-05-22 | 中国石油化工股份有限公司 | Preparation method of starch grafted copolymer inverse emulsion for drilling fluid |
| CN106543364A (en) * | 2015-09-18 | 2017-03-29 | 上海东升新材料有限公司 | A kind of method for preparing acrylamide graft guar gum and its application |
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