CN109912815B - High-redispersibility fluoroplastic aqueous dispersion liquid and preparation method and application thereof - Google Patents
High-redispersibility fluoroplastic aqueous dispersion liquid and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a high redispersibility fluoroplastic aqueous dispersion, a preparation method and application thereof, wherein the main components of the fluoroplastic aqueous dispersion comprise polytetrafluoroethylene, water-soluble resin PVP, a surfactant and deionized water; the content of the polytetrafluoroethylene accounts for 30-70% of the mass of the fluoroplastic water-based dispersion liquid, and the polytetrafluoroethylene is calculated by dry materials; the content of the water-soluble resin PVP is 0.05-0.3% of the mass of the polytetrafluoroethylene dry material; the content of the surfactant is 2.5-4.0% of the mass of the polytetrafluoroethylene dry material. According to the invention, the content of the surfactant in the polytetrafluoroethylene concentrated dispersion liquid is reduced, and the water-soluble resin PVP is added, so that the redispersibility of the concentrated dispersion liquid is greatly improved, and the obtained dispersion liquid has stable performance; the fluoroplastic water-based dispersion liquid prepared by the invention has good redispersibility and good mechanical stability.
Description
Technical Field
The invention relates to a high-redispersibility fluoroplastic aqueous dispersion liquid, and a preparation method and application thereof, and belongs to the technical field of chemical synthesis.
Background
The polytetrafluoroethylene concentrated dispersion is obtained by heating and concentrating a dispersion obtained by dispersion polymerization of tetrafluoroethylene in the presence of an emulsifier, and is excellent in corrosion resistance, weather resistance, solvent resistance, low friction coefficient, wear resistance, impact resistance and the like, and can be used for impregnating porous materials such as asbestos, glass fiber, ceramics, graphite and the like to form a film which shows excellent characteristics in terms of chemical stability, non-adhesiveness, weather resistance and the like, or can be prepared into a coating material and spun into polytetrafluoroethylene fiber to be used as an anti-sticking, anti-corrosion or sealing material, so that the polytetrafluoroethylene concentrated dispersion is widely used in applications such as cooking devices, linings of piping, glass cloth impregnated films and the like.
Mechanical stability refers to the stability of the emulsion when subjected to mechanical handling, since the emulsion and its coating survive mechanical handling during the coating preparation process, such as pumping, stirring, and spraying during coating. The existing polytetrafluoroethylene concentrated dispersion liquid has poor mechanical stability and is easy to agglomerate to generate aggregates.
In the storage process of the polytetrafluoroethylene concentrated dispersion, if the polytetrafluoroethylene concentrated dispersion is stored for a long time in a static way, a sedimentation phenomenon can be generated, and products with poor redispersibility can generate aggregates at the bottom to influence the use of the products.
Therefore, it is desirable to prepare aqueous polytetrafluoroethylene dispersions which exhibit not only good mechanical stability during processing and application, but also good redispersibility to facilitate long-term storage without changes in properties.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high redispersibility fluoroplastic aqueous dispersion and a preparation method and application thereof.
The technical scheme of the invention is as follows:
a fluoroplastic aqueous dispersion with high redispersibility mainly comprises polytetrafluoroethylene, water-soluble resin PVP, a surfactant and deionized water; the content of the polytetrafluoroethylene accounts for 30-70% of the mass of the fluoroplastic water-based dispersion liquid, and the polytetrafluoroethylene is calculated by dry materials; the content of the water-soluble resin PVP is 0.05-0.3% of the mass of the polytetrafluoroethylene dry material; the content of the surfactant is 2.5-4.0% of the mass of the polytetrafluoroethylene dry material.
According to the invention, the average molecular weight of the water-soluble resin PVP is preferably 50000-1300000.
According to the present invention, preferably, the surfactant is a nonionic surfactant; the surfactant TMN-10 is more preferable.
According to the present invention, the preparation method of the aqueous dispersion of the high redispersibility fluoroplastic comprises the following steps:
(1) adding a surfactant into the polytetrafluoroethylene aqueous polymer solution, adjusting the pH value of the system to 9-10, and heating and concentrating to obtain a polytetrafluoroethylene concentrated dispersion solution;
(2) adding a surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the total content of the surfactant in the system to be 2.5-4% of the mass of the polytetrafluoroethylene dry material, adding a water-soluble resin PVP to enable the content of the water-soluble resin PVP to be 0.05-0.3% of the mass of the polytetrafluoroethylene dry material, adjusting the pH value of the system to be 9-10, adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material of the system to be 30-70%, and obtaining the high-redispersibility fluoroplastic water-based dispersion liquid.
According to the preparation method of the invention, the polytetrafluoroethylene aqueous polymerization solution in the step (1) preferably contains 15-35% by mass of dried polytetrafluoroethylene and has an average particle size of 0.15-0.30 μm.
According to the preparation method of the present invention, preferably, the preparation method of the aqueous polytetrafluoroethylene polymer solution described in step (1) is prior art, and can be prepared by the following method: tetrafluoroethylene is polymerized under pressure in an aqueous solution of a polymerization emulsifier such as ammonium polyfluorocarboxylate under stirring using ammonium persulfate or succinic acid peroxide as a polymerization initiator, and is obtained by a dispersion polymerization method.
According to the preparation method provided by the invention, preferably, the addition amount of the surfactant in the step (1) is 12-20% of the mass of the polytetrafluoroethylene dry material.
According to the preparation method of the present invention, preferably, the concentration heating step in the step (1) is: heating the system to 75-90 ℃, standing for 3-4 h, standing the system to room temperature after a large number of transparent aqueous solution layers are formed on the upper layer, forming a transparent aqueous solution layer on the upper layer, and removing the upper aqueous solution layer to obtain the polytetrafluoroethylene concentrated dispersion.
According to the preparation method provided by the invention, preferably, the content of the surfactant in the polytetrafluoroethylene concentrated dispersion liquid in the step (1) is 1.5-2.5% of the mass of the polytetrafluoroethylene dry material; the content of the polytetrafluoroethylene dry material accounts for 61-75% of the mass of the polytetrafluoroethylene concentrated dispersion liquid.
According to the preparation method provided by the invention, preferably, ammonia water is adopted in the steps (1) and (2) to adjust the pH value of the system, and the mass fraction of the ammonia water is 25-28%.
According to the invention, the high redispersibility fluoroplastic aqueous dispersion is applied to processed products such as coatings, glass cloth impregnation and the like.
The invention has the following technical characteristics and beneficial effects:
1. according to the invention, the content of the surfactant in the polytetrafluoroethylene concentrated dispersion liquid is reduced, and a certain amount of water-soluble resin PVP is added, so that the redispersibility of the concentrated dispersion liquid is greatly improved, the prepared fluoroplastic water-based dispersion liquid can be uniformly redispersed after being stored for a long time, and the stable performance of the dispersion liquid is ensured.
2. The fluoroplastic water-based dispersion liquid prepared by the invention has good redispersibility, good mechanical stability, difficult demulsification in the machining process and good processing performance.
3. When the fluoroplastic water-based dispersion liquid prepared by the invention is used for coating, the obtained coating has good impact resistance, and can be used for preparing a flat and uniform coating; the prepared dipping product has the characteristics of good surface gloss, high limit film crack thickness, smoothness, excellent crack resistance and the like.
Detailed Description
The invention will be further described with reference to, but not limited to, specific examples.
The experimental methods described in the examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
The aqueous polytetrafluoroethylene polymer solution used in the examples was prepared as follows: tetrafluoroethylene is obtained by dispersion polymerization by pressure polymerization of ammonium persulfate or succinic acid peroxide as a polymerization initiator in an aqueous solution of a polymerization emulsifier such as ammonium polyfluorocarboxylate under stirring, and the polytetrafluoroethylene has a mass content of 30% and an average particle diameter of 0.20 μm, based on the weight of the polymerization solution.
The nonionic surfactant used in the examples was surfactant TMN-10, available from Dow chemical of Dow, USA;
the water-soluble resin PVP used was water-soluble resin PVP K90, with an average molecular weight of 1300000, available from BASF corporation, Germany.
Example 1
A preparation method of a fluoroplastic aqueous dispersion with high redispersibility comprises the following steps:
(1) adding 112.5g of nonionic surfactant into 3kg of polytetrafluoroethylene aqueous polymer solution, uniformly stirring, adding 25% by mass of ammonia water to adjust the pH value of the system to 10, heating the system to 87 ℃, standing for 3 hours at 87 ℃, standing for 3 hours until an upper layer forms a large number of transparent aqueous solution layers, standing the system to room temperature, forming a transparent aqueous solution layer on the upper layer, forming a concentrated emulsion layer on the lower layer, and removing the upper aqueous layer to obtain the polytetrafluoroethylene concentrated dispersion. Testing the polytetrafluoroethylene concentrated dispersion liquid to obtain that the content of a polytetrafluoroethylene dry material is 65% of the mass of the polytetrafluoroethylene concentrated dispersion liquid, and the content of a nonionic surfactant is 1.8% of the mass of the polytetrafluoroethylene dry material;
(2) adding a nonionic surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the total content of the nonionic surfactant to be 3.0% of the mass of the polytetrafluoroethylene dry material, adding a water-soluble resin PVP K90 to enable the content of the water-soluble resin PVP K90 to be 0.3% of the mass of the polytetrafluoroethylene dry material, adding 25% of ammonia water to adjust the pH value of the system to be 10, and adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material in the system to be 60% (based on the total mass of the system) to obtain the high-redispersibility fluoroplastic aqueous dispersion liquid.
Example 2
A process for preparing an aqueous dispersion of a highly redispersible fluoroplastic, as in example 1, except that:
in the step (2), adding a nonionic surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the total content of the nonionic surfactant to be 3.5% of the mass of the polytetrafluoroethylene dry material, adding a water-soluble resin PVP K90 to enable the content of the water-soluble resin PVP K90 to be 0.3% of the mass of the polytetrafluoroethylene dry material, adding 25% of ammonia water to adjust the pH value of the system to be 10, and adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material in the system to be 60% (based on the total mass of the system) to obtain the high-redispersibility fluoroplastic aqueous dispersion liquid.
Example 3
A process for preparing an aqueous dispersion of a highly redispersible fluoroplastic, as in example 1, except that:
in the step (2), adding a nonionic surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the content of the nonionic surfactant to be 4.0% of the mass of the polytetrafluoroethylene dry material, adding a water-soluble resin PVPK90 to enable the content of the water-soluble resin PVPK90 to be 0.1% of the mass of the polytetrafluoroethylene dry material, adding 25% of ammonia water to adjust the pH value of the system to be 10, and adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material in the system to be 60% (based on the total mass of the system) to obtain the high-redispersibility fluoroplastic aqueous dispersion liquid.
Comparative example 1
A fluoroplastic aqueous dispersion was prepared as in example 1, except that:
in the step (2), adding a nonionic surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the content of the nonionic surfactant to be 6.0% of the mass of the polytetrafluoroethylene dry material, adding 25% of ammonia water by mass percent to adjust the pH value of the system to be 10, and adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material in the system to be 60% (based on the total mass of the system) to obtain the fluoroplastic water-based dispersion liquid.
Comparative example 2
A fluoroplastic aqueous dispersion was prepared as in example 1, except that:
in the step (2), adding a nonionic surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the content of the nonionic surfactant to be 8.0% of the mass of the polytetrafluoroethylene dry material, adding 25% of ammonia water by mass percent to adjust the pH value of the system to be 10, and adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material in the system to be 60% (based on the total weight of the system) to obtain the fluoroplastic water-based dispersion liquid.
Comparative example 3
A fluoroplastic aqueous dispersion was prepared as in example 1, except that:
in the step (2), adding a nonionic surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the content of the nonionic surfactant to be 4.0% of the mass of the polytetrafluoroethylene dry material, adding 25% of ammonia water by mass fraction to adjust the pH value of the system to be 10, and adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material in the system to be 60% (based on the total mass of the system) to obtain the fluoroplastic water-based dispersion liquid.
Test examples
The aqueous fluoroplastic dispersions prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to measurements of the content of dry polytetrafluoroethylene and the content of surfactant, pH, viscosity at 25 ℃, mechanical stability at 25 ℃ and redispersibility of the aqueous fluoroplastic dispersion after 60 days.
1. Determination of the content of the dried Polytetrafluoroethylene and the content of the surfactant
The test method is as follows:
content of Polytetrafluoroethylene (PTFE) dry matter: about 10g of the dispersion was taken out of an aluminum bowl having a diameter of 10cm, dried at 110 ℃ for 1 hour and further dried at 300 ℃ for 1 hour to obtain a heated residue, and the content (P) of the polytetrafluoroethylene dried material was calculated by the following formula:
P＝Z/X×100％
wherein: p is the content of polytetrafluoroethylene dry materials in the dispersion liquid and is expressed by mass percent; z is the mass (g) of the heating residue; x represents the mass (g) of the dispersion.
Content of surfactant: about 10g of the dispersion was taken out from an aluminum bowl having a diameter of 10cm, and heated at 110 ℃ for 1 hour to obtain a heated residue I, and further heated at 300 ℃ for 1 hour to obtain a heated residue II, the content (N) of the surfactant being calculated by the formula:
N＝[(Y-Z)/Z]×100％
wherein: n is the content of the surfactant and is expressed by mass percent; y is the mass (g) of the heating residue I; z is the mass (g) of the heated residue II.
2. Measurement of pH and viscosity
Measuring the pH value of the fluoroplastic aqueous dispersion by using a pH meter; the viscosity of the aqueous fluoroplastic dispersions was measured at 25 ℃ using a rotational viscometer (DV-II + BROOKFIELD, USA).
3. Determination of mechanical stability at 25 deg.C
The mechanical stability test method is as follows:
using the appliance:
peristaltic pump, silicone tube, 100mL beaker, 200 mesh nylon filter cloth
The test method comprises the following steps:
connecting a silicone tube to a peristaltic pump;
② putting 150g of fluoroplastic water-based dispersion liquid into a 100mL beaker;
controlling the room temperature to be about 25 ℃;
fourthly, adjusting the inlet and outlet quantity of the peristaltic pump to be 200 mL/min;
circulating the aqueous dispersion liquid of the fluoroplastic for 2 hours under the conditions;
sixthly, filtering and collecting the condensate in the dispersion liquid by using a 200-mesh filter screen after 2 hours, and washing the condensate by using pure water;
seventhly, putting the taken-out aggregates into a drying oven, and drying for 2 hours at the temperature of 120 ℃;
after drying, the mass M of the aggregate was measured.
Ninthly, calculating the mechanical stability of the fluoroplastic aqueous dispersion liquid by the following method
Mechanical stability (%) - [ M/(150 XP) ]. times.100%,
wherein M is the mass (g) of the aggregate; p is the content of polytetrafluoroethylene dry materials and is expressed by mass percent. The smaller the mechanical stability value, the better the mechanical stability, and the less likely aggregates will appear during mechanical stirring.
4. Measurement of redispersibility
The test method is as follows:
using the appliance:
500mL measuring cylinder, 200-mesh nylon filter cloth, constant-temperature oven and sealing adhesive tape
The test method comprises the following steps:
500mL of fluoroplastic water-based dispersion liquid is filtered by a 200-mesh nylon filter cloth and then added into a 500mL measuring cylinder;
secondly, sealing the opening of the measuring cylinder by using an adhesive tape;
thirdly, placing the sealed measuring cylinder into a constant-temperature oven, and standing for 60 days;
adjusting the temperature of the constant-temperature oven to 25 ℃;
taking out the measuring cylinder after 60 days, inverting the measuring cylinder, and observing whether the bottom of the measuring cylinder is provided with aggregates or not;
the fluoroplastic aqueous dispersion liquid with good redispersibility has no aggregate at the bottom of the measuring cylinder.
The results of the above tests are shown in table 1 below.
TABLE 1 Performance test results of aqueous dispersions of fluoroplastics prepared in examples 1-3 and comparative examples 1-3
As can be seen from the above table, the re-dispersibility of the aqueous fluoroplastic dispersions prepared in examples 1 to 3 is significantly improved as compared with the aqueous fluoroplastic dispersions prepared in comparative examples 1 to 3. The dispersion prepared in comparative example 3, although having improved redispersibility, has poor mechanical stability. Therefore, the fluoroplastic aqueous dispersion prepared by the invention can obviously improve the redispersibility of the fluoroplastic aqueous dispersion and simultaneously keep good mechanical stability.
Claims (6)
1. A fluoroplastic aqueous dispersion with high redispersibility is characterized in that the main components of the fluoroplastic aqueous dispersion comprise polytetrafluoroethylene, water-soluble resin PVP, a surfactant and deionized water; the content of the polytetrafluoroethylene accounts for 30-70% of the mass of the fluoroplastic water-based dispersion liquid, and the polytetrafluoroethylene is calculated by dry materials; the content of the water-soluble resin PVP is 0.05-0.3% of the mass of the polytetrafluoroethylene dry material; the content of the surfactant is 3.0-4.0% of the mass of the polytetrafluoroethylene dry material; the surfactant is a surfactant TMN-10; the average molecular weight of the water-soluble resin PVP is 1300000;
the preparation method comprises the following steps:
(1) adding a surfactant into the polytetrafluoroethylene aqueous polymer solution, adjusting the pH value of the system to 9-10, and heating and concentrating to obtain a polytetrafluoroethylene concentrated dispersion solution; the content of the surfactant in the polytetrafluoroethylene concentrated dispersion liquid is 1.5-2.5% of the mass of the polytetrafluoroethylene dry material; the mass content of polytetrafluoroethylene dry materials in the polytetrafluoroethylene aqueous polymerization solution is 15-35%, and the average particle size is 0.15-0.30 mu m;
(2) adding a surfactant into the polytetrafluoroethylene concentrated dispersion liquid to enable the total content of the surfactant in the system to be 3-4% of the mass of the polytetrafluoroethylene dry material, adding a water-soluble resin PVP to enable the content of the water-soluble resin PVP to be 0.05-0.3% of the mass of the polytetrafluoroethylene dry material, adjusting the pH value of the system to be 9-10, adding deionized water to adjust the mass content of the polytetrafluoroethylene dry material of the system to be 30-70%, and obtaining the high-redispersibility fluoroplastic water-based dispersion liquid.
2. The aqueous dispersion of a highly redispersible fluoroplastic according to claim 1 wherein the surfactant is added in an amount of 12 to 20% by weight based on the dry polytetrafluoroethylene.
3. The aqueous dispersion of a highly redispersible fluoroplastic according to claim 1 wherein said concentrating and heating step in step (1) is: heating the system to 75-90 ℃, standing for 3-4 h, standing the system to room temperature after a large number of transparent aqueous solution layers are formed on the upper layer, forming a transparent aqueous solution layer on the upper layer, and removing the upper aqueous solution layer to obtain the polytetrafluoroethylene concentrated dispersion.
4. The aqueous dispersion of a highly redispersible fluoroplastic according to claim 1 wherein the dry polytetrafluoroethylene content of the concentrated dispersion of polytetrafluoroethylene in step (1) is from 61% to 75% by mass of the concentrated dispersion of polytetrafluoroethylene.
5. The aqueous dispersion of a highly redispersible fluoroplastic according to claim 1, wherein the aqueous dispersion of an aqueous ammonia solution is used in the steps (1) and (2) to adjust the pH of the system, and the mass fraction of the aqueous ammonia solution is 25 to 28%.
6. Use of the aqueous dispersion of a highly redispersible fluoroplastic according to claim 1 in coatings, glass cloth dipped articles.
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| CN101538394A (en) * | 2008-03-21 | 2009-09-23 | 大金工业株式会社 | Water-soluble fluid dispersion of fluorine-containing polymer |
| JP2013204181A (en) * | 2012-03-28 | 2013-10-07 | Toray Ind Inc | Polytetrafluoroethylene impregnated fiber and method for producing the same |
| CN104203386A (en) * | 2012-03-30 | 2014-12-10 | 大金工业株式会社 | Non-ionic surfactant composition and fluoropolymer aqueous dispersion |
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| CN101137711A (en) * | 2005-03-10 | 2008-03-05 | 大金工业株式会社 | Polytetrafluoroethylene aqueous dispersion composition, polytetrafluoroethylene resin film and polytetrafluoroethylene resin impregnated article |
| CN101538394A (en) * | 2008-03-21 | 2009-09-23 | 大金工业株式会社 | Water-soluble fluid dispersion of fluorine-containing polymer |
| JP2013204181A (en) * | 2012-03-28 | 2013-10-07 | Toray Ind Inc | Polytetrafluoroethylene impregnated fiber and method for producing the same |
| CN104203386A (en) * | 2012-03-30 | 2014-12-10 | 大金工业株式会社 | Non-ionic surfactant composition and fluoropolymer aqueous dispersion |
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