CN103483598B - Method for accelerating polyvinyl alcohol dissolution - Google Patents
Method for accelerating polyvinyl alcohol dissolution Download PDFInfo
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- CN103483598B CN103483598B CN201310444009.7A CN201310444009A CN103483598B CN 103483598 B CN103483598 B CN 103483598B CN 201310444009 A CN201310444009 A CN 201310444009A CN 103483598 B CN103483598 B CN 103483598B
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Abstract
The invention discloses a method for accelerating polyvinyl alcohol dissolution. Mechanical activation is adopted to treat the polyvinyl alcohol, the molecular structure of the polyvinyl alcohol is broken, a solid micromolecular solvent is added when the mechanical activation is carried out, the solid micromolecular solvent permeates into polyvinyl alcohol molecules, the polyvinyl alcohol molecules are enabled to be carried out solid phase swelling, so that quick dissolution of the polyvinyl alcohol is realized. The method adopted by the invention is low in energy consumption, short in time consumption, simple and convenient to operate, pollution-free, does not need high temperature and high pressure, and belongs to environment friendly methods; the mechanical activation is adopted to treat the polyvinyl alcohol, hydrogen bonds and crystalline structures between polyvinyl alcohol molecules are broken in advance, and the dissolution time of the polyvinyl alcohol is effectively shortened; the polyvinyl alcohol is enabled to be subjected to solid phase swelling, and the reaction time of the polyvinyl alcohol and a liquid solvent is shortened; during the dissolution process, a solid solvent and the liquid solvent are relatively permeated, and the dissolution efficiency of the polyvinyl alcohol is greatly improved; meanwhile the method is wide in applicability, can effectively improve the solubility of the water-soluble polymer, and particularly has an obvious function on polyol.
Description
Technical field
The invention belongs to polymeric material field, be specifically related to a kind of method adopting mechanical activation and the swelling acceleration polyvinyl alcohol dissolution of solid phase.
Background technology
Polyvinyl alcohol (Polyvinyl alcohol, PVA) is a kind of non-toxic water soluble high molecular polymer, is widely used in the fields such as fiber, film, medicine, tackiness agent.Polyvinyl alcohol is a kind of polyol, and wetting ability is very strong, but granule of polyvinyl alcohol is insoluble in water, the serious application limiting polyvinyl alcohol and development.The dissolution process of polyvinyl alcohol in water is complicated, and has very large difference with the difference of its polymerization degree, alcoholysis degree.Trace it to its cause be due between polyvinyl alcohol molecule and intramolecular hydrogen bond association and height crystallinity cause.Therefore, exploring a kind of method of energy rapid solution polyvinyl alcohol, is the large practical problems that current industrial production faces.
For rapid solution polyvinyl alcohol, existing scholar explores from the preparatory phase of polyvinyl alcohol.Such as Chinese patent CN 102827316 A discloses a kind of preparation method of polyvinyl alcohol with low crystallinity.The method comprises the processes such as polymerization, alcoholysis and each unit of drying, and by the warm air drying at 30 ~ 120 DEG C of the polyvinyl alcohol work in-process after alcoholysis, within 0.5 ~ 5 hour, obtain the polyvinyl alcohol of low-crystallinity, products made thereby solubility property increases.This method explores from the preparatory phase of polyvinyl alcohol, and for the difficult problem of dissolving of polyvinyl alcohol finished product, and inapplicable.
At present, the dissolving method that polyvinyl alcohol finished product is conventional has heated and stirred method and modification method.Heated and stirred method and high temperature are hotted plate, high-speed stirring, and dissolution process reaches 2 ~ 4 hours, and energy consumption is high; Modification rule introduces some hydrophilic radicals to polyvinyl alcohol molecule, enhanced polyethylene alcohol water-soluble, though this method can solve the problem of polyvinyl alcohol dissolution difficulty, under normal circumstances, the group introduced easily affects other performances of polyvinyl alcohol, such as, under sticky stickiness, perviousness degradation.Therefore, find low, the consuming time short and dissolving method not reducing polyvinyl alcohol excellent properties of a kind of new energy consumption to have important practical significance.
Summary of the invention
For above-mentioned the deficiencies in the prior art part, the invention provides a kind of method being intended to solve the acceleration polyvinyl alcohol dissolution that polyvinyl alcohol dissolution power consumption is high, the time is long.
In order to solve the problems of the technologies described above, present invention employs following technical scheme:
A kind of method accelerating polyvinyl alcohol dissolution, mechanical activation is adopted to process polyvinyl alcohol, destroy its molecular structure, solid small molecule solvent is added while mechanical activation, solid small molecule solvent penetrates in polyvinyl alcohol molecule, make it that solid phase occur swelling, thus realize rapid solution polyvinyl alcohol.
As a preferred embodiment of the present invention, described mechanical activation comprises two stages: the treatment stage of pretreatment stage and mechanical force;
Described pretreatment stage refers to and polyvinyl alcohol is carried out pre-treatment through microwave, rayed, ultrasonic, electric field or magnetic field;
Refer to the treatment stage of described mechanical force rubbing through pretreated polyvinyl alcohol, colliding, impact or the process of shearing mechanism power.
As another kind of preferred version of the present invention, described molecular structure is hydrogen bond structure and crystalline texture.
As another preferred version of the present invention, solid phase is swelling refer to the spontaneous or non-spontaneous of solid small-molecule substance enter polymer molecule interchain, weaken or destroy the reactive force of polymer molecule interchain, or be inserted in the lattice of polymkeric substance, making the lattice distortion of polymkeric substance, there is expansion to a certain degree in the volume of polymkeric substance.
As a modification of the present invention scheme, carry out solid phase swelling treatment to polyvinyl alcohol to refer to solid small molecule solvent is mixed with polyvinyl alcohol, in mechanical activation process, solid small-molecule substance enters between the molecular chain of polyvinyl alcohol, weaken or destroy the reactive force of polyvinyl alcohol molecule interchain, or be inserted in the lattice of polyvinyl alcohol, making the lattice distortion of polyvinyl alcohol, there is expansion to a certain degree in the volume of polyvinyl alcohol.
As another kind of improvement project of the present invention, described solid small molecule solvent has strong polarity or strong infiltrative material.
As another improvement project of the present invention, polyvinyl alcohol dissolution refers to that polyvinyl alcohol dissolves at 30 ~ 95 DEG C.
Scheme as a further improvement on the present invention, polyvinyl alcohol is through the polyvinyl alcohol after mechanical activation and solid phase swelling treatment.
Compared with prior art, the present invention has following beneficial effect:
1, the method applied in the present invention energy consumption is low, consuming time short, easy and simple to handle, pollution-free, without the need to High Temperature High Pressure, belongs to environmentally friendly method.
2, the present invention adopts mechanical activation process polyvinyl alcohol, destroys the hydrogen bond between polyvinyl alcohol molecule and crystalline texture in advance, effectively shortens the dissolution time of polyvinyl alcohol.
3, the present invention makes polyvinyl alcohol generation solid phase swelling, shortens the time with liquid solvent effect.
4, through the polyvinyl alcohol of the inventive method process, in dissolution process, solid-liquid two kinds of solvent relative permeate, greatly improve the dissolved efficiency of polyvinyl alcohol.
5, the method for the invention suitability is wide, effectively can improve the solvability of water-soluble polymers, especially obvious to polyol effect.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Accelerate a method for polyvinyl alcohol dissolution, adopt mechanical activation to carry out process 3min ~ 5min to polyvinyl alcohol; Then by pretreated polyvinyl alcohol and solid small molecule solvent Homogeneous phase mixing, mechanical force process 30min ~ 60min is carried out; Polyvinyl alcohol after mechanical activation and solid phase swelling treatment is added deionized water, carries out dissolving at 30 ~ 95 DEG C and dissolve.
Wherein, adopt mechanical activation method process polyvinyl alcohol (PVA), mechanical activation comprises two stages: the treatment stage of pretreatment stage and mechanical force.Pretreatment stage refers to and polyvinyl alcohol is carried out pre-treatment through microwave, rayed, ultrasonic, electric field or magnetic field etc., and the toughness of PVA is reduced, and fragility increases, for mechanical force process is prepared.Refer to rubbing through pretreated polyvinyl alcohol, colliding, impact or the mechanical force process such as shearing treatment stage of mechanical force, mechanical force treatment facility comprises stone mill, ball mill, pulverizer etc., according to the principle of energy conservation, mechanical energy is the interior energy of polyvinyl alcohol, can improve, increased activity, polymer stabilisation weakens, the order of its structure is weakened, intermolecular hydrogen bond association weakens, degree of crystallinity reduces, thus reach the object of rapid solution PVA.
Adopt solid phase swelling treatment PVA, between the molecular chain entering polyvinyl alcohol making the spontaneous or non-spontaneous of solid small-molecule substance, weaken or destroy the reactive force of polyvinyl alcohol molecule interchain, or be inserted in the lattice of polyvinyl alcohol, making the lattice distortion of polyvinyl alcohol, there is expansion to a certain degree in the volume of polyvinyl alcohol.Make its molecular structure, especially hydrogen bond and crystalline texture are destroyed.Also solid small molecule solvent can be mixed with polyvinyl alcohol, in mechanical activation process, solid small-molecule substance enters between the molecular chain of polyvinyl alcohol, weaken or destroy the reactive force of polyvinyl alcohol molecule interchain, or be inserted in the lattice of polyvinyl alcohol, making the lattice distortion of polyvinyl alcohol, there is expansion to a certain degree in the volume of polyvinyl alcohol.
Swelling to carrying out solid phase while polyvinyl alcohol mechanical activation, the two is mutually promoted, and can destroy crystalline texture and the hydrogen bond association of polyvinyl alcohol to the full extent, thus accelerates the dissolving of PVA further.Solid small molecule solvent has strong polarity or strong infiltrative material.Polyvinyl alcohol is through the polyvinyl alcohol after mechanical activation and solid phase swelling treatment.
Embodiment one
Take 30gPVA, ultrasonic pretreatment 4min, then with after the mixing of 0.03g urea and 0.05g nitroso-group ethene, with stone mill, activation treatment 30min is carried out to mixture, get the mixture after 20g process, add the water of 280g, then be warming up to 30 DEG C and dissolve.
Embodiment two
Take 30gPVA, put into microwave oven and process 4min, then with after the mixing of 0.25g urea and 0.3g Nitromethane 99Min., with ball mill, activation treatment 35min is carried out to mixture, get the mixture after 20g process, add the water of 280g, then be warming up to 45 DEG C and dissolve.
Embodiment three
Take 30gPVA, photo-irradiation treatment 5min, then after mixing with 0.5g trimeric cyanamide and 0.8g Nitromethane 99Min., with pulverizer, activation treatment 40min is carried out to mixture, get the mixture after 20g process, add the water of 280g, then be warming up to 65 DEG C and dissolve.
Embodiment four
Take 30gPVA, electric field treatment 5min, then with after the mixing of 0.8g trimeric cyanamide and 1.5g urea, with stone mill, activation treatment 45min is carried out to mixture, get the mixture after 20g process, add the water of 280g, then be warming up to 85 DEG C and dissolve.
Embodiment five
Take 30gPVA, put into magnetic field and process 3min, then with after the mixing of 1.2g trimeric cyanamide and 2g nitroso-group ethene, with pulverizer, activation treatment 50min is carried out to mixture, get the mixture after 20g process, add the water of 280g, then be warming up to 95 DEG C and dissolve.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (6)
1. one kind is accelerated the method for polyvinyl alcohol dissolution, it is characterized in that, mechanical activation is adopted to process polyvinyl alcohol, destroy its molecular structure, solid small molecule solvent is added while mechanical activation, solid small molecule solvent penetrates in polyvinyl alcohol molecule, makes it that solid phase occur swelling, thus realizes rapid solution polyvinyl alcohol;
Described mechanical activation comprises two stages: the treatment stage of pretreatment stage and mechanical force;
Described pretreatment stage refers to and polyvinyl alcohol is carried out pre-treatment through microwave, rayed, ultrasonic, electric field or magnetic field;
Refer to the treatment stage of described mechanical force and adopt graphite, ball milling or pulverizer to rubbing through pretreated polyvinyl alcohol, colliding, impact or the process of shearing mechanism power;
Described solid small molecule solvent has strong polarity or strong infiltrative material; Comprise urea, nitroso-group ethene, Nitromethane 99Min. or trimeric cyanamide.
2. a kind of method accelerating polyvinyl alcohol dissolution according to claim 1, is characterized in that, described molecular structure is hydrogen bond structure and crystalline texture.
3. a kind of method accelerating polyvinyl alcohol dissolution according to claim 1, it is characterized in that, solid phase is swelling refer to the spontaneous or non-spontaneous of solid small-molecule substance enter polymer molecule interchain, weaken or destroy the reactive force of polymer molecule interchain, or be inserted in the lattice of polymkeric substance, making the lattice distortion of polymkeric substance, there is expansion to a certain degree in the volume of polymkeric substance.
4. a kind of method accelerating polyvinyl alcohol dissolution according to claim 1, it is characterized in that, carry out solid phase swelling treatment to polyvinyl alcohol to refer to solid small molecule solvent is mixed with polyvinyl alcohol, in mechanical activation process, solid small-molecule substance enters between the molecular chain of polyvinyl alcohol, weakens or destroy the reactive force of polyvinyl alcohol molecule interchain, or is inserted in the lattice of polyvinyl alcohol, making the lattice distortion of polyvinyl alcohol, there is expansion to a certain degree in the volume of polyvinyl alcohol.
5. a kind of method accelerating polyvinyl alcohol dissolution according to claim 1, is characterized in that, polyvinyl alcohol dissolution refers to that polyvinyl alcohol dissolves at 30 ~ 95 DEG C.
6. a kind of method accelerating polyvinyl alcohol dissolution according to claim 1, is characterized in that, polyvinyl alcohol is through the polyvinyl alcohol after mechanical activation and solid phase swelling treatment.
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| CN107216464B (en) * | 2017-06-14 | 2018-06-01 | 荆州市九天化工科技有限公司 | A kind of preparation method of rapidly-soluble polyvinyl alcohol |
| CN109054265B (en) * | 2018-07-26 | 2021-02-05 | 上海全宇生物科技遂平有限公司 | Method for preparing expanded polyvinyl alcohol |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101250237A (en) * | 2008-03-31 | 2008-08-27 | 浙江工业大学 | Non-solvent ectraction method of chondroitin sulfate |
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| JPH05245138A (en) * | 1992-03-03 | 1993-09-24 | Terumo Corp | Production of polyvinyl alcohol gel for ultrasonic medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101250237A (en) * | 2008-03-31 | 2008-08-27 | 浙江工业大学 | Non-solvent ectraction method of chondroitin sulfate |
Non-Patent Citations (1)
| Title |
|---|
| "Effect of Interactions Between Poly(vinyl alcohol)and Urea on the Water Solubility of Poly(vinyl alcohol)";Chuntang Lei et al.;《Journal of Applied Polymer Science》;20090608;第114卷;第517-523页 * |
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