CN103319668B - A kind of preparation method of butyl methacrylate dimethylaminoethyl segmented copolymer - Google Patents
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Abstract
The present invention relates to a kind of preparation method of butyl methacrylate dimethylaminoethyl segmented copolymer, by reaction system monomers B MA, initiator A IBN, molecular weight regulator 1, the reaction of 1-diphenylethlene and solvent obtains poly-n-butyl methacrylate presoma, and the initiator that it can be used as dimethylaminoethyl methacrylate to react, by heated polymerizable, obtain butyl methacrylate dimethylaminoethyl segmented copolymer.The preparation method of a kind of butyl methacrylate dimethylaminoethyl segmented copolymer provided by the invention, compared with the butyl methacrylate dimethylaminoethyl segmented copolymer using ATRP method to prepare, reaction conditions is simple, easy handling, production cost are low, there is no the residual of organic catalyst, be conducive to suitability for industrialized production, have wide practical use in coating dispersant field.
Description
Technical field
The present invention relates to technical field of polymer chemistry, especially relate to a kind of preparation method of butyl methacrylate dimethylaminoethyl segmented copolymer.
Background technology
Amphipathic nature block polymer refers to the multipolymer be made up of hydrophilic and oleophylic section.Amphipathic nature polyalcohol becomes one of focus of current polymer subject area research owing to having special character, it is shell that this base polymer is formed with hydrophilic section in water, hydrophobic section is the micellar structure of core, then form structure contrary " reverse micelle " in organic solvent, research shows, micella also can by further assembling the aggregate forming compound with regular structure.Amphipathic nature block polymer can promote the mixing of aqueous phase and oil phase, and at tensio-active agent, dispersion agent field is widely used.
At present, the method for the synthetic segmented copolymer that development is comparatively perfect is anionoid polymerization.It is synthesis of narrow molecular weight distribution and block, the most important a kind of polymerization process of unique construction polymer such as star-like.But anionoid polymerization is easily inhibited by the trace impurity in system, polymerizing condition is harsh, has active group as also inapplicable in the monomer of hydroxyl, amido for some.
Butyl methacrylate is a kind of common oiliness monomer, and its glass transition temperature of polymer, near room temperature, is widely used at coating and adhesive area.Dimethylaminoethyl methacrylate (DMAEMA) is a kind of broad-spectrum functional monomer, and it has the characteristic of alkene, amine, ester compound simultaneously, can be polymerized under certain condition, addition, the chemical reaction such as quaternary ammoniated and hydrolysis.The segmented copolymer of butyl methacrylate dimethylaminoethyl has wide practical use in coating dispersant field.
Due to the impact of the amino in dimethylaminoethyl methacrylate, the segmented copolymer (PBMA-g-PDMAEMA) of butyl methacrylate dimethylaminoethyl can not be obtained by anionoid polymerization.Compared with other polyreaction types, Transfer Radical Polymerization (ATRP) polymerisable monomeric species is many, easy to control.The people such as Mao take CuCl/HMTETA as the atom transfer radical polymerization that initiator system carries out DMAEMA at 25 DEG C, obtain molecular weight and controlled PDMAEMA macromole evocating agent [MaoB., the GanL. of molecular weight; GanY.; LiX., RaviP., TamK..JPolymSciPartAPolymChem2004; 42:5161-9.].Macromole evocating agent PDMAEMA causes the atom transfer radical polymerization of second comonomer butyl methacrylate (BMA) further; and then obtain amphipathic nature block polymer PDMAEMA-b-PBMA [LeenaN.; SusannaH., JanneL..Ultra-thinfilmsofcationicamphiphilicpoly (2-(dimethylamino) ethylmethacrylate) basedblockcopolymersassurfacewettabilitymodifiersPolymer 2009; 50:5250-5261.].But the catalyzer used in the middle of ATRP method is generally transition metal salt, large usage quantity, poisonous and color is difficult to remove, and is polymerized part used also costly, is unfavorable for suitability for industrialized production.Simultaneously the polymer ends that obtains of ATRP is inevitably with carbon-bromine key end group that chemical bond energy is lower, and this will have influence on the heat-resisting of the finished product and ageing-resistant performance.
Summary of the invention
The technical problem to be solved in the present invention is: preparing to overcome ATRP in prior art the problem that catalyst levels in PBMA-b-PDMAEMA process is comparatively large, cost is high, resulting polymers has catalyst residue, providing a kind of method preparing butyl methacrylate dimethylaminoethyl segmented copolymer.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of butyl methacrylate dimethylaminoethyl segmented copolymer, comprises the following steps:
1) preparation of poly-n-butyl methacrylate: by monomers B MA, initiator A IBN, molecular weight regulator 1,1-diphenylethlene and solvent join in reactor and stir, repeatedly vacuumize and logical argon gas to remove oxygen and moisture, react 20-25h under being then heated to the condition of 70-75 DEG C.
The mol ratio of described BMA and AIBN is 100:0.4-1.5, and the mol ratio of described AIBN and 1，1-diphenylethylene is 1:2, and described solvent is the one in toluene, butylacetate;
2) purification of poly-n-butyl methacrylate: after having reacted, product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive methyl alcohol precipitate revolving the product after steaming, filter, the throw out obtained is joined in trichloromethane and dissolves completely, then, precipitate in throw out chloroform soln instillation excessive methanol, repeat 2-3 time to remove unreacted BMA, AIBN, 1, 1-diphenylethlene and a small amount of solvent, the throw out vacuum-drying finally will obtained, namely poly-n-butyl methacrylate is obtained, structure is as follows:
3) preparation of butyl methacrylate dimethylaminoethyl segmented copolymer: by step 2) PBMA of gained is dissolved in butylacetate, being joined by second comonomer DMAEMA is dissolved with in the butylacetate of PBMA again, repeatedly vacuumize after stirring and logical argon gas to remove oxygen and moisture, react 4-6h under being then heated to the condition of 85 DEG C.
Wherein, the mass ratio of described PBMA and DMAEMA is 1:0.5-5.
4) purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after having reacted, product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 2-3 time to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, structure is as follows:
Particularly, described type of heating is oil bath heating.
The invention has the beneficial effects as follows: the preparation method of a kind of butyl methacrylate dimethylaminoethyl segmented copolymer provided by the invention, compared with the butyl methacrylate dimethylaminoethyl segmented copolymer using ATRP method to prepare, reaction conditions is simple, easy handling, production cost are low, there is no the residual of organic catalyst, be conducive to suitability for industrialized production, effectively can solve the reduction causing the heat-resisting of product and ageing-resistant performance because organic catalyst remains.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the nuclear magnetic spectrogram of the butyl methacrylate dimethylaminoethyl segmented copolymer of embodiment 3 gained;
Fig. 2 is the gpc analysis of poly-n-butyl methacrylate and poly-(butyl methacrylate-b-dimethylaminoethyl methacrylate) in embodiment 3.
Embodiment
Below in conjunction with specific embodiment, further the present invention is set forth, should be understood that and quote embodiment only for illustration of the present invention, and be not used in and limit the scope of the invention.
Embodiment 1
(1) polymerization formula: the mol ratio of monomer (BMA), initiator (AIBN), 1，1-diphenylethylene is 100:0.4:0.8, then add equal total mass 50% toluene as solvent.
Polymerization procedure: add BMA monomer 50g(0.35mol in the 250mL four-hole boiling flask that thermometer, magnetic stir bar are housed), initiator A IBN0.2310g(0.0014mol), 1,1-diphenylethlene 0.5070g(0.0028mol), solvent toluene 50g, mix, system is vacuumized repeatedly logical argon gas three times, at 70 DEG C, react 25h.
The purification of poly-n-butyl methacrylate: after reaction terminates, the solvent in rotary evaporation removing system, till liquid no longer drips in rotatory evaporator, obtains the product of the micro-thickness of water white transparency.Instill in excessive methyl alcohol precipitate revolving the product after steaming, filter, the throw out obtained is joined in trichloromethane and dissolves completely, then, precipitate in throw out chloroform soln instillation excessive methanol, repeat 2 times to remove unreacted BMA, AIBN, 1,1-diphenylethlene and a small amount of solvent, the throw out vacuum-drying finally will obtained, namely obtains poly-n-butyl methacrylate, product quality is 33.88g, and gas phase tracking report transformation rate is 67.76%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=26400 of PBMA, PDI=1.58.
(2) polymerization formula: with the PBMA of synthesis in step (1) for macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:1, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 100mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA10g, solvent acetic acid butyl ester 20g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 5h.
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 2 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 4.51g, gas phase tracking report transformation rate is 49.31%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=49800 of PBMA-b-PDMAEMA, PDI=1.70.
Embodiment 2
Using the PBMA of synthesis in embodiment 1 step (1) as macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:5, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 100mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA50g, solvent acetic acid butyl ester 20g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 6h.
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 2 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 19.62g, gas phase tracking report transformation rate is 42.44%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=60200 of PBMA-b-PDMAEMA, PDI=2.36.
Embodiment 3
(1) polymerization formula: the mol ratio of monomer (BMA), initiator (AIBN), 1，1-diphenylethylene is 100:1:2, then add equal total mass 50% butylacetate as solvent.
Polymerization procedure: add BMA monomer 50g(0.35mol in the 250mL four-hole boiling flask that thermometer, magnetic stir bar are housed), initiator A IBN0.2310g(0.0035mol), DPE0.5070g(0.0070mol), solvent toluene 50g, mix, at 75 DEG C, react 20h.
The purification of poly-n-butyl methacrylate: after reaction terminates, the solvent in rotary evaporation removing system, till liquid no longer drips in rotatory evaporator, obtains the product of the micro-thickness of water white transparency.Instill in excessive methyl alcohol precipitate revolving the product after steaming, filter, the throw out obtained is joined in trichloromethane and dissolves completely, then, precipitate in throw out chloroform soln instillation excessive methanol, repeat 3 times to remove unreacted BMA, AIBN, 1,1-diphenylethlene and a small amount of solvent, the throw out vacuum-drying finally will obtained, namely obtains poly-n-butyl methacrylate, product quality is 31.52g, and gas phase tracking report transformation rate is 63.04%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=15100 of PBMA, PDI=1.43.
(2) polymerization formula: with the PBMA of synthesis in step (1) for macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:0.5, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 100mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA5g, solvent acetic acid butyl ester 15g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 5.5h.
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 2 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 2.56g, gas phase tracking report transformation rate is 50.35%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=25600 of PBMA-b-PDMAEMA, PDI=1.35.
Embodiment 4
Using the PBMA of synthesis in embodiment 3 step (1) as macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:1, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 100mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA10g, solvent acetic acid butyl ester 20g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 4h.
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 3 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 5.96g, gas phase tracking report transformation rate is 64.29%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=39000 of PBMA-b-PDMAEMA, PDI=1.69.
Embodiment 5
Using the PBMA of synthesis in embodiment 3 step (1) as macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:3, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 250mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA30g, solvent acetic acid butyl ester 40g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 4.5h.
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 3 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 12.16g, gas phase tracking report transformation rate is 50.20%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=43200 of PBMA-b-PDMAEMA, PDI=1.9.
Embodiment 6
Using the PBMA of synthesis in embodiment 3 step (1) as macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:5, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 250mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA50g, solvent acetic acid butyl ester 60g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 5h.
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 3 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 16.56g, gas phase tracking report transformation rate is 46.50%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=53700 of PBMA-b-PDMAEMA, PDI=1.91.
Embodiment 7
(1) polymerization formula: the mol ratio of monomer (BMA), initiator (AIBN), 1，1-diphenylethylene is 100:1.5:3, then add equal total mass 50% toluene as solvent.
Polymerization procedure: add BMA monomer 50g(0.35mol in the 250mL four-hole boiling flask that thermometer, magnetic stir bar are housed), initiator A IBN0.8662g(0.0053mol), DPE1.9014g(0.0105mol), solvent toluene 50g, mix, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 70 DEG C, react 25h.
The purification of poly-n-butyl methacrylate: after reaction terminates, the solvent in rotary evaporation removing system, till liquid no longer drips in rotatory evaporator, obtains the product of the micro-thickness of water white transparency.Instill in excessive methyl alcohol precipitate revolving the product after steaming, filter, the throw out obtained is joined in trichloromethane and dissolves completely, then, precipitate in throw out chloroform soln instillation excessive methanol, repeat 3 times to remove unreacted BMA, AIBN, 1,1-diphenylethlene and a small amount of solvent, the throw out vacuum-drying finally will obtained, namely obtains poly-n-butyl methacrylate, product quality is 36.02g, and gas phase tracking report transformation rate is 72.05%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=9200 of PBMA, PDI=1.67.
(2) polymerization formula: with the PBMA of synthesis in step (1) for macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:1, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 100mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA10g, solvent acetic acid butyl ester 20g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 6h.The reaction times particularly should be had in an embodiment
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 2 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 4.79g, gas phase tracking report transformation rate is 47.91%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=35300 of PBMA-b-PDMAEMA, PDI=1.59.
Embodiment 8
Using the PBMA of synthesis in embodiment 7 step (1) as macromole evocating agent, and the mass ratio of PBMA and DMAEMA is 1:5, then add equal total amount 50% butylacetate as solvent.
Polymerization procedure: add PBMA10g in the 250mL four-hole boiling flask that thermometer, magnetic stir bar are housed, monomer DMAEMA50g, solvent acetic acid butyl ester 60g, mixes, system is vacuumized repeatedly logical argon gas three times to remove oxygen and moisture, at 85 DEG C, react 6h.
The purification of butyl methacrylate dimethylaminoethyl segmented copolymer: after reaction terminates, the solvent in rotary evaporation removing system, obtains the product of water white transparency thickness.Product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 3 times to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely butyl methacrylate dimethylaminoethyl segmented copolymer is obtained, product quality is 18.95g, gas phase tracking report transformation rate is 40.96%.Gel permeation chromatography (GPC) test is carried out to final product, obtains the number-average molecular weight Mn=53300 of PBMA-b-PDMAEMA, PDI=2.25.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to right.
Claims (2)
1. a preparation method for butyl methacrylate dimethylaminoethyl segmented copolymer, is characterized in that comprising the following steps:
1) preparation of poly-n-butyl methacrylate
Monomers B MA, initiator A IBN, molecular weight regulator 1，1-diphenylethylene and solvent are joined in reactor and stir, repeatedly vacuumize and logical argon gas to remove oxygen and moisture, react 20-25h under being then heated to the condition of 70-75 DEG C,
The mol ratio of described BMA and AIBN is 100:0.4-1.5, and the mol ratio of described AIBN and 1，1-diphenylethylene is 1:2, and described solvent is the one in toluene, butylacetate;
2) purification of poly-n-butyl methacrylate
After having reacted, product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive methyl alcohol precipitate revolving the product after steaming, filter, the throw out obtained is joined in trichloromethane and dissolves completely, then, precipitate in throw out chloroform soln instillation excessive methanol, repeat 2-3 time to remove unreacted BMA, AIBN, 1，1-diphenylethylene and a small amount of solvent, the throw out vacuum-drying finally will obtained, namely obtain poly-n-butyl methacrylate, structure is as follows
3) preparation of butyl methacrylate dimethylaminoethyl segmented copolymer
By step 2) PBMA of gained is dissolved in butylacetate, being joined by second comonomer DMAEMA is dissolved with in the butylacetate of PBMA again, repeatedly vacuumize after stirring and logical argon gas to remove oxygen and moisture, react 4-6h under being then heated to the condition of 85 DEG C
Wherein, the mass ratio of described PBMA and DMAEMA is 1:0.5-5;
4) purification of butyl methacrylate dimethylaminoethyl segmented copolymer
After having reacted, product is revolved in a rotary evaporator and steams to remove desolventizing, till in rotatory evaporator, liquid no longer drips, instill in excessive sherwood oil precipitate revolving the product after steaming, filter, the throw out obtained is joined in THF and dissolves completely, then, sedimentary THF solution is instilled in excessive sherwood oil and precipitates, repeat 2-3 time to remove unreacted PBMA and a small amount of solvent, afterwards by throw out vacuum-drying, namely obtain butyl methacrylate dimethylaminoethyl segmented copolymer, structure is as follows
2. the preparation method of a kind of butyl methacrylate dimethylaminoethyl segmented copolymer as claimed in claim 1, is characterized in that: described type of heating is oil bath heating.
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