CN103509154B - Preparation method of zwitterionic polyacrylamide - Google Patents
Preparation method of zwitterionic polyacrylamide Download PDFInfo
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- CN103509154B CN103509154B CN201210216409.8A CN201210216409A CN103509154B CN 103509154 B CN103509154 B CN 103509154B CN 201210216409 A CN201210216409 A CN 201210216409A CN 103509154 B CN103509154 B CN 103509154B
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Abstract
The invention relates to a preparation method of zwitterionic polyacrylamide, and belongs to the field of high-molecular polymerization. The preparation method is characterized by comprising the following steps of: charging, namely adding deionized water into a polymerization reactor, and adding a 30wt% acrylamide water solution, a cationic monomer, an anionic monomer, a cosolvent and a chain transfer agent while stirring, and regulating the pH value of the system by use of alkali; introducing nitrogen for deoxygenization, and then, adding an initiator; performing adiabatic polymerization reaction, namely controlling the initiation temperature to be 2-25 DEG C, after 2-6 hours, terminating the reaction when the polymerization system temperature rises no longer, thereby obtaining the polymer gel; granulating, baking, smashing and sieving the gel to obtain zwitterionic polyacrylamide products with high intrinsic viscosity. The invention provides a preparation method of zwitterionic polyacrylamide with high intrinsic viscosity, and in the preparation method, azo initiator initiates a polymerization technology at a lower temperature, the operation technology is simple, and the intrinsic viscosity of the prepared product is not less than 2000ml/g.
Description
Technical field
The present invention relates to a kind of preparation method of amphoteric ionic polyacrylamide, belong to field of macromolecule polymerization.
Background technology
Amphoteric ionic polyacrylamide is anti-in sewage disposal, solid-liquid separation, drilling well as water soluble polymer product
Collapse filtrate reducing, is used widely in the industry such as the polymer displacement of reservoir oil of oil recovery industry, papermaking, weaving, printing and dyeing, coal washing.Especially exist
As in the sewage disposal of flocculant, because its suitable acidity value is wider, more preferable than PAMC effect.Oil
In exploitation, particularly tertiary phase, it is more complicated that high intrinsic viscosity amphoteric ionic polyacrylamide is used for oil reservoir situation
High salinity, hot environment, can obtain obvious temperature-resistant anti-salt effect.In paper industry, add amphion polyacrylamide
After amine, neutral high-quality paper of can manufacturing paper with pulp out.Preparation technology of the prior art also difficult to reach intrinsic viscosity >=
2300ml/g technical specification.
At present, the preparation method of amphoteric ionic polyacrylamide is mainly using the following two kinds method:
The first is two-step method, first by acrylamide homopolymerization, prepared non-ionic polyacrylamide, and then again that this is non-
Cationic polyacrylamide is modified, such as Mannich reaction and sulfomethylation, finally gives amphoteric ionic polyacrylamide
Dilute aqueous solution.Not only intrinsic viscosity is low for amphoteric ionic polyacrylamide acquired in the method, is usually no more than 2000ml/g,
And final products are 1%～5% weak solution, storage time is short, both increases difficulty to the transport and storage of this product.
Second method is ternary or the one-step method of multi-component copolymer.To in acrylamide aqueous solution, add one or more
Cationic monomer, anionic monomer and various auxiliary agent, with acid, alkali adjustment ph value to after predetermined value, letting nitrogen in and deoxidizing, add compound drawing
Send out agent polymerization, prepared amphoteric ionic polyacrylamide.In this composite initiation system, usually redox initiator is carried out
Initial stage low temperature causes, although the method is simple, cannot overcome that redox initiator brings due to initiator wear rate
Too soon, the drawbacks of monomer conversion reduces, and reducing agent easily participates in chain transfer reaction.Thus leading to polymer intrinsic viscosity to drop
Low it is difficult to obtain the product of high intrinsic viscosity.
A kind of initiator system preparing amphion polyacrylamide is disclosed in Chinese patent cn 1061013c, it
Purpose be to prepare a kind of efficient flocculant, its using effect has larger floccule body than the current cationic flocculant using
Diameter and relatively low filter cake moisture content.This initiator system is made up of chelating agen, oxidant, reducing agent and azo initiator, gathers
Close temperature at 25 DEG C～60 DEG C, belong to middle temperature polymerizations.
Chinese patent cn101514239 adopts aqueous dispersion polymerization method, with water as reaction medium, does not use organic solvent
And surfactant, decrease the pollution to environment, obtained product is that high molecular reactive component is uniform in aqueous phase, stable
Scattered liquid, solid content 20～30% is it is easy to preparing and using.In its polymerization technique, Deca feeds at twice, and initiator is
Persulfate, 50～80 DEG C of polymerization temperature, the weight average molecular weight of polymer is 5,000,000～18,000,000.
Content of the invention
According to the deficiencies in the prior art, the technical problem to be solved in the present invention is: provides a kind of amphoteric ion type polypropylene
The preparation method of amide, stable polymerization reaction, efficiency of initiation is high, and the polymer intrinsic viscosity of acquisition is high, in terms of products application,
The suitable ph value scope of sewage disposal is more wider than cationic polymer, and oil extraction in oil field is suitable for high temperature, high salinity media.
The technical solution adopted for the present invention to solve the technical problems is: provides a kind of amphoteric ionic polyacrylamide
Preparation method is it is characterised in that comprise the following steps:
(1) feed intake: deionized water is put in polymer reactor, under agitation, once puts into raw materials quality fraction
Acrylamide aqueous solution for 30%, cationic monomer, anionic monomer, cosolvent, chain-transferring agent, with alkali come regulation system
Ph value；Initiator is added after logical nitrogen deoxygenation；
(2) adiabatic polymerisation reaction: initiation temperature controls for 2～25 DEG C, and 2 ~ 6h post polymerization system temperature no longer raises i.e.
Terminate for reaction, obtain polymeric colloid；
(3) by granulating from colloid, drying, pulverizing, screening, obtain high intrinsic viscosity amphoteric ionic polyacrylamide product.
The addition of wherein ionized water is formula ratio.
The present invention can obtain the high intrinsic viscosity amphoteric ionic polyacrylamide product of intrinsic viscosity >=2000ml/g.
Heretofore described intrinsic viscosity adopts viscosimetry to measure, and measures intrinsic viscosity according to gb12005.1-89.
The high intrinsic viscosity amphoteric ionic polyacrylamide dissolubility of present invention preparation is preferable, the copolymerization process being adopted
Simple and practical, easy to operate it is easy to large-scale industrial production.
Initiator described in step (1) is water-soluble azo initiator, and described water-soluble azo initiator is azo two
Isopropyl cyanide, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-isobutyrate hydrochloride, azo diisopropylamidinateand quinoline hydrochlorate, azo two 2,2-Dimethylaziridine
One or more of quinoline hydrochlorate or azo two isocyano group valeric acid, its consumption be starting monomer quality 0.005%～
0.075%.
Cationic monomer described in step (1) is acrylyl oxy-ethyl-trimethyl salmiac, methylacryoyloxyethyl
One or more of trimethyl ammonium chloride or dimethyl diallyl ammonium chloride, its addition accounts for starting monomer gross mass
10%～60%.
Anionic monomer described in step (1) is in 2- acrylamido 2- methyl propane sulfonic acid, acrylic acid or sodium acrylate
One or more, its addition accounts for the 1%～30% of starting monomer gross mass.
Cosolvent described in step (1) is carbamide, and its addition accounts for the 0.1%～5% of starting monomer gross mass.
Chain-transferring agent described in step (1) is that in sodium formate, β-dimethylamino butyronitrile or isopropanol, its addition accounts for raw material
The 0.01%～0.07% of monomer gross mass.
Alkali described in step (1) is sodium hydroxide, and for adjusting ph value, its addition is adjusted with ph value and to 4～8 is
Accurate；
Polymerization technology condition described in step (2) is as follows:
Initiation temperature DEG C 2～25
It is passed through nitrogen amount m3/m360~80
Baking temperature DEG C 40～80
Wherein it is passed through the volume that nitrogen amount refers to the nitrogen that every cubic metre of polymeric solution is passed through.
Preferably 5 ~ 20 DEG C of initiation temperature described in step (2).
The invention has the beneficial effects as follows:
1st, a kind of azo initiator is provided to cause polymerization technique at low temperature, operating procedure is simple, prepared product attribute glues
The preparation method of the high intrinsic viscosity amphoteric ionic polyacrylamide of number >=2000ml/g.
2nd, the anti-collapse and filtrate reducing be applied to sewage disposal, solid-liquid separation, oil drilling, tertiary oil production in oil field high temperature
The polymer displacement of reservoir oil of high salt, and the industry such as papermaking, weaving, printing and dyeing.
Specific embodiment
With reference to embodiment, the present invention is described further:
Embodiment 1
56g deionized water is added in aggregation container, sequentially adds the acrylamide of 133g30% under agitation,
The acrylyl oxy-ethyl-trimethyl salmiac (dac) of 6.25g80%, 5g 2- acrylamido 2- methyl propane sulfonic acid (amps), 1g
Carbamide, 0.015g sodium formate, the ph value adjusting system with naoh is 6.5, adjusts system initiation temperature to 10 DEG C, in nitrogen simultaneously
After being passed through 15min under flow 4l/min, add the initiator azo two 2,2-Dimethylaziridine hydrochloric acid through the pretreatment in 10 minutes of 50 DEG C of constant temperature
Salt 0.005g, about mistake 3min polymerization system start polymerization tacky, intensification, and 2 ~ 6h post polymerization system temperature reaches 70 DEG C, then
System temperature begins to decline, continue to keep should at a temperature of 2h, then the colloid obtaining is carried out pelletize, dries material at 50 DEG C
Dry, pulverizing obtains the amphoteric ionic polyacrylamide dry powder of intrinsic viscosity 2376ml/g.Other several important technology indexs are:
Solid content (testing standard gb12005.2-89) 88.63%
Dissolution velocity (testing standard gb12005.8-89) 40min
Residual monomer content (testing standard gb/t 22312-2008) 0.035%
(testing standard is similarly hereinafter)
Embodiment 2
According to the method and steps of embodiment 1, difference is that the initial temperature of embodiment 2 is 5 DEG C, gained amphoteric ion type
Each technical specification of polyacrylamide dry powder is as follows:
Embodiment 3
According to the method and steps of embodiment 1, difference is that the initial temperature of embodiment 3 is 20 DEG C, gained amphion
Each technical specification of type polyacrylamide dry powder is as follows:
Embodiment 4
56g deionized water is added in aggregation container, sequentially adds the acrylamide of 133g30% under agitation,
The MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (dmc) of 6.25g80%, 5g acrylic acid, 1g carbamide, 0.015g sodium formate, use
The ph value that naoh adjusts system is 6.5, adjusts system initiation temperature to 20 DEG C simultaneously, is passed through under nitrogen flow 4l/min
After 15min, the initiator azo-bis-isobutyrate hydrochloride 0.045g through the pretreatment in 5 minutes of 60 DEG C of constant temperature, about mistake 3min is added to gather
Fit system starts polymerization tacky, intensification, and 2 ~ 6h post polymerization system temperature reaches 70 DEG C, and then system temperature begins to decline, and continues
2h at a temperature of this is held in continuation of insurance, then carries out pelletize, drying materials, pulverizing is obtained amphoteric ion type at 50 DEG C the colloid obtaining
Polyacrylamide dry powder, each technical specification is as follows:
Embodiment 5
560g deionized water is added in aggregation container, sequentially adds the acrylamide of 1333g30% under agitation,
The dac of 62.5g80%, 50gamps, 10g carbamide, 0.15g sodium formate, the ph value adjusting system with naoh is 6.5, is passed through nitrogen
To remove the dissolved oxygen in reaction system, adjust system initiation temperature to 10 DEG C simultaneously, add through 60 DEG C of perseverances after logical nitrogen 15min
The initiator azo-bis-isobutyrate hydrochloride 0.10g of warm pretreatment in 10 minutes, about cross 3min polymerization system start polymerization and tacky,
Heat up, 2h～6h post polymerization system temperature reaches 70 DEG C, and then system temperature begins to decline, 2h at a temperature of continuing to keep being somebody's turn to do, so
Afterwards by the colloid obtaining carry out pelletize, at 50 DEG C by drying materials, pulverize and obtain amphoteric ionic polyacrylamide dry powder.Its skill
Art index is:
Embodiment 6
According to the method and steps of embodiment 5, difference is that the initial temperature of embodiment 6 is 20 DEG C, gained amphion
Each technical specification of type polyacrylamide dry powder is as follows
Embodiment 7
879.5g deionized water is added in aggregation container, sequentially adds the acrylamide of 833g30% under agitation,
The dac of 187.5g80%, 100gamps, 10g carbamide, 0.15g sodium formate, the ph value adjusting system with naoh is 6.0, is passed through nitrogen
Gas, to remove the dissolved oxygen in reaction system, adjusts system initiation temperature to 15 DEG C simultaneously, add through 50 DEG C after logical nitrogen 15min
It is concurrent that the initiator azo-bis-isobutyrate hydrochloride 0.10g of constant temperature pretreatment in 10 minutes, about mistake 3min polymerization system start polymerization
Viscous, intensification, 2h～6h post polymerization system temperature reaches 70 DEG C, and then system temperature begins to decline, 2h at a temperature of continuing to keep being somebody's turn to do,
Then by the colloid obtaining carry out pelletize, at 50 DEG C by drying materials, pulverize and obtain amphoteric ionic polyacrylamide dry powder.
Its technical specification is:
Embodiment 8
According to the method and steps of embodiment 7, difference is that embodiment 8 colloid drying temperature is 60 DEG C, gained both sexes from
Each technical specification of subtype polyacrylamide dry powder is as follows
Comparative example 1
560g deionized water is added in aggregation container, sequentially adds the acrylamide of 1333g30% under agitation,
The dac of 62.5g80%, 50gamps, 10g carbamide, 0.15g sodium formate, the ph value adjusting system with naoh is 6.5, is passed through nitrogen
To remove the dissolved oxygen in reaction system, adjust system initiation temperature to 30 DEG C simultaneously, add initiator mistake after logical nitrogen 15min
Ammonium sulfate 0.1g, sodium sulfite 0.1g, not pretreated initiator azo-bis-isobutyrate hydrochloride 0.05g, about 2min excessively
Polymerization system starts polymerization tacky, intensification, and 1h post polymerization system temperature reaches 70 DEG C, and then system temperature begins to decline, and continues
Continuation of insurance hold 3h at a temperature of this, then by the colloid obtaining carry out pelletize, drying, pulverizing obtain amphoteric ionic polyacrylamide
Dry powder.
Its technical specification is:
Comparative example 2
According to the method and steps of comparative example 1, difference is that the initial polymerization temperature of comparative example 2 is 40 DEG C, gained both sexes
Each technical specification of Polyacrylamide dry powder is as follows
Comparative example 3
560g deionized water is added in aggregation container, sequentially adds the acrylamide of 1333g30% under agitation,
The dac of 62.5g80%, 50gamps, 10g carbamide, 0.15g sodium formate, the ph value adjusting system with naoh is 6.5, is passed through nitrogen
To remove the dissolved oxygen in reaction system, adjust system initiation temperature to 20 DEG C simultaneously, add not preprocessed after logical nitrogen 15min
Initiator azo-bis-isobutyrate hydrochloride 0.10g, result polymerization is slow, and is polymerized not exclusively, and clear liquid about 30% is it is impossible to survey
Try each technical specification.
Claims (6)
1. a kind of preparation method of amphoteric ionic polyacrylamide is it is characterised in that comprise the following steps:
(1) feed intake: deionized water is put in polymer reactor, under agitation, once putting into raw materials quality fraction is
30% acrylamide aqueous solution, cationic monomer, anionic monomer, cosolvent, chain-transferring agent, with alkali come the ph of regulation system
Value；Initiator is added after logical nitrogen deoxygenation；
(2) adiabatic polymerisation reaction: initiation temperature controls for 2～25 DEG C, and 2～6h post polymerization system temperature no longer raises as anti-
Should terminate, obtain polymeric colloid；
(3) by granulating from colloid, drying, pulverizing, screening, obtain high intrinsic viscosity amphoteric ionic polyacrylamide product；
Initiator described in step (1) is in azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile) or azo-bis-isobutyrate hydrochloride
One or more, its consumption is the 0.005%～0.075% of starting monomer quality；
Cationic monomer described in step (1) is acrylyl oxy-ethyl-trimethyl salmiac, methylacryoyloxyethyl front three
One or more of ammonium chloride or dimethyl diallyl ammonium chloride, its addition account for starting monomer gross mass 10%～
60%；
Anionic monomer described in step (1) is in 2- acrylamido 2- methyl propane sulfonic acid, acrylic acid or sodium acrylate
Plant or several, its addition accounts for the 1%～30% of starting monomer gross mass；
Through preheating, pre-heating technique is described initiator: through the pretreatment in 10 minutes of 50 DEG C of constant temperature.
2. the preparation method of amphoteric ionic polyacrylamide according to claim 1 is it is characterised in that institute in step (1)
Stating cosolvent is carbamide, and its addition accounts for the 0.1%～5% of starting monomer gross mass.
3. the preparation method of amphoteric ionic polyacrylamide according to claim 1 is it is characterised in that institute in step (1)
Stating chain-transferring agent is that in sodium formate, β-dimethylamino butyronitrile or isopropanol, its addition accounts for the 0.01% of starting monomer gross mass
～0.07%.
4. the preparation method of amphoteric ionic polyacrylamide according to claim 1 is it is characterised in that institute in step (1)
The alkali stated is sodium hydroxide, and for adjusting ph value, its addition is adjusted by ph value and is defined to 4～8.
5. the preparation method of amphoteric ionic polyacrylamide according to claim 1 is it is characterised in that described polymerization
Reaction process condition is as follows:
Initiation temperature DEG C 2～25
It is passed through nitrogen amount m3/m360～80
Baking temperature DEG C 40～80
Wherein it is passed through the volume that nitrogen amount refers to the nitrogen that every cubic metre of polymeric solution is passed through.
6. according to claim 1 or 5 the preparation method of amphoteric ionic polyacrylamide it is characterised in that step (2)
Described in preferably 5～20 DEG C of initiation temperature.
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| CN110527028B (en) * | 2019-09-05 | 2022-01-04 | 江苏富淼科技股份有限公司 | Instant cationic polyacrylamide and preparation method thereof |
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