CN106633104A - Preparation method of water-based polyether sulfone dispersion liquid - Google Patents
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
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- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/06—Polysulfones; Polyethersulfones
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Abstract
The invention relates to the field of high molecular materials, in particular to a preparation method of water-based polyether sulfone dispersion liquid. The preparation method includes swelling polyether sulfone resin in low-boiling-point organic solvent chloroform or tetrahydrofuran to form polyether sulfone suspension liquid, adding the polyether sulfone suspension liquid into dispersion equipment with shearing and grinding functions to perform forced dispersion, adding precipitation liquid into the dispersion equipment to continue dispersion until the polyether sulfone resin is separated out in the form of particles in the liquid to form mixed size, distilling the mixed size into distillation equipment and recycling organic solvent to obtain the water-based polyether sulfone dispersion liquid. The polyether sulfone resin prepared according to the method is separated out gradually in the precipitation liquid through grinding dispersion, the diameters of the particles are small and uniform, the molecular chain structure of the polyether sulfone resin is not damaged, production efficiency is high, and performance is stable.
Description
Technical field
The present invention relates to polymeric material field, and in particular to the preparation method of water-based polyether sulfone dispersion liquid.
Background technology
Polyether sulfone (PES) is amber transparent non-crystalline resin, with heat resistance, anti-flammability, chemical stability, chi
Excellent comprehensive performances such as very little stability, and stress cracking resistance is good, its creep resistant at 180 DEG C be thermoplastic resin in most
High.Polyethersulfone resin structural formula is：
There is the ether of rigid phenyl ring and flexibility in polyether sulfone strand, and sulfuryl is defined greatly with total unit
Conjugated system.Due to these features, polyether sulfone has the advantages that intensity height, high temperature resistant, radiation hardness, antiacid, anti-oxidant, and
And the good characteristics with biocompatibility.Water-based polyether sulfone dispersion liquid can be configured to corrosion-resistant, anti-with polytetrafluoroethylene (PTFE)
The non-viscous paint of the features such as radiation, good insulation preformance, fire-retardant, nontoxic, low friction and optimal metal adhesion, can extensively apply
In industries such as kitchen utensils, household electrical appliance, light industry five metals, industrial mould, plastic machines.
The Polyethersulfone Coating being widely used at present uses organic solvent and makees solvent.Since the end of the sixties in last century, with
The establishment of Zhe Ge developed countries environmental regulation and the enhancing of environmental consciousness, the volatile organic compound in traditional solvent based coating
The discharge of thing is more and more restricted.Therefore, develop low stain environment-friendly type water paint oneself become the main side of coating development
To.And aqueous Polyethersulfone Coating is developed, first have to prepare water-based polyether sulfone dispersion liquid.At present the country prepares water-based polyether sulfone point
Dispersion liquid is generally used and for polyether sulfone to be put into long-time wet grinding in ball mill, and the main deficiency of the method is：One is
High energy consumption, long the production cycle；Two is that polyethersulfone granules particle diameter is big, distribution is wide and shape differs；Three is polyethersulfone resin molecule knot
Structure is destroyed by mechanical force, easily occurs Yellowing during downstream industry application.
Domestic literature《The preparation of water-based polyether sulfone dispersion liquid and redispersible polyether sulfone micro mist》Author Zhang Shouguo, it is open
A kind of method that solvent volatile diffusion method prepares water-based polyether sulfone dispersion liquid.The method dissolves polyethersulfone resin and surfactant
In the mixed solution of chloroform and methyl alcohol, the solution of polyether sulfone organic solvent is made, then existed with colloid mill Forced Dispersion
In the aqueous solution containing surfactant, the polyether sulfone emulsion containing organic solvent is prepared into, then polyether sulfone emulsion is stirred
Mix, condense the prepared polyether sulfone dispersion liquid of recovery.The deficiency of the method is 2 points：One when being the application in polyether sulfone dispersion liquid later stage
Processing temperature can reach 400 DEG C, and surfactant has often decomposed at this temperature, causes the application product later stage easily to go out
Existing more obvious xanthochromia；Two is that surfactant is residued in waste water in production process, it is difficult to recycles, is easily caused environment
Pollution.
In order to solve the above problems, it is badly in need of a kind of preparation method of new water base ether sulfone dispersion liquid.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of water-based polyether sulfone dispersion liquid.
The preparation method of water-based polyether sulfone dispersion liquid, prepares as follows,
(1) by polyether sulfone and organic solvent in mass ratio 1:4～5 mixing, stir 4～6 hours at a temperature of 50～70 DEG C,
Obtain polyether sulfone suspension；
(2) after by the cooling of polyether sulfone suspension, disperse 4～8min, be 1 by polyether sulfone and precipitating liquid mass ratio:5～7 add
Enter precipitating liquid, continue to disperse 20～30min, obtain white mixed serum；The precipitating liquid is pressed for organic solvent with deionized water
Mass ratio 1:The liquid of 2～3 mixing；
(3) white mixed serum is distilled, water-based polyether sulfone dispersion liquid is obtained；
Wherein, organic solvent described in step (1) and (2) is chloroform or tetrahydrofuran, organic molten used by step (1) (2)
Agent is same.
Preferably, in step (1), polyether sulfone and organic solvent in mass ratio 1:5 mixing.
Preferably, in step (1), after polyether sulfone mixes with organic solvent, stir at a temperature of 60 DEG C.
Wherein, in step (2), scattered mode is for shearing and grinds.
Preferably, in step (2), Forced Dispersion, dispersing apparatus are carried out using the dispersing apparatus with shearing grinding function
Rotating speed is not less than 3000rpm, and preferred dispersing apparatus rotating speed is at least 4500rpm.
Preferably, in step (2), after dispersion 5min precipitating liquid is added.
Preferably, in step (2), precipitating liquid is organic solvent and deionized water in mass ratio 1:The liquid of 2 mixing；
Preferably, in step (2), polyether sulfone is 1 with precipitating liquid mass ratio:6.
Preferably, in step (3), distill to 65～70 DEG C of recovery organic solvents；It is preferred that distill to 65～66 DEG C of recovery having
Machine solvent.
The invention solves the problems that second technical problem be to provide a kind of water-based polyether sulfone dispersion liquid, by above-mentioned water base poly-
The preparation method of ether sulfone dispersion liquid is obtained.
Beneficial effects of the present invention：
1st, existing conventional wet grinding high energy consumption, the problem of long the production cycle are overcome, while also overcoming traditional handicraft
Middle product particle particle diameter is big, distribution is wide, the problem of the easy xanthochromia of subsequent applications.
2nd, particle diameter is quickly formed by the double action of dispersing apparatus and precipitating liquid in the state of resin swelling little and equal
Even water-based polyether sulfone dispersion liquid, while solving the problems, such as that polyethersulfone granules particle diameter is big in Conventional milling methods polyethers is not destroyed
The molecular chain structure of sulphone resin, it is ensured that the application performance of product.
3rd, it is the water-based polyether sulfone dispersion liquid excellent performance that prepared using the inventive method, stable.
4th, the inventive method production efficiency height, low cost.
Description of the drawings
Fig. 1 is polyether sulfone dispersion particle electromicroscopic photograph prepared by embodiment 1.
Fig. 2 is that the conventional wet of comparative example 1 grinds the polyether sulfone dispersion particle electromicroscopic photograph for obtaining.
Specific embodiment
The technical problem to be solved in the present invention is to provide a kind of preparation method of water-based polyether sulfone dispersion liquid.Using macromolecule
Swelling in organic solvent is greatly reduced macromolecular chain intermolecular forces, then by adding the precipitating liquid of compounding in high speed point
Be casually arranged with it is standby in gradually separate out and form that particle is little and uniform mixed serum, then by mixed serum distillating recovering solvent so as to obtaining water
Base polyether sulfone dispersion liquid.
The preparation method of water-based polyether sulfone dispersion liquid, prepares as follows,
(1) by polyether sulfone and organic solvent in mass ratio 1:4～5 mixing, stir 4～6 hours at a temperature of 50～70 DEG C,
Obtain polyether sulfone suspension；The step makes polyether sulfone swelling in organic solvent, stirs at this temperature, adds can polyether sulfone
Instant solution；Organic solvent selects low boiling point organic solvent, can not form azeotropic mixture in distillation, easily all reclaims.
(2) after by the cooling of polyether sulfone suspension, disperse 4～8min, be 1 by polyether sulfone and precipitating liquid mass ratio:5～7 add
Enter precipitating liquid, continue to disperse 20～30min, obtain white mixed serum；The precipitating liquid is pressed for organic solvent with deionized water
Mass ratio 1:The liquid of 2～3 mixing；
(3) white mixed serum is distilled, water-based polyether sulfone dispersion liquid is obtained；
Wherein, organic solvent described in step (1) and (2) is chloroform or tetrahydrofuran.It is organic molten used by step (1) (2)
Agent is same.
Preferably, in step (1), polyether sulfone and organic solvent in mass ratio 1:5 mixing.
Preferably, in step (1), after polyether sulfone mixes with organic solvent, stir at a temperature of 60 DEG C.
Wherein, in step (2), scattered mode is for shearing and grinds.
Preferably, in step (2), Forced Dispersion, dispersing apparatus are carried out using the dispersing apparatus with shearing grinding function
Rotating speed is not less than 3000rpm, and preferred dispersing apparatus rotating speed is at least 4500rpm.It is found through experiments, in equivalent constructions equipment,
Rotating speed is higher, and the shearing force of equipment is stronger, and the number of times that material is sheared circulation is also more, and polyethersulfone resin is forced scattered grain
Footpath is less, while its particle diameter distribution is also less.
Preferably, in step (2), after dispersion 5min precipitating liquid is added.
Preferably, in step (2), precipitating liquid is organic solvent and deionized water in mass ratio 1:The liquid of 2 mixing；
Preferably, in step (2), polyether sulfone is 1 with precipitating liquid mass ratio:6.
Preferably, in step (3), distill to 65～70 DEG C of recovery organic solvents；It is preferred that distill to 65～66 DEG C of recovery having
Machine solvent.
The invention solves the problems that second technical problem be to provide a kind of water-based polyether sulfone dispersion liquid, by above-mentioned water base poly-
The preparation method of ether sulfone dispersion liquid is obtained.Water-based polyether sulfone dispersion liquid obtained by this method does not contain surfactant, in the later stage
Xanthochromia is difficult during use.
The specific embodiment of the present invention is further described with reference to embodiment, not therefore by present invention limit
System is among described scope of embodiments.
The preparation (method of the present invention) of the water-based polyether sulfone dispersion liquid of embodiment 1
By taking the reactor of 100L as an example, by following quality raw material are prepared：It is polyethersulfone resin (8Kg), chloroform (40Kg), heavy
Analysis liquid (48Kg, wherein chloroform account for 16Kg, deionized water and account for 32Kg).
Above-mentioned recipe ingredient is distinguished into correct amount, to the 100L reactors with water knockout drum, agitator and heater
Middle addition polyethersulfone resin (8Kg) and chloroform (40Kg), open stirring, and reactor is heated to 60 DEG C, and stirring is gathered after 4 hours
Ether sulfone suspension.
Again temperature of reaction kettle is down to into normal temperature, polyether sulfone suspension is put into strong in the colloid mill with shearing grinding function
System dispersion, the rotating speed 4500rpm of colloid mill, Forced Dispersion is initially added into the precipitating liquid for having compounded after 5 minutes, when precipitating liquid is added
Continue afterwards to stir 25 minutes, you can obtain the white mixed serum of complete precipitating.
Mixed serum is put in distillation still, be heated to 65 DEG C distillation 3 hours after all reclaim organic solvent, that is, consolidated
Content (solid content：The mass fraction of solid part i.e. in polyether sulfone dispersion liquid) be 20% water-based polyether sulfone dispersion liquid, polyether sulfone
Mean particle size is 1.2 microns, 0.2～2 micron of particle size distribution range, polyether sulfone dispersion particle electromicroscopic photograph such as Fig. 1
It is shown.
The preparation (method of the present invention) of the water-based polyether sulfone dispersion liquid of embodiment 2
By taking the reactor of 100L as an example, by following quality raw material are prepared：It is polyethersulfone resin (8Kg), chloroform (32Kg), heavy
Analysis liquid (40Kg, wherein chloroform account for 10Kg, deionized water and account for 30Kg).
Above-mentioned recipe ingredient is distinguished into correct amount, to the 100L reactors with water knockout drum, agitator and heater
Middle addition polyethersulfone resin (8Kg) and chloroform (32Kg), open stirring, and reactor is heated to 50 DEG C, and stirring is gathered after 5 hours
Ether sulfone suspension.
Again temperature of reaction kettle is down to into normal temperature, polyether sulfone suspension is put into strong in the colloid mill with shearing grinding function
System dispersion, the rotating speed 4500rpm of colloid mill, Forced Dispersion is initially added into the precipitating liquid for having compounded after 6 minutes, when precipitating liquid is added
Continue afterwards to stir 20 minutes, you can obtain the white mixed serum of complete precipitating.
Mixed serum is put in distillation still, be heated to 65 DEG C distillation 3 hours after all reclaim organic solvent, that is, consolidated
Content is 21% water-based polyether sulfone dispersion liquid, and polyethersulfone granules average grain diameter is 1.5 microns, and particle diameter distribution 0.2～2.5 is micro-
Rice.
The preparation (method of the present invention) of the water-based polyether sulfone dispersion liquid of embodiment 3
By taking the reactor of 100L as an example, by following quality raw material are prepared：Polyethersulfone resin (8Kg), tetrahydrofuran
(40Kg), precipitating liquid (56Kg, wherein tetrahydrofuran account for 18Kg, deionized water and account for 38Kg).
Above-mentioned recipe ingredient is distinguished into correct amount, to the 100L reactors with water knockout drum, agitator and heater
Middle addition polyethersulfone resin (8Kg) and tetrahydrofuran (40Kg), open stirring, and reactor is heated to 70 DEG C, and stirring is obtained after 6 hours
Obtain polyether sulfone suspension.
Again temperature of reaction kettle is down to into normal temperature, polyether sulfone suspension is put into strong in the colloid mill with shearing grinding function
System dispersion, the rotating speed 4500rpm of colloid mill, Forced Dispersion is initially added into the precipitating liquid for having compounded after 5 minutes, when precipitating liquid is added
Continue afterwards to stir 29 minutes, you can obtain the white mixed serum of complete precipitating.
Mixed serum is put in distillation still, be heated to 70 DEG C distillation 3 hours after all reclaim organic solvent, that is, consolidated
Content is 17.4% water-based polyether sulfone dispersion liquid, and polyethersulfone granules average grain diameter is 1.1 microns, 0.2～2 micron of particle diameter distribution.
The preparation (conventional wet polishing) of the water-based polyether sulfone dispersion liquid of comparative example 1.
Polyether sulfone powder is carried out into lasting water mill more than 48h together with water using levigator, polyether sulfone dispersion liquid is obtained, should
Polyether sulfone dispersion particle electromicroscopic photograph is as shown in fig. 2, it can be seen that the polyether sulfone discrete particles particle diameter is big, be distributed wide and shape
Shape differs.
The stability test of embodiment 4, test water-based polyether sulfone solid content used is 20%.
Polyether sulfone dispersion liquid is measured into 100ML to be put in conical flask, 1 time-of-week is stood, it is as a result as shown in the table.
| Polyether sulfone dispersion liquid | Standing time (1 week) | Yellowing | Lamination |
| Embodiment 1 | Microprecipitation | Non yellowing | Without layering |
| Embodiment 2 | Microprecipitation | Non yellowing | Without layering |
| Embodiment 3 | Microprecipitation | Non yellowing | Without layering |
| Comparative example 1 | A large amount of precipitations | Xanthochromia | Layering |
| Solvent volatile diffusion method | Microprecipitation | Xanthochromia | Without layering |
Claims (10)
1. the preparation method of water-based polyether sulfone dispersion liquid, it is characterised in that prepare as follows,
(1) by polyether sulfone and organic solvent in mass ratio 1:4～5 mixing, stir 4～6 hours at a temperature of 50～70 DEG C, obtain
Polyether sulfone suspension；
(2) after by the cooling of polyether sulfone suspension, disperse 4～8min, be 1 by polyether sulfone and precipitating liquid mass ratio:5～7 additions are heavy
Analysis liquid, continues to disperse 20～30min, obtains white mixed serum；The precipitating liquid is that organic solvent presses quality with deionized water
Than 1:The liquid of 2～3 mixing；
(3) white mixed serum is distilled, water-based polyether sulfone dispersion liquid is obtained；
Wherein, organic solvent described in step (1) and (2) is chloroform or tetrahydrofuran, and organic solvent used by step (1) (2) is
It is same.
2. the preparation method of water-based polyether sulfone dispersion liquid according to claim 1, it is characterised in that in step (1), polyethers
Sulfone and organic solvent in mass ratio 1:5 mixing.
3. the preparation method of water-based polyether sulfone dispersion liquid according to claim 1 and 2, it is characterised in that in step (1),
After polyether sulfone mixes with organic solvent, stir at a temperature of 60 DEG C.
4. the preparation method of the water-based polyether sulfone dispersion liquid according to any one of claims 1 to 3, it is characterised in that step
(2) in, scattered mode is for shearing and grinds.
5. the preparation method of the water-based polyether sulfone dispersion liquid according to any one of Claims 1 to 4, it is characterised in that step
(2) in, Forced Dispersion is carried out using the dispersing apparatus with shearing grinding function, dispersing apparatus rotating speed is not less than 3000rpm, excellent
Dispersing apparatus rotating speed is selected to be at least 4500rpm.
6. the preparation method of the water-based polyether sulfone dispersion liquid according to any one of Claims 1 to 5, it is characterised in that step
(2) in, after dispersion 5min precipitating liquid is added.
7. the preparation method of the water-based polyether sulfone dispersion liquid according to any one of claim 1～6, it is characterised in that step
(2) in, precipitating liquid is organic solvent and deionized water in mass ratio 1:The liquid of 2 mixing.
8. the preparation method of the water-based polyether sulfone dispersion liquid according to any one of claim 1～7, it is characterised in that step
(2) in, polyether sulfone is 1 with precipitating liquid mass ratio:6.
9. the preparation method of the water-based polyether sulfone dispersion liquid according to any one of claim 1～8, it is characterised in that step
(3) in, distill to 65～70 DEG C of recovery organic solvents；It is preferred that distilling to 65～66 DEG C of recovery organic solvents.
10. a kind of water-based polyether sulfone dispersion liquid, it is characterised in that by the water-based polyether sulfone dispersion liquid described in claim 1～9
Method is obtained.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114232129A (en) * | 2021-12-21 | 2022-03-25 | 包头稀土研究院 | Polyether sulfone fiber and preparation method and application thereof |
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| CN101302335A (en) * | 2008-06-25 | 2008-11-12 | 吉林大学 | Bisphenol A type polyaromatic ether ketone water-based fluid dispersion and preparation thereof |
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2017
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| CN101302335A (en) * | 2008-06-25 | 2008-11-12 | 吉林大学 | Bisphenol A type polyaromatic ether ketone water-based fluid dispersion and preparation thereof |
| CN103881118A (en) * | 2014-04-06 | 2014-06-25 | 吉林大学 | Preparation method of redispersible polyether sulphone micro powder |
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| 张守国: "《水基聚醚砜分散液与可再分散性聚醚砜微粉的制备》", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114232129A (en) * | 2021-12-21 | 2022-03-25 | 包头稀土研究院 | Polyether sulfone fiber and preparation method and application thereof |
| CN114232129B (en) * | 2021-12-21 | 2023-06-16 | 包头稀土研究院 | Polyether sulfone fiber and preparation method and application thereof |
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