CN108102502B - Preparation method of water-soluble polyether-ether-ketone coating - Google Patents
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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
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- 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 the field of polyether-ether-ketone materials, and particularly discloses a preparation method of a water-soluble polyether-ether-ketone coating, which comprises the following steps: (1) synthesizing polyether-ether-ketone, (2) preparing dispersion liquid, (3) preparing aqueous solution, (4) removing solvent, and (5) coating and crosslinking. The water-soluble polyether-ether-ketone coating prepared by the invention can be kept stable in a water dispersion system for a long time, the viscosity of the coating system can be adjusted through a pure water phase, no auxiliary agent is needed to be added, the coating thickness can be flexibly constructed according to the requirements of different working conditions and environments in the using process, a dry-to-touch coating can be obtained in a short time, and the dust adsorption and defect repair are reduced.
Description
Technical Field
The invention belongs to the field of polyether-ether-ketone materials, and particularly discloses a preparation method of a water-soluble polyether-ether-ketone coating.
Background
Along with the rapid development of world economy, the requirements of people on the material performance are higher and higher, polyetheretherketone is favored by people with excellent comprehensive performance, the polyetheretherketone is successfully developed by the empire chemical company of the great kingdom in the last 70 century, and the polyetheretherketone has the comprehensive performance of high heat resistance grade, radiation resistance, chemical resistance, fatigue resistance, impact resistance, creep resistance, wear resistance, hydrolysis resistance, flame resistance, excellent electrical performance and the like as a semi-crystalline polymer material, so the polyetheretherketone can be successfully applied to the high-technology fields of aviation, aerospace, nuclear energy, information, communication, electronics, petrifaction, machinery, traffic and the like, and the traditional products of many industries are updated.
The development of the polyether-ether-ketone series polymer coating as an important application field of a high polymer material is very rapid in recent years. The emission of volatile organic compounds in traditional solvent-based coatings is harmful to the environment and human health, so that the use limit of harmful organic solvents in the coatings is regulated by many countries in the form of laws, and in order to solve the emission problem of the volatile organic compounds to a certain extent, the development of low-pollution environment-friendly water-based coatings, powder coatings and solvent-free coatings is one of the main directions for the research and development of coatings.
In the case of polyetheretherketone, the most critical technique for developing a water-soluble coating is to prepare a water-soluble polyetheretherketone dispersion or a redispersible polymer fine powder, and the water solubility of the polymer is to disperse the polymer in a water medium in the form of fine particles, so that the application field of the polyetheretherketone is limited because the conventional polyetheretherketone has extremely stable chemical properties and is insoluble in common organic solvents.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a water-soluble polyether-ether-ketone coating.
The technical scheme of the invention is as follows:
a preparation method of a water-soluble polyether-ether-ketone coating comprises the following steps:
(1) polyether-ether-ketone synthesis:
adding 4, 4-difluorobenzophenone, bisphenol A, hydroquinone, sodium carbonate, dimethyl sulfoxide and nitrogen into a reactor, continuously introducing for 100-120 min, and then starting to heat; heating to 150 ℃ at a heating rate of 2-3 ℃/min, keeping the temperature for 80-90 min, starting and continuously stirring after materials in the system are completely dissolved, wherein the stirring rate is 10-15 r/min; raising the temperature of the system to 200-205 ℃ again, and stirring for 240-360 min at constant temperature; after the reaction is completed, post-treating for later use;
the material ratio of the reaction is as follows: 4, 4-difluorobenzophenone in parts by weight: 10-15 parts of bisphenol A: 5-10 parts of hydroquinone: 1-5 parts of sodium carbonate: 2-4 parts of dimethyl sulfoxide: 65-75 parts.
The post-treatment is to introduce the material system after the reaction into cold water for cooling and solidification, and then repeatedly wash the material system by ethanol and deionized water; finally, drying the mixture in a vacuum drying oven at the temperature of 100-110 ℃, and cooling the dried mixture to room temperature;
the reaction equation of the step (1) is as follows:
(2) preparing a dispersion liquid:
crushing the particles treated in the step (1) to 100-110 microns by a high-speed crusher, dissolving the micro powder particles and dibutyl sebacate in trichloromethane and methanol, and dispersing the mixed solution to obtain a dispersion liquid;
the material ratio of the reaction is as follows: the micro powder particles comprise the following components in parts by weight: 5-15 parts of dibutyl sebacate (plasticizer): 1-2 parts, trichloromethane: 65-85 parts of methanol: 5-10 parts.
The dispersion step is controlled to rotate at 8000-10000 rpm for 180-210 min.
(3) Preparation of an aqueous solution:
putting the dispersion liquid prepared in the step (2) into sodium alkyl benzene sulfonate, polyacrylamide, methyl pyrrolidone and pure water, and mixing and dispersing;
the dispersion step is controlled to rotate at 8000-10000 rpm for 180-210 min.
The material ratio of the reaction is as follows: the dispersion liquid prepared in the step (2) comprises the following components in parts by weight: 45-55 parts of a solvent; sodium alkyl benzene sulfonate (surfactant): 1-2 parts of polyacrylamide (thickening agent): 1-2 parts of methyl pyrrolidone (flatting agent): 2-3 parts of pure water: 45-55 parts.
(4) Desolventizing agent
Putting the aqueous solution obtained in the step (3) into a reactor, heating to 55-65 ℃ for 360-420 min, and continuously introducing nitrogen for eliminating bubbles and evaporating an organic solvent;
(5) coating and crosslinking
And (4) coating the solution obtained in the step (4), and continuously irradiating for 10-20 min by using an ultraviolet curing lamp to finally obtain the polyether-ether-ketone water-soluble coating.
The wavelength of the ultraviolet rays is 300-400 nm.
The reactors described in steps (1) and (4) are three-neck flasks equipped with mechanical stirring, thermometers, condensation recovery devices.
The curing crosslinking A type, B type and C type chemical structural formulas are as follows:
in the step (1), after the bisphenol A and the hydroquinone act together, a polyether-ether-ketone main chain structure is connected, a high-hybridization degree of dimethyl is introduced through the bisphenol A, and a double-chain winding effect appears on a side chain group introduced into the main chain, so that the stability of the original polyether-ether-ketone structure is destroyed, and different changes appear on indexes such as glass transition temperature, melting temperature and the like, so that the polyether-ether-ketone structure has a certain dissolubility;
the dibutyl sebacate substance added in the step (2) has the effect of normal-temperature physical plasticization, and can be effectively attached to the product in the step (1), so that the product in the step (1) is more uniformly dispersed in a mixed solution of chloroform and methanol, and the product in the step (1) is subjected to organic phase dissolution; the reason for selecting the mixed solution of the trichloromethane and the methanol for dissolving is that the mixed solution can be dissolved to the maximum extent by utilizing the characteristics of low boiling point and high polarity of the trichloromethane and the methanol, and simultaneously, the process of removing the solvent in the step (4) is relatively quick;
step (3) is that the blending solution in the step (2) is evenly dispersed in pure water after being blended by sodium alkyl benzene sulfonate (surfactant), polyacrylamide (thickener) and methyl pyrrolidone (leveling agent), and the used sodium alkyl benzene sulfonate has the function of enhancing the surface activity of substances, so that the blending solution in the step (2) has better hydrophilicity and wettability; polyacrylamide is used as a thickening agent, and the mixed solution obtained in the step (2) has low viscosity and excellent fluidity and is not suitable for film formation, so that polyacrylamide is added to prepare film products with different thickness specifications; the methyl pyrrolidone plays a leveling role, when the viscosity of the solution in the step (3) is increased, the fluidity is greatly weakened, and the problems of local wrinkles, foaming, cracking and the like occur in the film forming process, and the problems can be effectively solved after the methyl pyrrolidone is added; the diluent selected is pure water, and the main purpose is to avoid the introduction of metal ion impurities, which may adversely affect the ultraviolet crosslinking curing in step (5).
The main function of the step (4) is to evaporate the organic solvent of the blending solution in the step (3) at low temperature to make the final product be water-based paint;
the film preparation process in the step (5) has the main function that the solution is prepared into a film with a specified size according to actual needs, wherein ultraviolet curing is the last step of film formation, the curing time and the ultraviolet wavelength are both within a given control range, the ultraviolet wavelength is controlled within 300-400 nm, the ultraviolet wavelength is obtained according to the bond energy of a ketone bond and a bisphenol A methyl group in a product, and the maximum crosslinking speed can be achieved at the wavelength. After the wavelength of ultraviolet light changes, substances in the solution cannot generate a crosslinking effect, the purpose of film formation cannot be finally achieved, the problem of low film formation strength can be caused when the irradiation time is too short, and energy waste can be caused when the crosslinking reaction is completely finished if the irradiation time is too long.
The invention introduces side groups or flexible bonds (side groups and double chains of a bisphenol A structure) into a polymer, thereby destroying the regularity and crystallinity of the chains, finally preparing a polyether-ether-ketone product which keeps the original performance of the material and has good solubility, introducing crosslinking points (ketone bonds and methyl introduced by bisphenol A) into the polyether-ether-ketone material, obtaining a high-performance material by forming a crosslinking structure, improving the curing rate, generating crosslinking reaction after ultraviolet irradiation, finally curing and forming, and preparing the water-soluble polyether-ether-ketone coating, wherein the polyether-ether-ketone coating can keep stability in a water dispersion system for a long time, the viscosity of the coating system can be adjusted by a pure water phase, and any auxiliary agent is not required to be added, and the coating can be flexibly constructed according to the requirements of different working conditions and environments in the using process, and a dry-to-touch coating can be obtained in a short time, reduce dust adsorption and repair of defects.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention.
Example 1:
1. synthesis of
Adding 10 parts of 4, 4-difluorobenzophenone, 6 parts of bisphenol A, 5 parts of hydroquinone, 4 parts of sodium carbonate and 75 parts of dimethyl sulfoxide into a 3L three-neck flask provided with a mechanical stirrer, a thermometer and high-purity nitrogen protection, and starting to heat after nitrogen is continuously introduced for 120 min; heating to 150 deg.C at a rate of 3 deg.C/min, maintaining the temperature for 90min, and stirring at a rate of 15r/min after the materials in the system are completely dissolved; raising the temperature of the system to 200 ℃ again, and stirring for 300min at constant temperature; after the reaction is completed, introducing the materials in the system into cold water for cooling and solidification, and repeatedly washing by ethanol and deionized water; finally, drying the mixture in a vacuum drying oven at 100 ℃, and cooling the dried mixture to room temperature for later use;
2. preparation of the Dispersion
Crushing the particles dried and cooled in the step 1 to 100 microns by a high-speed crusher, dissolving 15 parts of micro powder particles and 1 part of dibutyl sebacate (plasticizer) in 74 parts of trichloromethane and 10 parts of methanol, and forcibly dispersing the mixed solution by a colloid mill at the rotation speed of 10000rpm for 180 min;
3. preparation of aqueous solutions
Adding 45 parts of the dispersion liquid prepared in the step 2 into 1 part of sodium alkyl benzene sulfonate (surfactant), 2 parts of polyacrylamide (thickener), 3 parts of methyl pyrrolidone (leveling agent) and 49 parts of pure water, and forcibly mixing by a colloid mill at the rotation speed of 10000rpm for 180 min;
4. desolventizing agent
Putting the aqueous solution in the step 3 into a three-neck flask provided with a stirring device, a thermometer and a condensation recovery device, heating to 65 ℃ for 360min, and continuously introducing nitrogen for eliminating bubbles and evaporating an organic solvent;
5. coating and crosslinking
And coating the glass sheet by using a natural flow casting mode, repeatedly coating for many times, continuously irradiating for 10min by using the ultraviolet wavelength of an ultraviolet curing lamp of 400nm, and finally preparing the polyether-ether-ketone water-soluble coating film with excellent performance.
Example 2:
1. synthesis of
Adding 15 parts of 4, 4-difluorobenzophenone, 10 parts of bisphenol A, 5 parts of hydroquinone, 4 parts of sodium carbonate and 66 parts of dimethyl sulfoxide into a 3L three-neck flask provided with a mechanical stirrer, a thermometer and high-purity nitrogen protection, and starting to heat after nitrogen is continuously introduced for 120 min; heating to 150 deg.C at a rate of 3 deg.C/min, maintaining the temperature for 90min, and stirring at a rate of 15r/min after the materials in the system are completely dissolved; raising the temperature of the system to 200 ℃ again, and stirring for 300min at constant temperature; after the reaction is completed, introducing the materials in the system into cold water for cooling and solidification, and repeatedly washing by ethanol and deionized water; finally, drying the mixture in a vacuum drying oven at 100 ℃, and cooling the dried mixture to room temperature for later use;
2. preparation of the Dispersion
Crushing the particles dried and cooled in the step 1 to 100 microns by a high-speed crusher, dissolving 10 parts of the micro powder particles and 2 parts of dibutyl sebacate (plasticizer) in 78 parts of trichloromethane and 10 parts of methanol, and forcibly dispersing the mixed solution by a colloid mill at the rotation speed of 10000rpm for 180 min;
3. preparation of aqueous solutions
Adding 48 parts of the dispersion liquid prepared in the step 2 into pure water containing 2 parts of sodium alkyl benzene sulfonate (surfactant), 2 parts of polyacrylamide (thickener), 3 parts of methyl pyrrolidone (leveling agent) and 45 parts of pure water, and forcibly mixing by a colloid mill at the rotation speed of 10000rpm for 180 min;
4. desolventizing agent
Putting the aqueous solution in the step 3 into a three-neck flask provided with a stirring device, a thermometer and a condensation recovery device, heating to 65 ℃ for 360min, and continuously introducing nitrogen for eliminating bubbles and evaporating an organic solvent;
5. coating and crosslinking
And coating the glass sheet by using a natural flow casting mode, repeatedly coating for many times, continuously irradiating for 10min by using the ultraviolet wavelength of an ultraviolet curing lamp of 400nm, and finally preparing the polyether-ether-ketone water-soluble coating film with excellent performance.
Example 3:
1. synthesis of
Adding 14 parts of 4, 4-difluorobenzophenone, 9 parts of bisphenol A, 5 parts of hydroquinone, 4 parts of sodium carbonate and 68 parts of dimethyl sulfoxide into a 3L three-neck flask provided with a mechanical stirrer, a thermometer and high-purity nitrogen protection, and starting to heat after nitrogen is continuously introduced for 120 min; heating to 150 deg.C at a rate of 3 deg.C/min, maintaining the temperature for 90min, and stirring at a rate of 15r/min after the materials in the system are completely dissolved; raising the temperature of the system to 200 ℃ again, and stirring for 300min at constant temperature; after the reaction is completed, introducing the materials in the system into cold water for cooling and solidification, and repeatedly washing by ethanol and deionized water; finally, drying the mixture in a vacuum drying oven at 100 ℃, and cooling the dried mixture to room temperature for later use;
2. preparation of the Dispersion
Crushing the dried and cooled particles in the step 1 to 100 microns by a high-speed crusher, dissolving 5 parts of micro powder particles and 2 parts of dibutyl sebacate (plasticizer) in 83 parts of trichloromethane and 10 parts of methanol, and forcibly dispersing the mixed solution by a colloid mill at the rotation speed of 10000rpm for 180 min;
3. preparation of aqueous solutions
Putting 47 parts of the dispersion liquid prepared in the step 2 into pure water containing 2 parts of sodium alkyl benzene sulfonate (surfactant), 2 parts of polyacrylamide (thickener), 3 parts of methyl pyrrolidone (leveling agent) and 46 parts of pure water, and forcibly mixing by a colloid mill at the rotation speed of 10000rpm for 180 min;
4. desolventizing agent
Putting the aqueous solution in the step 3 into a three-neck flask provided with a stirring device, a thermometer and a condensation recovery device, heating to 65 ℃ for 360min, and continuously introducing nitrogen for eliminating bubbles and evaporating an organic solvent;
5. coating and crosslinking
The glass sheet is coated by natural flow casting, and the coating can be repeatedly carried out for many times. And (3) continuously irradiating for 10min by using an ultraviolet curing lamp with the ultraviolet wavelength of 400nm to finally prepare the polyether-ether-ketone water-soluble coating film with excellent performance.
Comparative example:
at present, the commercial product has no solubility, the hygroscopicity is relatively low, the product can be stably used for a long time under most conditions of strong acid and alkali corrosion, the chemical property is extremely stable and is difficult to dissolve, and the solubility is mainly compared in the following table.
Table 1: table of Property data for coatings prepared in examples and comparative examples
Claims (5)
1. A preparation method of a water-soluble polyether-ether-ketone coating is characterized by comprising the following steps: the method comprises the following steps:
(1) polyether-ether-ketone synthesis:
adding 4, 4-difluorobenzophenone, bisphenol A, hydroquinone, sodium carbonate, dimethyl sulfoxide and nitrogen into a reactor, continuously introducing for 100-120 min, and then starting to heat; heating to 150 ℃ at a heating rate of 2-3 ℃/min, keeping the temperature for 80-90 min, starting and continuously stirring after materials in the system are completely dissolved, wherein the stirring rate is 10-15 r/min; raising the temperature of the system to 200-205 ℃ again, and stirring for 240-360 min at constant temperature; after the reaction is completed, post-treating for later use; the material ratio of the reaction is as follows: 4, 4-difluorobenzophenone in parts by weight: 10-15 parts of bisphenol A: 5-10 parts of hydroquinone: 1-5 parts of sodium carbonate: 2-4 parts of dimethyl sulfoxide: 65-75 parts of a solvent;
(2) preparing a dispersion liquid:
crushing the particles treated in the step (1) to 100-110 microns by a high-speed crusher, dissolving the micro powder particles and dibutyl sebacate in trichloromethane and methanol, and dispersing the mixed solution to obtain a dispersion liquid; the material ratio of the reaction is as follows: the micro powder particles comprise the following components in parts by weight: 5-15 parts of dibutyl sebacate: 1-2 parts, trichloromethane: 65-85 parts of methanol: 5-10 parts;
(3) preparation of an aqueous solution:
putting the dispersion liquid prepared in the step (2) into sodium alkyl benzene sulfonate, polyacrylamide, methyl pyrrolidone and pure water, and mixing and dispersing; the material ratio of the reaction is as follows: the dispersion liquid prepared in the step (2) comprises the following components in parts by weight: 45-55 parts of a solvent; sodium alkyl benzene sulfonate: 1-2 parts of polyacrylamide: 1-2 parts of methyl pyrrolidone: 2-3 parts of pure water: 45-55 parts of a solvent;
(4) desolventizing agent
Putting the aqueous solution obtained in the step (3) into a reactor, heating to 55-65 ℃ for 360-420 min, and continuously introducing nitrogen;
(5) coating and crosslinking
And (4) coating the solution obtained in the step (4), and continuously irradiating for 10-20 min by using an ultraviolet curing lamp to finally obtain the polyether-ether-ketone water-soluble coating.
2. The method for preparing the water-soluble polyether-ether-ketone coating according to claim 1, wherein the method comprises the following steps: the post-treatment in the step (1) is to introduce the material system after the reaction into cold water for cooling and solidification, and then repeatedly wash the material system by ethanol and deionized water; and finally drying the mixture in a vacuum drying oven at 100-110 ℃, and cooling the dried mixture to room temperature.
3. The method for preparing the water-soluble polyether-ether-ketone coating according to claim 1, wherein the method comprises the following steps: the dispersing step in the steps (2) and (3) controls the rotating speed to be 8000-10000 rpm, and the dispersing time is 180-210 min.
4. The method for preparing the water-soluble polyether-ether-ketone coating according to claim 1, wherein the method comprises the following steps: the wavelength of the ultraviolet rays in the step (5) is 300-400 nm.
5. The method for preparing the water-soluble polyether-ether-ketone coating according to claim 1, wherein the method comprises the following steps: the reactors described in steps (1) and (4) are three-neck flasks equipped with mechanical stirring, thermometers, condensation recovery devices.
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