CN109912815A - A kind of high redispersibility fluoroplastics aqueous liquid dispersion and the preparation method and application thereof - Google Patents
A kind of high redispersibility fluoroplastics aqueous liquid dispersion and the preparation method and application thereof Download PDFInfo
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Abstract
The present invention provides a kind of high redispersibility fluoroplastics aqueous liquid dispersion and the preparation method and application thereof, the main component of the fluoroplastics aqueous liquid dispersion includes polytetrafluoroethylene (PTFE), water-soluble resin PVP, surfactant and deionized water；The content of the polytetrafluoroethylene (PTFE) is the 30~70% of fluoroplastics aqueous liquid dispersion quality, and polytetrafluoroethylene (PTFE) is in terms of siccative；The content of the water-soluble resin PVP is the 0.05~0.3% of polytetrafluoroethylene (PTFE) siccative quality；The content of the surfactant is the 2.5~4.0% of polytetrafluoroethylene (PTFE) siccative quality.The content that surfactant in dispersion liquid is concentrated by reducing polytetrafluoroethylene (PTFE) in the present invention, while water-soluble resin PVP is added, the redispersibility of concentration dispersion liquid is substantially improved, obtained dispersion liquid performance is stablized；Fluoroplastics aqueous liquid dispersion prepared by the present invention has good mechanical stability while with good redispersibility.
Description
Technical field
The present invention relates to a kind of high redispersibility fluoroplastics aqueous liquid dispersions and the preparation method and application thereof, belong to chemical industry conjunction
At technical field.
Background technique
Polytetrafluoroethylene (PTFE) is concentrated dispersion liquid dispersion liquid as made from tetrafluoroethene dispersin polymerization and adds in the presence of emulsifier
Dispersion liquid is concentrated up to polytetrafluoroethylene (PTFE) in thermal concentration, it has excellent corrosion resistance, weatherability, solvent resistance, low friction system
Number, wearability, impact resistance etc. can be used for the porous materials such as impregnated asbestos, glass fibre and ceramics, graphite, be formed in chemistry
Stability, non-adhesive, weatherability etc. show the film of excellent characteristics, can also be made into coating, and polytetrafluoroethyl-ne is made in spinning
Alkene fiber is used as anti-sticking, anti-corrosion or sealing material, thus in device for cooking, the lining of piping, glass cloth infiltration film etc. on the way
It is widely used.
Mechanical stability refers to stability when lotion is subjected to mechanically actuated, because during preparing coating, it be through pumping
It send, stir and the operations such as spraying when coating, therefore lotion and its coating will withstand mechanically actuated.Existing polytetrafluoroethyl-ne
Alkene concentration dispersion liquid mechanical stability is poor, is easy agglomeration and generates agglutinator.
Dispersion liquid is concentrated during storage in polytetrafluoroethylene (PTFE), if static storage for a long time, can generate sedimentation phenomenon, then
The poor product of dispersibility can generate agglutinator in bottom, influence its use.
Therefore, it is necessary to prepare a kind of aqueous dispersion of polytetrafluoroethyland, make the dispersion liquid during processed and applied not only
With good mechanical stability, moreover it is possible to good redispersibility is made it have, so that long-time storage performance will not be sent out
Changing.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of high redispersibility fluoroplastics aqueous liquid dispersion and its preparation side
Method and application.
Technical scheme is as follows:
A kind of high redispersibility fluoroplastics aqueous liquid dispersion, the main component of the fluoroplastics aqueous liquid dispersion includes polytetrafluoro
Ethylene, water-soluble resin PVP, surfactant and deionized water；The content of the polytetrafluoroethylene (PTFE) is aqueous point of fluoroplastics
The 30~70% of dispersion liquid quality, polytetrafluoroethylene (PTFE) is in terms of siccative；The content of the water-soluble resin PVP is dry for polytetrafluoroethylene (PTFE)
Expect the 0.05~0.3% of quality；The content of the surfactant is the 2.5~4.0% of polytetrafluoroethylene (PTFE) siccative quality.
, according to the invention it is preferred to, the average molecular weight of the water-soluble resin PVP is 50000~1300000.
, according to the invention it is preferred to, the surfactant is nonionic surface active agent；Further preferred surface
Activating agent TMN-10.
According to the present invention, the preparation method of above-mentioned high redispersibility fluoroplastics aqueous liquid dispersion, comprises the following steps that
(1) surfactant is added into aqueous polytetrafluoroethyldispersion polymer fluid, the pH value of regulation system is 9~10, heating
It is concentrated to get polytetrafluoroethylene (PTFE) concentration dispersion liquid；
(2) surfactant is added into polytetrafluoroethylene (PTFE) concentration dispersion liquid, makes the total content of surfactant in system
It is the 2.5~4% of polytetrafluoroethylene (PTFE) siccative quality, water-soluble resin PVP is added, makes water-soluble resin PVP content polytetrafluoro
The 0.05~0.3% of ethylene siccative quality, regulation system pH value are 9~10, and the polytetrafluoroethyl-ne of deionized water adjustment system is added
The mass content of alkene siccative is 30~70%, obtains high redispersibility fluoroplastics aqueous liquid dispersion.
Preparation method according to the present invention, it is preferred that poly- four in aqueous polytetrafluoroethyldispersion polymer fluid described in step (1)
The mass content of vinyl fluoride siccative is 15~35%, and average grain diameter is 0.15~0.30 μm.
Preparation method according to the present invention, it is preferred that the preparation of aqueous polytetrafluoroethyldispersion polymer fluid described in step (1)
Method is the prior art, can be prepared by following methods: tetrafluoroethene is that polymerization is drawn with ammonium persulfate or succinic acid peroxide
Agent is sent out, pressure polymerization under stirring in the polymeric emulsifiers aqueous solution of multi-fluoro carboxy acid's ammonium etc. is obtained by dispersion copolymerization method.
Preparation method according to the present invention, it is preferred that the additional amount of surfactant described in step (1) is polytetrafluoro
The 12~20% of ethylene siccative quality.
Preparation method according to the present invention, it is preferred that concentration heating stepses described in step (1) are as follows: heat system
3~4h is stood after to 75~90 DEG C, is formed a large amount of transparent aqueous solution layers to upper layer, system is stood to room temperature, upper layer is formed
Aqueous solution layer, lower layer are the emulsion layer of concentration, remove upper layer aqueous layer, and polytetrafluoroethylene (PTFE) concentration dispersion liquid can be obtained.
Preparation method according to the present invention, it is preferred that surface in dispersion liquid is concentrated in polytetrafluoroethylene (PTFE) described in step (1)
The content of activating agent is the 1.5~2.5% of polytetrafluoroethylene (PTFE) siccative quality；The content of polytetrafluoroethylene (PTFE) siccative is polytetrafluoroethylene (PTFE)
It is concentrated the 61~75% of dispersion liquid quality.
Preparation method according to the present invention, it is preferred that described using the pH value of ammonia water conditioning system in step (1), (2)
The mass fraction of ammonium hydroxide is 25~28%.
According to the present invention, the application of the high redispersibility fluoroplastics aqueous liquid dispersion is applied to coating, glass cloth soaks
The fabricated products such as stain.
It technical characterstic of the invention and has the beneficial effect that:
1, the content that surfactant in dispersion liquid is concentrated by reducing polytetrafluoroethylene (PTFE) in the present invention, while being added a certain amount of
Water-soluble resin PVP, substantially improve concentration dispersion liquid redispersibility, when the fluoroplastics aqueous liquid dispersion being prepared is long
Between store can also be uniform with redisperse, ensure that the performance of dispersion liquid is stablized.
2, fluoroplastics aqueous liquid dispersion prepared by the present invention has good machine while with good redispersibility
Tool stability is not easy to be demulsified in being subjected to mechanical processing process, has good processing performance.
3, fluoroplastics aqueous liquid dispersion prepared by the present invention is used for coating, and obtained coating impact resistance is preferable, can be with
Prepare smooth, uniform coating；For impregnation processability product, with surface gloss, good, limit film is split obtained impregnation processability product
The features such as thickness height, smoothness, excellent crack resistance.
Specific embodiment
Combined with specific embodiments below, the invention will be further described, but not limited to this.
Experimental method described in embodiment is unless otherwise specified conventional method；The reagent and material, such as without spy
Different explanation, commercially obtains.
Aqueous polytetrafluoroethyldispersion polymer fluid used is prepared via a method which to obtain in embodiment: tetrafluoroethene is with persulfuric acid
Ammonium or succinic acid peroxide are polymerization initiator, are pressurizeed under stirring in the polymeric emulsifiers aqueous solution of multi-fluoro carboxy acid's ammonium etc. poly-
It closes, is obtained by dispersion copolymerization method, on the basis of the weight of polymer fluid, the mass content of polytetrafluoroethylene (PTFE) is 30%, is averaged
Partial size is 0.20 μm.
Nonionic surface active agent used is surfactant TMN-10 in embodiment, and Dow Chemical DOW is on sale；
Water-soluble resin PVP used is water-soluble resin PVP K90, average molecular weight 1300000, German BASF
Company is on sale.
Embodiment 1
A kind of preparation method of high redispersibility fluoroplastics aqueous liquid dispersion, comprises the following steps that
(1) 112.5g nonionic surface active agent is added into 3kg aqueous polytetrafluoroethyldispersion polymer fluid to stir evenly, adds
The pH value for entering the ammonia water conditioning system that mass fraction is 25% is 10, and system is heated to 87 DEG C, in 87 DEG C of standing 3h, to upper layer
A large amount of transparent aqueous solution layers are formed, system is stood to room temperature, upper layer forms transparent aqueous solution layer, and lower layer is the lotion of concentration
Layer removes upper aqueous layer, and polytetrafluoroethylene (PTFE) concentration dispersion liquid can be obtained.It tests polytetrafluoroethylene (PTFE) and dispersion liquid is concentrated, obtain poly- four
The content of vinyl fluoride siccative is that polytetrafluoroethylene (PTFE) is concentrated the 65% of dispersion liquid quality, and the content of nonionic surface active agent is poly-
The 1.8% of tetrafluoroethene siccative quality；
(2) nonionic surface active agent is added into polytetrafluoroethylene (PTFE) concentration dispersion liquid, makes non-ionic surfactant
The total content of agent is the 3.0% of polytetrafluoroethylene (PTFE) siccative quality, and water-soluble resin PVP K90 is added, makes water-soluble resin PVP
K90 content is the 0.3% of polytetrafluoroethylene (PTFE) siccative quality, and the pH value that the ammonia water conditioning system that mass fraction is 25% is added is
10, the mass content that polytetrafluoroethylene (PTFE) siccative in deionized water adjustment system is added is 60% (on the basis of system gross mass),
Obtain high redispersibility fluoroplastics aqueous liquid dispersion.
Embodiment 2
A kind of preparation method of high redispersibility fluoroplastics aqueous liquid dispersion, with embodiment 1, the difference is that:
In step (2), nonionic surface active agent is added into polytetrafluoroethylene (PTFE) concentration dispersion liquid, makes non-ionic table
The total content of face activating agent is the 3.5% of polytetrafluoroethylene (PTFE) siccative quality, and water-soluble resin PVP K90 is added, makes water-soluble tree
Rouge PVP K90 content is the 0.3% of polytetrafluoroethylene (PTFE) siccative quality, and the pH for the ammonia water conditioning system that mass fraction is 25% is added
Value is 10, and the mass content that polytetrafluoroethylene (PTFE) siccative in deionized water adjustment system is added is 60% (using system gross mass as base
It is quasi-), obtain high redispersibility fluoroplastics aqueous liquid dispersion.
Embodiment 3
A kind of preparation method of high redispersibility fluoroplastics aqueous liquid dispersion, with embodiment 1, the difference is that:
In step (2), nonionic surface active agent is added into polytetrafluoroethylene (PTFE) concentration dispersion liquid, makes non-ionic table
Face active agent content is the 4.0% of polytetrafluoroethylene (PTFE) siccative quality, and water-soluble resin PVPK90 is added, makes water-soluble resin
The content of PVPK90 is the 0.1% of polytetrafluoroethylene (PTFE) siccative quality, and the pH for the ammonia water conditioning system that mass fraction is 25% is added
Value is 10, and the mass content that polytetrafluoroethylene (PTFE) siccative in deionized water adjustment system is added is 60% (using system gross mass as base
It is quasi-), obtain high redispersibility fluoroplastics aqueous liquid dispersion.
Comparative example 1
A kind of preparation method of fluoroplastics aqueous liquid dispersion, with embodiment 1, the difference is that:
In step (2), nonionic surface active agent is added into polytetrafluoroethylene (PTFE) concentration dispersion liquid, makes non-ionic table
Face active agent content is the 6.0% of polytetrafluoroethylene (PTFE) siccative quality, and the pH for the ammonia water conditioning system that mass fraction is 25% is added
Value is 10, and the mass content that polytetrafluoroethylene (PTFE) siccative in deionized water adjustment system is added is 60% (using system gross mass as base
It is quasi-), obtain fluoroplastics aqueous liquid dispersion.
Comparative example 2
A kind of preparation method of fluoroplastics aqueous liquid dispersion, with embodiment 1, the difference is that:
In step (2), nonionic surface active agent is added into polytetrafluoroethylene (PTFE) concentration dispersion liquid, makes non-ionic table
Face active agent content is the 8.0% of polytetrafluoroethylene (PTFE) siccative quality, and the pH for the ammonia water conditioning system that mass fraction is 25% is added
Value is 10, and the mass content that polytetrafluoroethylene (PTFE) siccative in deionized water adjustment system is added is 60% (using system total weight as base
It is quasi-), obtain fluoroplastics aqueous liquid dispersion.
Comparative example 3
A kind of preparation method of fluoroplastics aqueous liquid dispersion, with embodiment 1, the difference is that:
In step (2), nonionic surface active agent is added to polytetrafluoroethylene (PTFE) concentration dispersion liquid, makes non-ionic surface
Active agent content is the 4.0% of polytetrafluoroethylene (PTFE) siccative quality, and the pH value for the ammonia water conditioning system that mass fraction is 25% is added
It is 10, the mass content that polytetrafluoroethylene (PTFE) siccative in deionized water adjustment system is added is 60% (using system gross mass as base
It is quasi-), obtain fluoroplastics aqueous liquid dispersion.
Test example
Fluoroplastics aqueous liquid dispersion prepared by embodiment 1-3 and comparative example 1-3 carries out the content of polytetrafluoroethylene (PTFE) siccative
With the viscosity at the content of surfactant, pH value, 25 DEG C, mechanical stability and fluoroplastics aqueous dispersion after 60 days at 25 DEG C
The measurement of the redispersibility of liquid.
1, the measurement of the content of the content and surfactant of polytetrafluoroethylene (PTFE) siccative
Test method is as follows:
The content of polytetrafluoroethylene (PTFE) (PTFE) siccative: about 10g dispersion liquid is taken in the aluminium bowl that diameter is 10cm, in 110 DEG C
It is 1 hour dry and then 1 hour dry in 300 DEG C, obtain heating residue, the calculation formula of the content (P) of polytetrafluoroethylene (PTFE) siccative
Are as follows:
P=Z/X × 100%
Wherein: P is the content of polytetrafluoroethylene (PTFE) siccative in dispersion liquid, is indicated with mass percent；Z is the matter of heating residue
It measures (g)；X is the quality (g) of dispersion liquid.
The content of surfactant: taking about 10g dispersion liquid in the aluminium bowl that diameter is 10cm, heats 1 hour in 110 DEG C
Gained heating residue I is heated 1 hour to heating residue I, and then in 300 DEG C, obtains heating residue II, surfactant contains
Measure the calculation formula of (N) are as follows:
N=[(Y-Z)/Z] × 100%
Wherein: N is the content of surfactant, is indicated with mass percent；Y is the quality (g) of heating residue I；Z is to add
The quality (g) of hot residue II.
2, the measurement of pH value and viscosity
With the pH value of pH meter measurement fluoroplastics aqueous liquid dispersion；It is surveyed with rotational viscometer (II+U.S. BROOKFIELD of DV-)
Determine viscosity of the fluoroplastics aqueous liquid dispersion at 25 DEG C.
3, at 25 DEG C mechanical stability measurement
Mechanical stability test method is as follows:
Appliance:
Peristaltic pump, silicone tube, 100mL beaker, 200 mesh nylon filtering cloths
Test method:
1. silicone tube is connected on peristaltic pump；
2. 150g fluoroplastics aqueous liquid dispersion is taken to be put into 100mL beaker；
3. controlling room temperature at 25 DEG C or so；
4. the output for adjusting peristaltic pump is 200mL/min；
5. fluoroplastics aqueous liquid dispersion is recycled 2 hours under the above conditions；
6. the condensation product in dispersion liquid is collected by filtration with 200 mesh filter screens after 2 hours, and condensation product is rinsed with pure water and is done
Only；
7. the condensation product of taking-up is put into baking oven, it is 2 hours dry at 120 DEG C；
8. measuring the mass M of condensation product after dry.
9. calculating the mechanical stability of fluoroplastics aqueous liquid dispersion, calculation method is as follows
Mechanical stability (%)=[M/ (150 × P)] × 100%,
Wherein, M is the quality (g) of condensation product；P is the content of polytetrafluoroethylene (PTFE) siccative, is indicated with mass percent.It is mechanical
Stability numerical value is smaller, and mechanical stability is better, and when mechanical stirring is less susceptible to agglutinator occur.
4, the measurement of redispersibility
Test method is as follows:
Appliance:
500mL graduated cylinder, 200 mesh nylon filtering cloths, constant temperature oven, sealing tape
Test method:
1. taking 500mL fluoroplastics aqueous liquid dispersion, it is added in 500mL graduated cylinder after being filtered with 200 mesh nylon filtering cloths；
2. graduated cylinder mouth is sealed with adhesive tape；
3. the graduated cylinder for sealing mouth is put into constant temperature oven, static storage 60 days；
4. adjusting constant temperature oven temperature is 25 DEG C；
5. being inverted graduated cylinder after taking out graduated cylinder after 60 days, whether observed quantity bottom has agglutinator；
The good fluoroplastics aqueous liquid dispersion of redispersibility, graduated cylinder bottom does not have agglutinator.
It is above-mentioned that test result is as follows shown in table 1.
The fluoroplastics aqueous liquid dispersion the performance test results of table 1 embodiment 1-3 and comparative example 1-3 preparation
The fluoroplastics of the fluoroplastics aqueous liquid dispersion of embodiment 1-3 preparation and comparative example 1-3 preparation as can be seen from the above table
Aqueous liquid dispersion is compared, and the redispersibility of the fluoroplastics aqueous liquid dispersion of embodiment 1-3 preparation improves significantly.Comparative example 3
Although the redispersibility of the dispersion liquid of preparation has improvement, but its mechanical stability is poor.So fluoroplastics prepared by the present invention
Aqueous liquid dispersion is while being obviously improved the redispersibility of fluoroplastics aqueous liquid dispersion, moreover it is possible to keep mechanically stable well
Property.
Claims (10)
1. a kind of high redispersibility fluoroplastics aqueous liquid dispersion, which is characterized in that the main component of the fluoroplastics aqueous liquid dispersion
Including polytetrafluoroethylene (PTFE), water-soluble resin PVP, surfactant and deionized water；The content of the polytetrafluoroethylene (PTFE) is fluorine
The 30~70% of plastics aqueous liquid dispersion quality, polytetrafluoroethylene (PTFE) is in terms of siccative；The content of the water-soluble resin PVP is poly-
The 0.05~0.3% of tetrafluoroethene siccative quality；The content of the surfactant is the 2.5 of polytetrafluoroethylene (PTFE) siccative quality
~4.0%.
2. high redispersibility fluoroplastics aqueous liquid dispersion according to claim 1, which is characterized in that the water-soluble tree
The average molecular weight of rouge PVP is 50000~1300000.
3. high redispersibility fluoroplastics aqueous liquid dispersion according to claim 1, which is characterized in that the surface-active
Agent is nonionic surface active agent；Preferred surfactant TMN-10.
4. the preparation method of the described in any item high redispersibility fluoroplastics aqueous liquid dispersions of claim 1-3, including step is such as
Under:
(1) surfactant is added into aqueous polytetrafluoroethyldispersion polymer fluid, the pH value of regulation system is 9~10, heating concentration
Obtain polytetrafluoroethylene (PTFE) concentration dispersion liquid；
(2) surfactant is added into polytetrafluoroethylene (PTFE) concentration dispersion liquid, keeps the total content of surfactant in system poly-
The 2.5~4% of tetrafluoroethene siccative quality are added water-soluble resin PVP, make water-soluble resin PVP content polytetrafluoroethylene (PTFE)
The 0.05~0.3% of siccative quality, regulation system pH value are 9~10, and the polytetrafluoroethylene (PTFE) that deionized water adjustment system is added is dry
The mass content of material is 30~70%, obtains high redispersibility fluoroplastics aqueous liquid dispersion.
5. the preparation method according to claim 4, which is characterized in that aqueous polytetrafluoroethyldispersion described in step (1) is poly-
The mass content for closing polytetrafluoroethylene (PTFE) siccative in liquid is 15~35%, and average grain diameter is 0.15~0.30 μm.
6. the preparation method according to claim 4, which is characterized in that the addition of surfactant described in step (1)
Amount is the 12~20% of polytetrafluoroethylene (PTFE) siccative quality.
7. the preparation method according to claim 4, which is characterized in that concentration heating stepses described in step (1) are as follows: will
System stands 3~4h after being heated to 75~90 DEG C, forms a large amount of transparent aqueous solution layers to upper layer, system is stood to room temperature, on
Layer forms transparent aqueous solution layer, and lower layer is the emulsion layer of concentration, removes upper layer aqueous layer, and polytetrafluoroethylene (PTFE) concentration point can be obtained
Dispersion liquid.
8. the preparation method according to claim 4, which is characterized in that the concentration point of polytetrafluoroethylene (PTFE) described in step (1)
The content of surfactant is the 1.5~2.5% of polytetrafluoroethylene (PTFE) siccative quality in dispersion liquid；The content of polytetrafluoroethylene (PTFE) siccative is
The 61~75% of dispersion liquid quality are concentrated in polytetrafluoroethylene (PTFE).
9. the preparation method according to claim 4, which is characterized in that using ammonia water conditioning system in step (1), (2)
PH value, the mass fraction of the ammonium hydroxide are 25~28%.
10. the application of the described in any item high redispersibility fluoroplastics aqueous liquid dispersions of claim 1-3 is applied to coating, glass
Glass cloth impregnating fabricated product.
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