Summary of the invention
The object of the present invention is to provide a kind of dispersing method and the application of dispersion liquid in non-viscous paint thereof of PTFE super-fine powder, the present invention, in conjunction with the feature of PTFE super-fine powder, proposes a kind of dispersing method of PTFE super-fine powder, and the application of this dispersion liquid in non-viscous paint.Dispersion effect of the present invention is desirable, solves the technical deficiency of adding PTFE super-fine powder in existing non-viscous paint.
In order to solve the problems of the technologies described above, adopt following technical scheme:
A dispersing method for PTFE super-fine powder, is characterized in that comprising the steps:
(1) get the solvent of 5-7.5g cleaning, in the solvent of cleaning, add 7-20gPTFE super-fine powder, 0.5-0.75g dispersion agent, 22-33g resin, above-mentioned medicament is mixed, form mixed solution;
(2) be uniformly mixed liquid with water screw dispersion, stirring velocity is 200-300rmp, and jitter time is 1-4h, and dispersion temperature is less than 30 DEG C, obtains the dispersion liquid of PTFE super-fine powder.
Preferably, PTFE super-fine powder is obtained by telomerization method or irradiation method.
Preferably, in dispersion liquid, the weight of PTFE super-fine powder is T1, in dispersion liquid the gross weight of resin and PTFE super-fine powder be T2, T1/T2 be scope 15.2-44.9%.PTFE super-fine powder to account in dispersion liquid resin and PTFE super-fine powder gross weight mark is more low more easily disperses in theory, but what in fact PTFE super-fine powder accounted for dispersion liquid weighs less than 15.2%, the ratio of PTFE super-fine powder in dispersion liquid is very few, the layering in dispersion liquid of the static rear PTFE super-fine powder of dispersion liquid, the PTFE super-fine powder of bottom flocculates again, PTFE super-fine powder to account in dispersion liquid resin and PTFE super-fine powder gross weight higher than 44.9%, the mobility of PTFE super-fine powder in dispersion liquid is deteriorated, and causes difficulties in dispersion and uneven.
Preferably, the stirring velocity that the water screw dispersion of step (2) is stirred is 250rmp.
Preferably, the jitter time of step (2) is 3h.
Preferably, dispersion liquid fineness is less than or equal to 10 μm.The particle diameter of PTFE super-fine powder is 5-10 μm, if the fineness of dispersion liquid is more than 10 μm, illustrates that PTFE super-fine powder disperses in dispersion liquid uneven, there occurs secondary agglomeration.Can be used as the reference differentiating dispersion liquid quality.
Adopt the application of above-mentioned dispersion liquid in non-viscous paint, it is characterized in that comprising the steps:
(1) metering takes 0.5-0.75g dispersion agent, 22-33g resin, 0.8-1g flow agent, 0.3-0.5g defoamer, 0.1-0.5g not sticky auxiliary agent, 5-10g talcum powder, 5-8g solvent, 5-10g pigment, 1-2g aerosil, joins in grinding pot by above-mentioned medicament;
(2) grinding distribution 2-6h is carried out to the medicament in grinding pot, after filtration, obtain masterbatch;
(3) masterbatch is contributed in dispersion liquid, and stir, obtain the non-viscous paint of dispersion liquid;
(4) non-viscous paint is sprayed on the metal base after degreasing in advance, polishing, cleaning by the method for aerial spraying, after spraying, metal base is toasted at 220 DEG C 15min and form non-sticky metallic coating.
Preferably, dispersion agent is the polyphosphazene polymer hydroxy acid salt dispersion agent with active function groups.
Preferably, solvent is the mixed solvent of one or more compositions in N-BUTYL ACETATE, 1-Methoxy-2-propyl acetate and dimethylbenzene.
Preferably, resin is the one in urethane resin, epoxy polyamide resin, acrylic resin, resol, silicone resin.
Owing to adopting technique scheme, there is following beneficial effect:
The present invention is a kind of dispersing method and the application of dispersion liquid in non-viscous paint thereof of PTFE super-fine powder, and the present invention, in conjunction with the feature of PTFE super-fine powder, proposes a kind of dispersing method of PTFE super-fine powder, and the application of this dispersion liquid in non-viscous paint.It is simple that the inventive method has technique, easy to operate, do not need to increase new installation, this inventive method is adopted to improve PTFE super-fine powder and resin has good moisture dispersibility and dispersion stability, after storage there is not secondary agglomeration in PTFE super-fine powder, solves PTFE super-fine powder and add a difficult problem of disperseing in coating as additive to.Specifically there is following beneficial effect:
Non-viscous paint resin, solvent, dispersion agent, PTFE super-fine powder is comprised in the dispersing method of 1, PTFE super-fine powder, non-viscous paint resin is as external phase, PTFE super-fine powder is as disperse phase, solvent is used for adjusting the viscosity of dispersion liquid, and the PTFE super-fine powder that dispersion agent is used in stable resin prevents reflocculation.
Resin in the dispersing method of 2, PTFE super-fine powder of the present invention is dispersion medium, and the resin in described resin and non-viscous paint masterbatch is same resin, and is preferably polyester modified organic silicon resin.Compare with the resin-phase of other kinds: Good Heat-resistance, compared with the silicone resin (pure organosilicon, epoxy modified silicone) of other kinds: solidification value reduces makes construction convenient, with the Adhesion enhancement of metal base, demoulding persistence is greatly improved, snappiness strengthens makes impact property improve, and hardness does not obviously reduce simultaneously, resistance toheat improves has widened temperature applicable range.
Solvent action in the dispersing method of 3, PTFE super-fine powder of the present invention is adjustment viscosity, and described solvent is same solvent with the solvent in non-viscous paint masterbatch, and the mixed solvent of preferably N-BUTYL ACETATE and 1-Methoxy-2-propyl acetate 1:1 in mass ratio.Consumption is the 30-50% with solvent gross weight in non-viscous paint, preferably 50%, and consumption is high lower than the viscosity of 30% dispersion liquid, and dispersion effect is bad; Consumption is higher than 50%, and mixed solvent amount in non-viscous paint reduces, and dope viscosity is high, be unfavorable for grinding.
Dispersion agent in the dispersing method of 4, PTFE super-fine powder of the present invention, without particular requirement, is drawn materials easily, good to coating system consistency, has good lubrication dispersed, and can improve the package stability of coating to coating.Consumption is the 30-50% of dispersion agent gross weight in non-viscous paint, preferably 50%, and consumption declines lower than the less efficient dispersal of 30% PTFE super-fine powder, stability in storage; Consumption can affect the dispersion effect of silicone resin and other color stuffings in non-viscous paint higher than 50%.
PTFE super-fine powder in the dispersing method of 5, PTFE super-fine powder of the present invention is as the additive of the not sticky effect in non-viscous paint, and its Oil repellent is high, surface tension is little, migrates to film coated surface after film forming, thus gives the non-adhesion behavior of non-viscous paint coating excellence.PTFE micro mist can be obtained by telomerization method or irradiation method, and particle diameter is preferably 5-10 μm.Consumption is 5-50%, consumption lower than after 5% film forming its coatingsurface skewness, not its tack; Consumption is higher than 50%, and non-adhesion behavior is without enhancing, and simultaneously because addition is excessive, the mechanical property of coating can be deteriorated.Consumption, at 20-50%, although viscosity does not strengthen, can affect other performances of coating, preferred 5-20%.
6, dispersion liquid dispersion process temperature control < 30 DEG C of the present invention, the mobility of more than 30 DEG C PTFE super-fine powder is deteriorated and easily reunites, dispersion liquid does not produce heat at dispersion whipping process itself, if envrionment temperature is higher than 30 DEG C, take environment temperature reduction or the external type of cooling of clean container, as the in-house operation closed, can turn on the aircondition and make room temp < 30 DEG C, or clean container leads to water coolant with chuck or clean container carried out in the water-bath of mixture of ice and water dispersion stirring.
Adopt water screw to carry out dispersion in the dispersing method of 7, PTFE super-fine powder of the present invention to stir, utilize the screw blade that there is certain speed and rotate, PTFE super-fine powder and silicone resin are moved downward, after they strike clean container bottom surface, just flow to wall of container direction, after encountering wall of container, upwards return along wall again.The PTFE super-fine powder and the silicone resin that are in agitated pool upper strata are sucked by water screw, and by water screw depress, form the flow state of a volume circulation.The rotation of water screw also makes PTFE super-fine powder and silicone resin produce turning motion.Due to the viscosity of silicone resin and the resistance of stirred vessel wall, cause the velocity contrast between each layer liquid stream on turning radius direction.The silicone resin block moved with PTFE super-fine powder, is also subject to the shearing of high speed propeller leaf, effect of impact sometimes.Due to the synthesis of above-mentioned several motion, make the PTFE super-fine powder in agitated pool be in very disorderly kinestate, so PTFE super-fine powder is immersed loose, PTFE super-fine powder is uniformly dispersed.
8, lower than 200rmp, dispersion effect is poor, and jitter time is long, and efficiency is low, higher than 300rmp, can produce bubble in dispersion process, can have a negative impact to adding in non-viscous paint.
9, lower than 1h, disperse uneven, PTFE super-fine powder can not by abundant wetting and dispersing, and higher than 4h, although dispersion effect is good, dispersion efficiency is low.
Embodiment
Present invention comprises a kind of dispersing method of PTFE super-fine powder, prepared by following steps:
(1) get the solvent of 5-7.5g cleaning, in the solvent of cleaning, add 7-20gPTFE super-fine powder, 0.5-0.75g dispersion agent, 22-33g resin, above-mentioned medicament is mixed, form mixed solution.PTFE super-fine powder is obtained by telomerization method or irradiation method, and fusing point is 320-340 DEG C, apparent density 200-600g/cm
3, molecular weight 3-20 ten thousand, particle diameter 1-20 μm, be preferably 5-10 μm.In dispersion liquid, the weight of PTFE super-fine powder is T1, in dispersion liquid the gross weight of resin and PTFE super-fine powder be T2, T1/T2 be scope 15.2-44.9%.
Wherein dispersion agent is the polyphosphazene polymer hydroxy acid salt dispersion agent with active function groups, dispersion agent in the dispersing method of PTFE super-fine powder of the present invention is without particular requirement, as long as in principle can compatible with non-viscous paint system, have good lubrication dispersed and the auxiliary agent that can improve the package stability of coating can be selected, identical with the dispersion agent in non-viscous paint masterbatch; The solvent phase of solvent and non-viscous paint masterbatch with, be mixed solvents of one or more compositions in N-BUTYL ACETATE, 1-Methoxy-2-propyl acetate and dimethylbenzene, the mixed solvent of preferably butylacetate and 1-Methoxy-2-propyl acetate 1:1 in mass ratio.Solvent action in the dispersing method of PTFE super-fine powder of the present invention is adjustment viscosity, and the organic solvent that other additives such as the resin of non-viscous paint and dispersion agent dissolve can be made in theory all can to use; The resin-phase of resin and non-viscous paint masterbatch is same, is the one in urethane resin, epoxy polyamide resin, acrylic resin, resol, silicone resin, is preferably polyester modified organic silicon resin.
(2) liquid is uniformly mixed with water screw dispersion, stirring velocity is 200-300rmp, jitter time is 1-4h, and dispersion temperature is less than 30 DEG C (mobility of more than 30 DEG C PTFE super-fine powder is deteriorated and easily reunites), obtains the dispersion liquid of PTFE super-fine powder.The stirring velocity that wherein water screw dispersion is stirred is preferably 250rmp, and lower than 200rmp, dispersion effect is poor, and jitter time is long, and efficiency is low, higher than 300rmp, can produce bubble in dispersion process, can have a negative impact to adding in non-viscous paint; Jitter time is preferably 3h, lower than 1h, disperses uneven, and PTFE super-fine powder can not by abundant wetting and dispersing, and higher than 4h, although dispersion effect is good, dispersion efficiency is low; Dispersion liquid fineness is less than or equal to 10 μm.The particle diameter of PTFE super-fine powder is 5-10 μm, if the fineness of dispersion liquid is more than 10 μm, illustrates that PTFE super-fine powder disperses in dispersion liquid uneven, there occurs secondary agglomeration.
After obtaining above-mentioned dispersion liquid, adopt the application of above-mentioned dispersion liquid in non-viscous paint, comprise the steps:
(1) metering takes 0.5-0.75g dispersion agent, 22-33g resin, 0.8-1g flow agent, 0.3-0.5g defoamer, 0.1-0.5g not sticky auxiliary agent, 5-10g talcum powder, 5-8g solvent, 5-10g pigment, 1-2g aerosil, joins in grinding pot by above-mentioned medicament; Dispersion agent, resin and solvent phase in above-mentioned dispersion agent, resin and solvent and dispersion liquid with.Dispersion liquid solvent load is the 30-50% of solvent load in non-viscous paint, is preferably 50%; Dispersion liquid dispersant dosage is the 30-50% of dispersion agent in non-viscous paint, is preferably 50%
(2) grinding distribution 2-6h is carried out to the medicament in grinding pot, after filtration, obtain masterbatch;
(3) masterbatch is contributed in dispersion liquid, and stir, obtain the non-viscous paint of dispersion liquid;
(4) non-viscous paint is sprayed on the metal base after degreasing in advance, polishing, cleaning by the method for aerial spraying, after spraying, metal base is toasted at 220 DEG C 15min and form non-sticky metallic coating.PTFE super-fine powder is as the additive of the not sticky effect in non-viscous paint, and its Oil repellent is high, surface tension is little, migrates to film coated surface after film forming, thus gives the non-adhesion behavior of non-viscous paint coating excellence.Consumption is 5% ~ 50%, consumption lower than after 5% film forming its coatingsurface skewness, not its tack; Consumption is higher than 50%, and non-adhesion behavior is without enhancing, and simultaneously because addition is excessive, the mechanical property of coating can be deteriorated.Consumption, 20% ~ 50%, although viscosity does not strengthen, can affect other performances of coating, preferably 5% ~ 20%.
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
Step 1:(1) in clean solvent, add 5.0gPTFE super-fine powder, 0.5g dispersion agent, 6.5g mixed solvent, 28.0g superpolyester modified organic silicone resin successively, the weight of PTFE super-fine powder accounts for 15.2% of resin and PTFE super-fine powder gross weight in dispersion liquid; (2) carry out dispersion with water screw to stir, stirring velocity is 250rmp, and jitter time is 3h, and dispersion temperature is 25 DEG C, obtains the dispersion liquid of PTFE super-fine powder.
Step 2: metering takes 28.0g superpolyester modified organic silicone resin, 7.5g mixed solvent, 0.5g dispersion agent, 0.9g flow agent, 0.3g defoamer, 0.1g not sticky auxiliary agent, 10g talcum powder, 1.7g aerosil R972,10.0g white pigment, add in grinding pot, and grinding distribution 2-6h, filter the masterbatch obtaining non-viscous paint;
Step 3: joined by the masterbatch of the non-viscous paint obtained in step 2 in the dispersion liquid of the PTFE super-fine powder that step 1 obtains, and stir, namely obtains the non-viscous paint containing PTFE super-fine powder dispersion liquid.
The non-viscous paint made by aforesaid method is sprayed on the metal base after degreasing in advance, polishing, cleaning by the method for aerial spraying, toasts 15min and form non-sticky metallic coating after spraying at 220 DEG C of temperature.
Embodiment 2-10
Adopt method in the same manner as in Example 1, prepare dispersion liquid and non-viscous paint masterbatch according to such as table 1 and the weight of table 2, finally obtain non-sticky metallic coating:
The composition of table 1 embodiment 2-5
The composition of table 2 embodiment 6-10
The dispersion liquid prepared by embodiment of the present invention 1-10 adopts fineness method to carry out the evaluation of dispersing uniformity; The non-viscous paint prepared by embodiment of the present invention 1-10 carries out package stability evaluation, and method carries out sticking power, shock-resistant, the performance evaluation such as hardness and hot hardness, chemical reagent resistance, salt fog resistance, contact angle and non-viscosity after non-viscous paint being made test sample (solidification value 220 DEG C, set time 15min) according to the rules; Be applied in by non-viscous paint on rubber product molding mould, carry out demoulding evaluation, evaluation result refers to table 3 and table 4.
Assessment item 1: fineness method
Dispersion liquid dispersing uniformity of the present invention performs according to GB 1724-1979 " coating fineness assay method ".Judgement criteria is: in the groove deepest part of Hegman grind gage, instill several dispersion liquids, to be slightly unnecessaryly advisable can be full of groove, with held by both hands scraper, horizontal in the dull and stereotyped upper end of polishing, makes scraper and polishing planar surface perpendicular contact.In 3 seconds, the position of ditch groove depth is had by scraper to be pulled through to shallow position, make dispersion liquid be full of groove and flat board do not leave unnecessary dispersion liquid, after scraper is pulled through, (be no more than for 5 seconds) immediately and make sight line become 15 ~ 30 degree of angles with groove flat, uniform particles in groove is observed to light and appears place, take reading.When being revealed in other reticule if any individual particles, then reading and adjacent reticule scope are no more than three particles.
Assessment item 2: package stability
Package stability test of the present invention performs according to GB 6753.3-1986 " coating storage stability test method ".Judgement criteria is: loft drier non-viscous paint being put into 40 ± 2 DEG C stores 3 months, observe the changing conditions putting into non-viscous paint before and after loft drier, with non-viscous paint without or slight skinning, without sedimentation or sedimentation stirring is redispersible, viscosity B coefficent be less than 15% and non-viscous paint coating be qualified without particle, otherwise be defective.
Assessment item 3: sticking power
Sticking power test of the present invention performs according to GB 1720-1979 " paint film adhesion assay method ".Judgement criteria is: draw a circle on sample with adherometer, check the test sample integrated degree at each position in order, quadrille more than 70% as a certain position is intact, it is intact for being then decided to be this position, such as, otherwise should think damage, position 1 test sample is intact, sticking power is best, is decided to be one-level; Position 1 test sample damages and position 2 is intact, and sticking power takes second place, and is decided to be secondary.The like, seven grades is that sticking power is the poorest.
Assessment item 4: thermotolerance
Thermotolerance test of the present invention performs according to GB/T1735-2009 " mensuration of paint and varnish thermotolerance ".Judgement criteria is: after three pieces of test samples are put into 200 DEG C of constant temperature oven 16h, be chilled to temperature 25 ± 1 DEG C, compare with the one piece of test sample stayed in advance, check that being no less than two pieces of test samples is qualified without phenomenons such as aliquation, elephant skin, bubbling, cracking, variable colors, otherwise be defective.
Assessment item 5: shock-resistance
Shock-resistance test of the present invention performs according to GB/T 1732-1993 " the shock-resistant assay method of paint film ".Judgement criteria is: the test sample observing the position that is hit with 4 times of magnifying glasses, with flawless, wrinkle and the phenomenon such as to peel off be qualified, and records the maximum height of drop of weight.
Assessment item 6: hardness and hot hardness
Hardness of the present invention and hot hardness test are according to the B method in GB/T 6739-2006 " hardness of film pencil assay method ", and namely manual method performs.Hardness is the test carried out normal temperature test sample, and hot hardness is the test carried out the test sample be placed in 200 DEG C of constant temperature ovens after 10min.Evaluation criteria is: increase the hardness of pencil gradually until the defects such as permanent impression or visible abrade or scratch appear in test sample surface, the pencil hardness label adjacent with there is defect pencil is the hardness of test sample.
Assessment item 7: chemical reagent resistance
Chemical reagent resistance test of the present invention performs according to GB 9274-1988 " mensuration of paint and varnish resistant to liquid medium " first method.10%H is immersed in respectively by 2/3 of test sample
2sO
4, 10%NaOH, 10% NaCl solution in, evaluation method is as follows: rinse with clear water, after the globule being blotted with filter paper, with 4 times of magnifying glass observation test specimen surfaces with without peeling off, wrinkling, foaming, spot, get rusty, the phenomenon such as variable color and loss of gloss is qualified, otherwise is defective.
Assessment item 8: salt fog resistance
Salt-fog resistant test of the present invention performs according to GB/T 1771-2007 " mensuration of the resistance to neutral salt spray performance of paint and varnish ".Judgement criteria is: with without rust spot, bubble, the phenomenon such as to come off is qualified, otherwise is defective.
Assessment item 9: contact angle
Adopt contact angle instrument to carry out contact angle test to test sample, test fluid adopts deionized water, and probe temperature controls in (25 ± 1) DEG C.A sample at least will survey three times, gets its mean value.
Assessment item 10: not viscosity
The method that not viscosity test of the present invention can refer on GB/T 2792-1998 " pressure-sensitive adhesive tape 180 ° of peeling strength test methods " performs.Unlike testing herein: the non-viscous paint prepared by embodiment of the present invention 1-10 according to the rules method makes the stripping strength of test sample and the common sealing tape of one side, sealing tape width adopts 20mm ± 1mm.After sealing tape pastes test sample, under deadweight, test sample on carry out rollback with the speed of about 300mm/min with pressure roller and press three times (model and sealing tape bonding place have not allowed bubble to exist).By sealing tape free end doubling 180 degree, and from strip off adhesive face 25mm model.Sealing tape free end and model are clipped on upper and lower clamper respectively.Release surface and the trier line of force should be made to be consistent.Trier is peeled off continuously with 300mm/min ± 10mm/min lowering speed, and draws stripping curve by self-registering instrument.In the span peeled off, read a number every 20mm, at least read 3 numbers, ask its mean value.Stripping strength is less shows that the not viscosity of coating to viscous substance is better.Judgement criteria is: stripping strength is not more than 3N/cm
2then not think that viscosity is qualified, otherwise defective.
Assessment item 11: demoulding
The non-viscous paint adopting spraying coating process to be prepared by embodiment of the present invention 1-10 is coated to steel die surface, and solidifies 15min at 220 DEG C, forms non-sticky metallic coating, carries out demoulding evaluation subsequently to paracril, foamed silastic and viton.These three kinds of rubber only for explaining the demoulding of non-viscous paint of the present invention, instead of for limiting the use range of the present composition.
Demoulding judgement criteria is:
(1) if less (demoulding power is not more than 3N/10cm to demoulding power
2), goods and mould coating zero defect produce after demoulding, then thought a demoulding, and proceed the test of next demoulding, otherwise should stop demoulding test.Demoulding number of times is the demoulding number of times before stopping demoulding.
(2) be used on rubber item mould with 3500 times for standard, see goods or mould damaged degree.
The properties test result of the non-viscous paint of table 3 embodiment 1-5
The properties test result of the non-viscous paint of table 4 embodiment 6-10
These are only specific embodiments of the invention, but technical characteristic of the present invention is not limited thereto.Any based on the present invention, for solving substantially identical technical problem, realize substantially identical technique effect, done ground simple change, equivalent replacement or modification etc., be all covered by among protection scope of the present invention.