CN108102502A - A kind of preparation method of water-soluble poly ether ether ketone coating - Google Patents
A kind of preparation method of water-soluble poly ether ether ketone coating Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09D161/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/02—Condensation polymers of aldehydes or ketones with phenols only of ketones
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Abstract
The invention belongs to polyetheretherketonematerials materials fields, specifically disclose a kind of preparation method of water-soluble poly ether ether ketone coating, comprise the following steps：(1) polyether-ether-ketone synthesizes, prepared by (2) dispersion liquid, and prepared by (3) aqueous solution, (4) remove solvent, (5) application, crosslinking.Water-soluble poly ether ether ketone coating is prepared in the present invention, it can keep stablizing in aqueous dispersion for a long time, coating system viscosity can be mutually adjusted by simple water, any auxiliary agent need not be added, it in use can be according to the requirement of different operating modes and environment, it is flexibly constructed to coating layer thickness, i.e. available " touching dry " coating, reduces the absorption of dust and the repairing of defect in the short period of time.
Description
Technical field
The invention belongs to polyetheretherketonematerials materials fields, specifically disclose a kind of preparation method of water-soluble poly ether ether ketone coating.
Background technology
With the high speed development of world economy, requirement of the people to material property is higher and higher, and polyether-ether-ketone is excellent with its
Comprehensive performance favored be subject to people, polyether-ether-ketone is succeeded in developing by ICI Imperial Chemical Industries of Britain in the seventies in last century, make
For a kind of hemicrystalline high molecular material have temperature classification height, radiation hardness, chemical-resistant resistance, endurance, impact resistance, resist it is compacted
The comprehensive performances such as change, wear-resisting, hydrolytic resistance, anti-flammability and excellent electrical properties, thus quickly Aeronautics and Astronautics, nuclear energy, information,
The application that the high-tech sectors such as communication, electronics, petrochemical industry, machinery, traffic are succeeded, so that the traditional product of many industries is real
Update is showed.
An important applied field of the polyether-ether-ketone series polymer coating as high molecular material, developed very in recent years
Rapidly.The discharge of volatile organic compounds in traditional solvent based coating be all to environmental and human health impacts it is harmful, because
This many country carrys out the use limitation of the harmful organic solvent in specification coating in the form of law, for a certain extent
It solves the emission problem of above-mentioned volatile organic compounds, develops the water paint of low stain environment-friendly type, powdery paints and without molten
Agent coating has become one of Main way of coating research and development.
For polyether-ether-ketone, the technology of exploitation water soluble paint most critical is to prepare water-soluble poly ether ether ketone dispersion liquid
Or the polymer micro mist of redispersible, the water solubility of polymer are exactly that polymer is made to be scattered in aqueous medium in the form of particle
In, since existing polyether-ether-ketone chemical property is extremely stable, common organic solvent is not dissolved in, this is just allowed to the field applied
It is restricted.
The content of the invention
In view of the above problems, the present invention provides a kind of preparation method of water-soluble poly ether ether ketone coating.
Technical scheme is as follows：
A kind of preparation method of water-soluble poly ether ether ketone coating, comprises the following steps：
(1) polyether-ether-ketone synthesizes：
4,4- difluoro benzophenones, bisphenol-A, hydroquinone, sodium carbonate, dimethyl sulfoxide (DMSO), nitrogen are added in into reactor
Heating is proceeded by after being continually fed into 100~120min；2~3 DEG C/min of heating rate, is warming up to 150 DEG C, and constant temperature 80~
90min after material is completely dissolved in system, is opened and is persistently stirred, 10~15r/min of stir speed (S.S.)；Again by body
It is that temperature is warming up to 200~205 DEG C, constant temperature stirs 240~360min；After complete reaction, post-process spare；
The substance proportioning of above-mentioned reaction is as follows：In terms of parts by weight, 4,4- difluoro benzophenones：10~15 parts, bisphenol-A：5
~10 parts, hydroquinone：1~5 part, sodium carbonate：2~4 parts, dimethyl sulfoxide (DMSO)：65~75 parts.
The post processing is to import the material system after the reaction was complete in cold water to cool down, and is cured, then through ethyl alcohol
And deionized water is washed repeatedly；It is dry at last vacuum dried 100~110 DEG C of case, it is cooled to room temperature；
Step (1) reaction equation is as follows：
(2) prepared by dispersion liquid：
By treated in step (1), particle is crushed to 100~110 microns through high speed disintegrator, by above-mentioned micro powder granule,
Sebacic acid dibutyl ester is dissolved in chloroform, methanol, mixed liquor is disperseed, obtains dispersion liquid；
The substance proportioning of above-mentioned reaction is as follows：In terms of parts by weight, micro powder granule：5~15 parts, sebacic acid dibutyl ester (increases
Mould agent)：1~2 part, chloroform：65~85 parts, methanol：5~10 parts.
Dispersion steps the control 8000~10000rpm of rotating speed, 180~210min of jitter time.
(3) prepared by aqueous solution：
Dispersion liquid obtained in step (2) is put into containing sodium alkyl benzene sulfonate, polyacrylamide, crassitude
In ketone, pure water, mixing is scattered；
Dispersion steps the control 8000~10000rpm of rotating speed, 180~210min of jitter time.
The substance proportioning of above-mentioned reaction is as follows：In terms of parts by weight, dispersion liquid obtained in step (2)：45~55 parts；Alkane
Base benzene sulfonic acid sodium salt (surfactant)：1~2 part, polyacrylamide (thickener)：1~2 part, methyl pyrrolidone (levelling agent)：
2~3 parts, pure water：45~55 parts.
(4) solvent is removed
Aqueous solution in step (3) is put into reactor, 55~65 DEG C is warming up to and continues 360~420min, and hold
It is continuous to be passed through nitrogen, for eliminating the evaporation of bubble and organic solvent；
(5) application, crosslinking
Step (4) solution is subjected to application, using ultraviolet curing lamp 10~20min of prolonged exposure, finally can be prepared by gathering
Ether ether ketone water soluble paint overlay film.
300~the 400nm of ultraviolet wavelength.
Reactor described in step (1) and (4) is equipped with mechanical agitation, thermometer, three mouthfuls of burnings of condensate recycling device
Bottle.
It is as follows to cure crosslinking A types, Type B, c-type chemical structural formula：
In step (1), after bisphenol-A, hydroquinone collective effect, polyether-ether-ketone backbone structure is accessed, is drawn by bisphenol-A
Enter double methyl of high hydridization degree, while the effect of double-strand winding occurs in the side-chain radical introduced in main chain, destroys original
The characteristic of polyether-ether-ketone stabilized structure, while occur different changes in the indexs such as glass transition temperature, melting temperature,
It is allowed to possessed certain soluble-type；
The effect that sebacic acid dibutylester substance plays the plasticising of room temperature physics is added in step (2), can be effectively attached to
On the product of step (1), make what the product of step (1) was more uniformly distributed to be dispersed in the mixed solution of chloroform and methanol, it is right
The product of step (1) carries out organic phased soln；The reason for selection chloroform, the blend solution of methanol are dissolved is to utilize three
Chloromethanes, methanol solvate low boiling point, it is highly polar the characteristics of, can be dissolved to greatest extent, while step (4) removes solvent
Process it is relatively quick；
Step (3) is through sodium alkyl benzene sulfonate (surfactant), polyacrylamide by the blend solution in step (2)
After the blending of (thickener), methyl pyrrolidone (levelling agent), it is dispersed in pure water, sodium alkyl benzene sulfonate used has
The effect of enhancing material surface-active makes the blend solution in step (2) have better hydrophily and wellability；Polyacrylamide
Amine is thickener, and viscosity of mixed liquid is relatively low in step (2), and mobility is splendid, is unsuitable for forming a film, thus add in polyacrylamide with
Prepare the film product of different-thickness specification；Methyl pyrrolidone plays the role of levelling, when step (3) solution viscosity increases
Afterwards, mobility significantly weakens, and occurs the problems such as partial drape, blistering, cracking in film forming procedure, adds in methyl pyrrolidone
After can effectively solve the above problems；The diluent selected is to avoid introducing impurity metal ion, metal for the main purpose of pure water
Being introduced into for ionic impurity can cure the ultraviolet-crosslinkable in step (5) generation harmful effect.
The main function of step (4) is that the blend solution in step (3) is removed organic solvent through low-temperature evaporation, is made final
Product is water based paint；
The most important effect of film-forming process in step (5) is exactly according to actual needs, solution to be made given size
Film, wherein ultraviolet curing are film forming final steps, and hardening time and ultraviolet wavelength have provided control range, ultraviolet waves
In 300~400nm, ultraviolet wavelength is drawn according to the bond energy of ketonic bond in product, bisphenol-A methyl for long control, at this wavelength,
Maximum crosslinking rate can be reached.After ultraviolet wavelength changes, substance can not generate crosslinked action, final nothing in solution
Method achievees the purpose that film forming, and the too short film strength that can also lead to the problem of of irradiation time is relatively low, if irradiation time is long, works as crosslinking
After the reaction was complete, i.e., it can generate the waste of the energy.
Side group or flexible bond (side group and double-strand of structure of bisphenol A) are introduced into polymer by the present invention, so as to destroy chain
Regularity and crystallinity, final be made maintain the original performance of the material polyether-ether-ketone product with good solubility again,
Introducing crosslinked point (methyl introduced for ketonic bond, bisphenol-A) in polyetheretherketonematerials materials, high-performance is obtained by forming cross-linked structure
Material improves solidification rate, after ultraviolet irradiation, generates cross-linking reaction, water-soluble poly is prepared in final curing molding
Ether ether ketone coating, the polyether-ether-ketone coating can keep stability in aqueous dispersion for a long time, and coating system viscosity can pass through
Simple water is mutually adjusted, without adding any auxiliary agent, in use can according to the requirement of different operating modes and environment,
It is flexibly constructed to coating layer thickness, in the short period of time i.e. available " touching dry " coating, reduces absorption and the defect of dust
Repairing.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is described in further detail.It should be appreciated that specific embodiment described herein does not limit only to explain the present invention
In the present invention.
Embodiment 1：
1st, synthesize
10 parts of 4,4- difluorodiphenyls are added in the 3L three-necked flasks protected equipped with mechanical agitation, thermometer, high pure nitrogen
Ketone, 6 parts of bisphenol-As, 5 parts of hydroquinones, 4 parts of sodium carbonate, 75 parts of dimethyl sulfoxide (DMSO)s, nitrogen be continually fed into after 120min start into
Row heating；3 DEG C/min of heating rate is warming up to 150 DEG C, constant temperature 90min, after material is completely dissolved in system, opens and holds
It is continuous to be stirred, stir speed (S.S.) 15r/min；System temperature is warming up to 200 DEG C again, constant temperature stirring 300min；It waits to have reacted
Material in system is imported in cold water and cooled down by Quan Hou, is cured, then is washed repeatedly through ethyl alcohol and deionized water；Most afterwards through true
It is dry at empty 100 DEG C of drying box, it is cooled to room temperature spare；
2nd, prepared by dispersion liquid
Through high speed disintegrator, 100 μm will be crushed to by dry particle after cooling in step 1, by above-mentioned 15 parts of micro powder granule,
1 part of sebacic acid dibutyl ester (plasticizer), is dissolved in 74 parts of chloroforms, in 10 parts of methanol, is carried out mixed liquor using colloid mill
Forced Dispersion, rotating speed 10000rpm, jitter time 180min；
3rd, prepared by aqueous solution
By 45 parts of dispersion liquid obtained in step 2, put into containing sodium alkyl benzene sulfonate 1 part (surfactant), poly- third
Acrylamide 2 parts (thickeners), methyl pyrrolidone 3 parts (levelling agents), in 49 parts of pure water, through colloid mill Forced Mixing, rotating speed
10000rpm, jitter time 180min；
4th, solvent is removed
By the aqueous solution in step 3 put into equipped with stirring, thermometer, condensate recycling device three-necked flask in, heat up
To 65 DEG C of lasting 360min, and nitrogen is continually fed into, for eliminating the evaporation of bubble and organic solvent；
5th, application, crosslinking
Carry out application on the glass sheet using the mode of curtain coating naturally, and can repeated multiple times application, ultraviolet curing lamp is ultraviolet
Line wavelength 400nm, prolonged exposure 10min finally can be prepared by the polyether-ether-ketone water solubility coating film with excellent properties.
Embodiment 2：
1st, synthesize
15 parts of 4,4- difluorodiphenyls are added in the 3L three-necked flasks protected equipped with mechanical agitation, thermometer, high pure nitrogen
Ketone, 10 parts of bisphenol-As, 5 parts of hydroquinones, 4 parts of sodium carbonate, 66 parts of dimethyl sulfoxide (DMSO)s, nitrogen start after being continually fed into 120min
It heats up；3 DEG C/min of heating rate is warming up to 150 DEG C, constant temperature 90min, after material is completely dissolved in system, opens simultaneously
It is persistently stirred, stir speed (S.S.) 15r/min；System temperature is warming up to 200 DEG C again, constant temperature stirring 300min；It waits to react
After completely, material in system is imported in cold water and is cooled down, cured, then washed repeatedly through ethyl alcohol and deionized water；Most pass through afterwards
It is dry at 100 DEG C of vacuum drying chamber, it is cooled to room temperature spare；
2nd, prepared by dispersion liquid
Through high speed disintegrator, 100 μm will be crushed to by dry particle after cooling in step 1, by above-mentioned 10 parts of micro powder granule,
2 parts of sebacic acid dibutyl esters (plasticizer), are dissolved in 78 parts of chloroforms, in 10 parts of methanol, are carried out mixed liquor using colloid mill
Forced Dispersion, rotating speed 10000rpm, jitter time 180min；
3rd, prepared by aqueous solution
By 48 parts of dispersion liquid obtained in step 2, put into containing sodium alkyl benzene sulfonate 2 parts (surfactants), poly- third
Acrylamide 2 parts (thickeners), methyl pyrrolidone 3 parts (levelling agents), in 45 parts of pure water, through colloid mill Forced Mixing, rotating speed
10000rpm, jitter time 180min；
4th, solvent is removed
By the aqueous solution in step 3 put into equipped with stirring, thermometer, condensate recycling device three-necked flask in, heat up
To 65 DEG C of lasting 360min, and nitrogen is continually fed into, for eliminating the evaporation of bubble and organic solvent；
5th, application, crosslinking
Carry out application on the glass sheet using the mode of curtain coating naturally, and can repeated multiple times application, ultraviolet curing lamp is ultraviolet
Line wavelength 400nm, prolonged exposure 10min finally can be prepared by the polyether-ether-ketone water solubility coating film with excellent properties.
Embodiment 3：
1st, synthesize
14 parts of 4,4- difluorodiphenyls are added in the 3L three-necked flasks protected equipped with mechanical agitation, thermometer, high pure nitrogen
Ketone, 9 parts of bisphenol-As, 5 parts of hydroquinones, 4 parts of sodium carbonate, 68 parts of dimethyl sulfoxide (DMSO)s, nitrogen be continually fed into after 120min start into
Row heating；3 DEG C/min of heating rate is warming up to 150 DEG C, constant temperature 90min, after material is completely dissolved in system, opens and holds
It is continuous to be stirred, stir speed (S.S.) 15r/min；System temperature is warming up to 200 DEG C again, constant temperature stirring 300min；It waits to have reacted
Material in system is imported in cold water and cooled down by Quan Hou, is cured, then is washed repeatedly through ethyl alcohol and deionized water；Most afterwards through true
It is dry at empty 100 DEG C of drying box, it is cooled to room temperature spare；
2nd, prepared by dispersion liquid
Through high speed disintegrator, 100 μm will be crushed to by dry particle after cooling in step 1, by above-mentioned 5 parts of micro powder granule, 2
Part sebacic acid dibutyl ester (plasticizer), is dissolved in 83 parts of chloroforms, in 10 parts of methanol, is carried out mixed liquor using colloid mill strong
System is scattered, rotating speed 10000rpm, jitter time 180min；
3rd, prepared by aqueous solution
By 47 parts of dispersion liquid obtained in step 2, put into containing sodium alkyl benzene sulfonate 2 parts (surfactants), poly- third
Acrylamide 2 parts (thickeners), methyl pyrrolidone 3 parts (levelling agents), in 46 parts of pure water, through colloid mill Forced Mixing, rotating speed
10000rpm, jitter time 180min；
4th, solvent is removed
By the aqueous solution in step 3 put into equipped with stirring, thermometer, condensate recycling device three-necked flask in, heat up
To 65 DEG C of lasting 360min, and nitrogen is continually fed into, for eliminating the evaporation of bubble and organic solvent；
5th, application, crosslinking
Application is carried out on the glass sheet using the mode of curtain coating naturally, and can repeated multiple times application.Ultraviolet curing lamp is ultraviolet
Line wavelength 400nm, prolonged exposure 10min finally can be prepared by the polyether-ether-ketone water solubility coating film with excellent properties.
Comparative example：
Commercial product does not have any dissolubility at this stage, while hygroscopicity is relatively low, rotten to most of strong acid, alkali
It can be used steadily in the long term under conditions of erosion, chemical property is extremely stable, it is difficult to be dissolved, mainly dissolubility is compared in following table
It is right.
Table 1：The performance data table of coating prepared by embodiment and comparative example
Claims (8)
1. a kind of preparation method of water-soluble poly ether ether ketone coating, it is characterised in that：Comprise the following steps：
(1) polyether-ether-ketone synthesizes：
Add in 4,4- difluoro benzophenones into reactor, bisphenol-A, hydroquinone, sodium carbonate, dimethyl sulfoxide (DMSO), nitrogen is lasting
Heating is proceeded by after being passed through 100~120min；2~3 DEG C/min of heating rate, is warming up to 150 DEG C, and 80~90min of constant temperature is treated
After material is completely dissolved in system, opens and be persistently stirred, 10~15r/min of stir speed (S.S.)；Again by system temperature liter
For temperature to 200~205 DEG C, constant temperature stirs 240~360min；After complete reaction, post-process spare；
(2) prepared by dispersion liquid：
By treated in step (1), particle is crushed to 100~110 microns through high speed disintegrator, by above-mentioned micro powder granule, certain herbaceous plants with big flowers two
Dibutyl phthalate is dissolved in chloroform, methanol, mixed liquor is disperseed, obtains dispersion liquid；
(3) prepared by aqueous solution：
By dispersion liquid obtained in step (2), put into and contain sodium alkyl benzene sulfonate, polyacrylamide, methyl pyrrolidone, pure
In water, mixing is scattered；
(4) solvent is removed
Aqueous solution in step (3) is put into reactor, 55~65 DEG C is warming up to and continues 360~420min, and persistently lead to
Enter nitrogen；
(5) application, crosslinking
Step (4) solution is subjected to application, using ultraviolet curing lamp 10~20min of prolonged exposure, polyether-ether-ketone water is finally made
Soluble paint overlay film.
2. a kind of preparation method of water-soluble poly ether ether ketone coating according to claim 1, it is characterised in that：Step (1)
The substance proportioning of middle reaction is as follows：In terms of parts by weight, 4,4- difluoro benzophenones：10~15 parts, bisphenol-A：It is 5~10 parts, right
Benzenediol：1~5 part, sodium carbonate：2~4 parts, dimethyl sulfoxide (DMSO)：65~75 parts.
3. a kind of preparation method of water-soluble poly ether ether ketone coating according to claim 1, it is characterised in that：Step (1)
Described in post processing be to import the material system after the reaction was complete in cold water to cool down, cure, then through ethyl alcohol and go from
Sub- water washs repeatedly；It is dry at last vacuum dried 100~110 DEG C of case, it is cooled to room temperature.
4. a kind of preparation method of water-soluble poly ether ether ketone coating according to claim 1, it is characterised in that：Step (2)
The substance proportioning of middle reaction is as follows：In terms of parts by weight, micro powder granule：5~15 parts, sebacic acid dibutyl ester：1~2 part, three chloromethanes
Alkane：65~85 parts, methanol：5~10 parts.
5. a kind of preparation method of water-soluble poly ether ether ketone coating according to claim 1, it is characterised in that：Step (2)
(3) dispersion steps control 8000~10000rpm of rotating speed, 180~210min of jitter time described in.
6. a kind of preparation method of water-soluble poly ether ether ketone coating according to claim 1, it is characterised in that：Step (3)
The substance proportioning of middle reaction is as follows：In terms of parts by weight, dispersion liquid obtained in step (2)：45~55 parts；Alkyl benzene sulphonate
Sodium：1~2 part, polyacrylamide：1~2 part, methyl pyrrolidone：2~3 parts, pure water：45~55 parts.
7. a kind of preparation method of water-soluble poly ether ether ketone coating according to claim 1, it is characterised in that：Step (5)
Described in 300~400nm of ultraviolet wavelength.
8. a kind of preparation method of water-soluble poly ether ether ketone coating according to claim 1, it is characterised in that：Step (1)
(4) reactor described in is equipped with mechanical agitation, thermometer, the three-necked flask of condensate recycling device.
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| CN114989416A (en) * | 2022-06-14 | 2022-09-02 | 中国科学院长春应用化学研究所 | Polyaryletherketone heat-shrinkable material and preparation method thereof |
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| CN108102502B (en) | 2020-06-05 |
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