CN105153439B - A kind of preparation method of polyarylether polymer aqueous-based dispersions - Google Patents
A kind of preparation method of polyarylether polymer aqueous-based dispersions Download PDFInfo
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- CN105153439B CN105153439B CN201510430234.4A CN201510430234A CN105153439B CN 105153439 B CN105153439 B CN 105153439B CN 201510430234 A CN201510430234 A CN 201510430234A CN 105153439 B CN105153439 B CN 105153439B
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- aqueous
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- based dispersions
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Abstract
A kind of preparation method of polyarylether polymer aqueous-based dispersions, belongs to technical field of polymer materials.Be by mass ratio be 8~16：100 polyarylether polymer and organic solvent is added in reaction vessel, in the case where nitrogen is protected and is stirred, and is heated to 120~270 DEG C, is incubated 10~30 minutes, is cooled to 20 DEG C~20 DEG C and obtain solid product；In the aqueous surfactant solution that solid product is poured into 0 DEG C~20 DEG C, then crushed, so as to obtain the aqueous-based dispersions of polyarylether polymer.Preparation method of the present invention is simple, stably, it is easy, and do not need the extreme conditions such as liquid nitrogen frozen.Polyarylether aqueous-based dispersions can be used as the varnish of polyarylether coating, and the preparation method of traditional polyarylether dispersion liquid is added in aqueous phase for mechanical crushing superfine powder, prepares aqueous-based dispersions.Is polymer gel is made in polyarylether by the method for invention, and the gel hardness is small, it is easy to scattered, it is to avoid the drawbacks of traditional liquid nitrogen cold machinery is crushed.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of system of polyarylether polymer aqueous-based dispersions
Preparation Method.
Background technology
Polyarylether polymer refers to the special engineering plastics such as PAEK and polyether sulphone.Polyarylether polymer relies on
Its excellent physical and mechanical properties, hot property, electrical property and chemical property, make it in electronic apparatus, machinery instrument, traffic fortune
The fields such as defeated and aerospace are widely used.Polyarylether class material can be used with variforms such as film, fiber and coatings.
Used as coating and can be applied to the fields such as chemical anticorrosion, food, medical treatment, machinery and oil.
Polyarylether polymer can be divided into two major classes according to dissolubility：Soluble poly aromatic ether, non-solubility polyarylether.It is solvable
Property polyarylether polymer refers to be dissolved in common organic solvents, such as chloroform, N-N- dimethylformamides etc..This kind of material can be with
With solution spraying or powder spray.Non-solubility polyarylether refers to the polyarylether polymer insoluble in conventional organic solvent, should
Class polyarylether polymer typically uses powder spray technology.Powder spray can be electrostatically sprayed, and can also use aqueous dispersion
Liquid.Relative to powder spray, aqueous-based dispersions, which can be sprayed, prepares very thin film.
The preparation of polyether sulfone and bisphenol A type polyaromatic ether ketone water-based fluid dispersion, ZL20081005088.0 and
In ZL20051001665.4 it has been reported that.This kind of method is to be dissolved in the polyether sulfone or bisphenol A type polyaromatic ether ketone of preparation
Machine solvent, is added after water and surfactant-dispersed, and stirring, which steams organic solvent, can prepare aqueous-based dispersions.Polyether-ether-ketone
Aqueous-based dispersions can also be dispersed in the water containing surfactant using superfine powder.Polyether-ether-ketone superfine powder is usually with ultralow
Superfine powder prepared by the crushing technologies such as the gentle mill of temperature cooling ball milling.Chinese patent ZLCN201410381914 reports a kind of high temperature
Spheronization techniques of the fluid bed to superfine powder.At present, simple instrument and equipment efficient pulverizing polyarylether resin also is utilized without a kind of,
The method for preparing polyarylether aqueous-based dispersions.
The content of the invention
The mesh of the present invention is to provide a kind of preparation method of polyarylether polymer aqueous-based dispersions, method is simple, stably,
It is easy, and do not need the extreme conditions such as liquid nitrogen frozen.The present invention utilizes double dispersions of solvent miscible with water, dispersion liquid system
Standby more to stablize, polyarylether polymer and organic solvent form solvent-borne type gel at low temperature, and the gel tissue is soft, it is easy to
Disperse in the aqueous solution.
Polyarylether aqueous-based dispersions can be used as the varnish of polyarylether coating, the preparation side of traditional polyarylether dispersion liquid
Method is that mechanical crushing polyarylether superfine powder is added in aqueous phase, prepares aqueous-based dispersions.The inventive method is by polyarylether system
Into polymer gel, the gel hardness is small, and intermolecular force is small, it is easy to scattered, it is to avoid traditional liquid nitrogen frozen machinery is crushed
The drawbacks of.With common disintegrating apparatus, you can obtain less powder particle.
Polyarylether polymer of the present invention, its structure is as follows：
Wherein X can be following molecular structure, but be not specific to following molecular structure：
Wherein Y can be following structure, but be not specific to following molecular structure：
N is positive integer, represents the degree of polymerization.
The preparation of polyarylether polymer aqueous-based dispersions of the present invention, be by mass ratio be 8~16：100 it is poly-
Fragrant ether polymer and organic solvent are added in reaction vessel, in the case where nitrogen is protected and is stirred, are heated to 120~270 DEG C, into
After uniform solution, 10~30 minutes are incubated, then cools to -20 DEG C~20 DEG C and obtains solid product；By solid product
Pour into 0~20 DEG C of aqueous surfactant solution, then carry out powder using reducing mechanisms such as tissue mashing machine or colloid mills
It is broken, so as to obtain the aqueous-based dispersions of polyarylether polymer；
Wherein, organic solvent is one or more combinations in dichloroacetic acid, m-Chlorophenol and Pentafluorophenol, but is not specific to
This several solvent.The mass concentration of aqueous surfactant solution is 1 × 10-4~3 × 10-4Grams per milliliter, surfactant includes
But it is not specific to neopelex, polyvinyl alcohol；Polyarylether polymer and the quality of aqueous surfactant solution reclaimed water
Than for 4~8：100.
Embodiment
Embodiment 1：
By polyether sulfone20.00g and m-Chlorophenol 180.00g are added to equipped with mechanical agitation, temperature
In the there-necked flask of meter, 120 DEG C, after dissolving are heated under nitrogen protection, stirs 30 minutes, under agitation, closes heating, cooling drop
Temperature, when temperature is reduced to 10 DEG C, solid product is poured into 360g, 10 DEG C of sodium dodecyl benzene sulfonate aqueous solution.Dodecane
The mass concentration of the aqueous solution of base benzene sulfonic acid sodium salt is a ten thousandth.Add mixture to tissue mashing machine, 900 revs/min of rotating speed
Clock, obtains the polyether sulfone aqueous-based dispersions that mesh number is 80 mesh, mass concentration is 3.6% after crushing 10min.
Embodiment 2：
By polyether-ether-ketone20.00g and m-Chlorophenol 180.00g be added to equipped with mechanical agitation,
In the there-necked flask of thermometer, nitrogen protection is heated to 180 DEG C, after dissolving, stir 20 minutes, under agitation, close heating, it is cold
But cool, when temperature is 10 DEG C, product is poured into 360g, 10 DEG C of sodium dodecyl benzene sulfonate aqueous solution.Dodecyl
The mass concentration of the aqueous solution of benzene sulfonic acid sodium salt is 1 × 10-4Grams per milliliter.Add mixture to tissue mashing machine, 900 turns of rotating speed/
Minute, the polyether-ether-ketone aqueous-based dispersions that mesh number is 80 are obtained after crushing 10min, concentration is 3.6%.
Embodiment 3：
By polyether-ether-ketone20.00g and Pentafluorophenol 180.00g are added to and stirred equipped with machinery
Mix, in the there-necked flask of thermometer, nitrogen protection is heated to 210 DEG C, after being completely dissolved, stir 15 minutes, under agitation, close
Heating, is cooled, and when temperature is 10 DEG C, product is poured into 360g, 10 DEG C of sodium dodecyl benzene sulfonate aqueous solution.Ten
The mass concentration of the aqueous solution of dialkyl benzene sulfonic acids sodium is 1 × 10-4Grams per milliliter.Add mixture to tissue mashing machine, rotating speed
900 revs/min, the polyether-ether-ketone aqueous-based dispersions that mesh number is 80 mesh are obtained after crushing 10min, concentration is 3.6%.
Embodiment 4：
By polyether-ether-ketone20.00g and m-Chlorophenol 90.00g and Pentafluorophenol 90.00g, plus
Enter in equipped with mechanical agitation, the there-necked flask of thermometer, nitrogen protection is heated to 270 DEG C, after being completely dissolved, stirred 10 minutes,
Under agitation, heating is closed, is cooled, when temperature is 10 DEG C, product is poured into 360g 10 DEG C of detergent alkylate sulphur
In acid sodium aqueous solution.The mass concentration of the aqueous solution of neopelex is 1 × 10-4Grams per milliliter.Add mixture to
Tissue mashing machine, 900 revs/min of rotating speed obtains the polyether-ether-ketone aqueous-based dispersions that mesh number is 80 mesh, concentration after crushing 10min
It is 3.6%.
Embodiment 5：
By polyether-ether-ketone20.00g and m-Chlorophenol 180.00g be added to equipped with mechanical agitation,
In the there-necked flask of thermometer, nitrogen protection is heated to 180 DEG C, after being completely dissolved, and stirs 20 minutes, under agitation, closes and add
Heat, is cooled, and when temperature is 10 DEG C, product is poured into 360g, 10 DEG C of sodium dodecyl benzene sulfonate aqueous solution.12
The mass concentration of the aqueous solution of sodium alkyl benzene sulfonate is 1 × 10-4Grams per milliliter.Add mixture to colloid mill, rotating speed 4000
Rev/min, the polyether-ether-ketone aqueous-based dispersions that 270 mesh are obtained after 10min are crushed, concentration is 3.6%.
Embodiment 6：
By polyether-ether-ketone12.80g and m-Chlorophenol 160.00g be added to equipped with mechanical agitation,
In the there-necked flask of thermometer, nitrogen protection is heated to 180 DEG C, after being completely dissolved, and stirs 20 minutes, under agitation, closes and add
Heat, is cooled, and when temperature is 20 DEG C, product is poured into 360g, 10 DEG C of sodium dodecyl benzene sulfonate aqueous solution.12
The mass concentration of the aqueous solution of sodium alkyl benzene sulfonate is 3 × 10-4Grams per milliliter.Add mixture to colloid mill, rotating speed 4000
Rev/min, the polyether-ether-ketone aqueous-based dispersions that 230 mesh are obtained after 10min are crushed, concentration is 3.6%.
Embodiment 7：
By polyether-ether-ketone28.80g and m-Chlorophenol 180.00g be added to equipped with mechanical agitation,
In the there-necked flask of thermometer, nitrogen protection is heated to 180 DEG C, after being completely dissolved, and stirs 20 minutes, under agitation, closes and add
Heat, is cooled, and when temperature is -20 DEG C, product is poured into 360g, 0 DEG C of sodium dodecyl benzene sulfonate aqueous solution.12
The mass concentration of the aqueous solution of sodium alkyl benzene sulfonate is 3 × 10-4Grams per milliliter.Add mixture to colloid mill, rotating speed 4000
Rev/min, the polyether-ether-ketone aqueous-based dispersions that 325 mesh are obtained after 10min are crushed, concentration is 3.6%.
Claims (4)
1. a kind of preparation method of polyarylether polymer aqueous-based dispersions, it is characterised in that：Be by mass ratio be 8~16：100
Polyarylether polymer and organic solvent be added in reaction vessel, nitrogen protect and stir under, be heated to 120~270
DEG C, after being completely dissolved, 10~30 minutes are incubated, then cools to -20 DEG C~20 DEG C and obtains solid product；By solid product
Pour into 0~20 DEG C of aqueous surfactant solution, then crushed using tissue mashing machine or colloid mill reducing mechanism, from
And obtain the aqueous-based dispersions of polyarylether polymer；Organic solvent be dichloroacetic acid, m-Chlorophenol, Pentafluorophenol in one kind or
A variety of combinations.
2. a kind of preparation method of polyarylether polymer aqueous-based dispersions as claimed in claim 1, it is characterised in that：Poly- virtue
The structure of ether polymer is as follows,
Wherein X is compound shown in one of having structure,
Wherein Y is compound shown in one of having structure,
N is positive integer；Represent the degree of polymerization.
3. a kind of preparation method of polyarylether polymer aqueous-based dispersions as claimed in claim 1, it is characterised in that：Surface
The mass concentration of aqueous surfactant solutions is 1 × 10-4~3 × 10-4Grams per milliliter, surfactant be neopelex or
Polyvinyl alcohol.
4. a kind of preparation method of polyarylether polymer aqueous-based dispersions as claimed in claim 1, it is characterised in that：Poly- virtue
Ether polymer and the mass ratio of aqueous surfactant solution reclaimed water are 4~8：100.
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| CN201510430234.4A CN105153439B (en) | 2015-07-21 | 2015-07-21 | A kind of preparation method of polyarylether polymer aqueous-based dispersions |
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| CN106633104B (en) * | 2017-01-06 | 2020-11-03 | 自贡川滤设备制造有限公司 | Preparation method of water-based polyether sulfone dispersion liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663983A (en) * | 2005-03-25 | 2005-09-07 | 吉林大学 | Aqueous polyarylethersulphones dispersion liquid and process for preparing same |
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663983A (en) * | 2005-03-25 | 2005-09-07 | 吉林大学 | Aqueous polyarylethersulphones dispersion liquid and process for preparing same |
| 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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