CN102408571B - Water-soluble cross-lined polymer and preparation method thereof - Google Patents
Water-soluble cross-lined polymer and preparation method thereof Download PDFInfo
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- CN102408571B CN102408571B CN2011102788542A CN201110278854A CN102408571B CN 102408571 B CN102408571 B CN 102408571B CN 2011102788542 A CN2011102788542 A CN 2011102788542A CN 201110278854 A CN201110278854 A CN 201110278854A CN 102408571 B CN102408571 B CN 102408571B
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Abstract
The invention relates to a water-soluble cross-lined polymer and a preparation method thereof. A technique for synthesizing polyacrylic acid water-soluble cross-linked polymer poly(acrylic acid-malic anhydride)-polyethylene glycol 4000 (P(AA-MAh)-PEG4000) through esterification reaction is characterized in that: the raw material formula comprises 50.0 g of P(AA-MAh) and 3.0-3.5 g of PEG4000; and the process conditions are as follows: the reaction temperature is 75 DEG C, a solvent is butanone, an initiator is para-toluenesulfonic acid (PTSA) and the reaction time is respectively 15 hours. The preparation method has the beneficial effects that: a novel polyacrylic acid water-soluble cross-linked polymer is synthesized, thereby laying a foundation for the application of the water-soluble polymers in wider fields; the needed raw materials are inexpensive, the operation process is direct and simple, and the preparation method has wide applicability and certain practical popularization significance.
Description
Technical field
The present invention relates to a kind of cross linked water soluble polymer and preparation method thereof.
Background technology
Water-soluble polymers has obtained in fields such as petroleum exploration and development, water treatment, papermaking, weaving, coating, food, daily-use chemical industries using widely owing to have diversified kind and property.At present, in miscellaneous water-soluble polymers, polyacrylic research and application are comparatively extensive.But self forms single ROHM water-soluble polymers, the constraint of structure owing to receiving, and has limited its application.If polyacrylic composition, structure are designed, synthesize serial polyacrylic polymer.Based on the thought of molecular designing, to acrylic acid polymer form, structure design, synthetic to obtain new polymkeric substance be the comparatively practicable method of development this type water-soluble polymers, also is research focus in recent years.
With vinylformic acid, maleic anhydride is monomer, and (vinylformic acid-maleic anhydride) copolymer p of a kind of gathering (AA-MAh) is synthesized in copolymerization, and the synthesis technique of this multipolymer field very ripe, practical application is also very extensive.Clearly, let maleic anhydride and polyethylene glycol long chain generation esterification in this copolymer chain just can prepare a kind of polyacrylic cross linked water soluble polymer.The cross-linked polymer of this composition, structure will inevitably enrich the kind of polyacrylic water-soluble polymers, increases the scope of its application.At present, do not see any relevant research report as yet.
Summary of the invention
The technical problem that solves
In order to enlarge the Application Areas of polyacrylic water-soluble polymers, the while the present invention proposes a kind of preparation method of polymkeric substance also in order to expand this base polymer of ROHM, synthesizes to have obtained a kind of polyacrylic cross linked water soluble polymer.
Technical scheme
The present invention gathers (vinylformic acid-maleic anhydride) P (AA-MAh) with a kind of multipolymer and with polyoxyethylene glycol (PEG4000) esterification takes place, synthetic polyacrylic cross linked water soluble polymer P (AA-MAh)-PEG4000.Its purpose is to obtain a kind of new polyacrylic cross linked water soluble polymer P (AA-MAh)-PEG4000.
A kind of method for preparing polyacrylic cross linked water soluble polymer P (AA-MAh)-PEG4000 of the present invention, its technical characterictic is:
Synthesizing formula
P(AA-MAh) 50.0?g
PEG4000 3.0~3.5?g
Processing condition
Initiator tosic acid (PTSA)
2.0 g
Solvent butanone 200 ml
75 ℃ of temperature
The environment nitrogen protection
Reaction times 15 h
A kind of method for preparing polyacrylic cross linked water soluble polymer P (AA-MAh)-PEG4000, it is characterized in that: concrete steps are following:
A) take by weighing the P (AA-MAh) of 50.0g and the PEG4000 of 3.0~3.5g, add the butanone dissolving of 200ml, add 2.0g tosic acid (PTSA) then, mix being placed in three mouthfuls of reaction flasks;
B) under the nitrogen protection, at 75 ℃ of following constant temperature stirring reaction 15h;
C) solution that obtains is poured in the beaker, be settled out faint yellow gluey thing, be crude product with absolute ethyl alcohol;
D) be that solvent, absolute ethyl alcohol are the precipitation agent reprecipitation with the butanone, dissolve repeatedly, precipitate 4 times, can obtain the white rubber shaped polymer;
E) at last products therefrom is washed 4 times with sherwood oil respectively repeatedly, vacuum-drying 3 days obtains purified polymer.
Beneficial effect
The invention has the beneficial effects as follows; The synthesis technique that a kind of method is feasible, be easy to realize is provided; Synthesize and obtained a kind of new polyacrylic cross linked water soluble polymer P (AA-MAh)-PEG4000; This has not only expanded this type of ROHM water-soluble polymers, and lays the first stone in the application in the wide spectrum more for this base polymer.
Description of drawings
Fig. 1 is the synthesis process flow diagram of polymkeric substance.
Embodiment
Obtain polymer P (AA-MAh)-PEG4000 for synthetic, the present invention has taked following embodiment:
Take by weighing 50.0g P (AA-MAh) and 3.0~3.5g PEG4000, add the dissolving of 200ml butanone, add 2.0g tosic acid (PTSA) then, mix being placed in three mouthfuls of reaction flasks; Under the nitrogen protection, at 75 ℃ of following constant temperature stirring reaction 15h; Reaction is poured the viscous solution that obtains in the beaker into after finishing, and is settled out faint yellow gluey thing with absolute ethyl alcohol, is crude product; Be that solvent, absolute ethyl alcohol are the precipitation agent reprecipitation then with the butanone, dissolve repeatedly, precipitate 4 times, can obtain the white rubber shaped polymer; At last products therefrom is washed 4 times with sherwood oil respectively repeatedly, vacuum-drying 3 days obtains purified polymer.
Claims (2)
1. polyacrylic cross linked water soluble polymer, its technical characterictic is that its preparation method is: composition of raw materials: ROHM maleic anhydride P (AA-MAh) quality 50.0g, polyoxyethylene glycol PEG4000 quality 3.0~3.5g; Processing condition: temperature of reaction is 75 ℃, and solvent is a butanone, and initiator is tosic acid (PTSA), and the reaction times is respectively 15h.
2. method for preparing the polyacrylic cross linked water soluble polymer of claim 1, it is characterized in that: concrete steps are following:
A) take by weighing the P (AA-MAh) of 50.0g and the PEG4000 of 3.0~3.5g, add the butanone dissolving of 200ml, add 2.0g tosic acid (PTSA) then, mix being placed in three mouthfuls of reaction flasks;
B) under the nitrogen protection, at 75 ℃ of following constant temperature stirring reaction 15h;
C) solution that obtains is poured in the beaker, be settled out faint yellow gluey thing, be crude product with absolute ethyl alcohol;
D) be that solvent, absolute ethyl alcohol are the precipitation agent reprecipitation with the butanone, dissolve repeatedly, precipitate 4 times, can obtain the white rubber shaped polymer;
E) at last products therefrom is washed 4 times with sherwood oil respectively repeatedly, vacuum-drying 3 days obtains purified polymer.
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