CN109580554A - A kind of test method of emulsion paint storage stability - Google Patents
A kind of test method of emulsion paint storage stability Download PDFInfo
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- CN109580554A CN109580554A CN201811447750.8A CN201811447750A CN109580554A CN 109580554 A CN109580554 A CN 109580554A CN 201811447750 A CN201811447750 A CN 201811447750A CN 109580554 A CN109580554 A CN 109580554A
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- storage stability
- emulsion paint
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- test method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/59—Transmissivity
Abstract
The invention discloses a kind of test methods of emulsion paint storage stability, the condition of emulsion paint normal storage is simulated under acceleration conditions, and then acquisition stores sample and carries out the evaluation of three aspect of a point water degree, illumination and deposition degree to judge storage stability, simulates 1 during heat is stored up) viscosity reduction；2) dissociated ion amount increases；3) flocculated generation；And pass through the viscosity that aqueous latex paint is diluted with water to 63 ± 2Ku, the variation tendency of light transmittance is tested in the graduated cylinder of high transparency, to calculate its very poor standard deviation and determine the storage stability test method of the present invention of product relative to former 50 DEG C of heating store 30 days test method can more rapidly, the storage stability of quantitative judgement product, determine that the time shorten to the 1/10 of former heat storage standard time, is equivalent to the 1/120 of normal temperature storage time.Detecting efficiency and data reliability are greatly improved.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of test method of emulsion paint storage stability.
Background technique
It is decentralized medium that emulsion paint, which is by water, and pigments and fillers and auxiliary agent is added, obtained uniform using lotion as film forming matter
Suspension.In the quality requirement of emulsion paint: 1) construction is smooth；2) coating is reliable, this two o'clock is wanted at all to its quality
It asks.
Emulsion paint requires its liquid condition when production, storage, transport are constructed to the end, and no change has taken place, there is no
Point water, return thick, the problems such as sinking to the bottom, agglomerate, being gelled could smooth construction.Water provides environment friendly, safety as medium
Many advantages, such as.But very big trouble is also brought to storage stability.The surface of water can be high, so that pigments and fillers particle is being ground
The primary particle formed in dispersion process is difficult to be stabilized, i.e., causes problems during storage.These problems are after all
It is exactly primary particle during storage due to the problem of ceaselessly Blang is with occurring agglomeration, aggregation, flocculation.
Within the quality guarantee period of existing emulsion paint, it how to be allowed the problem of storing state do not occur, in existing technology, GB
The prolonged storage for mentioning us in 6753.3-86 and simulating by thermmal storage emulsion paint, under 50 ± 2 DEG C of acceleration environment
30d is stored, is roughly equivalent to store half a year to 1 year under natural environment.The principle of this method: it 1) is increased point under heated condition
Dissipate the impact kinetic energy of particle Brownian movement, it is easier to collision flocculation；2) viscosity of emulsion paint is reduced；3) part pigment is increased
The solubility of filler increases metal ion in solution amount.And the result of simulation, by the leakproofness of storage container, temperature is to water
Volatilization and condensation, the influence of the factors such as central temperature and container edge temperature difference, the property of can refer to is low.Although this method is current
It can only rest on and qualitatively determine storage stability, but equipment needed for method is simple, simulation is direct, still by most enterprises institute
Using.
30 days storage periods were a short slabs in research and development process, referring to present " resin latex dope "
Elementary item tests curing cycle all at 7 days in standard, i.e., all tests can be completed in 8 days.It in the period for shortening storage experiment, mentions
The quantitative judgement of storage stability experiment detecting result after high dispersive, storage will be become by providing more rapidly reliable basis for research and development of products
Deposit the key of stability test.
Summary of the invention
In view of the deficienciess of the prior art, the present invention provides a kind of test method of emulsion paint storage stability, the cream
The test method of shellac varnish storage stability can shorten to the time of stability test within 8 days, and energy quicklook is quantitative
Read test data.
The technical solution of the present invention is as follows:
A kind of test method of emulsion paint storage stability, comprising the following steps:
S1: emulsion paint to be measured is stood to placement 23~25 hours in 25 DEG C &50%RH constant-temperature constant-humidity environments；
S2: the emulsion paint after S1 is stood is sampled according to GB 3186-82 regulation, and is mounted in the PP container of 330ml
In, dispersed by the way that water is added in high speed disperser, the emulsion paint is diluted to sample of the viscosity within the scope of 63 ± 2Ku；
S3: sample made from S2 is tested into the viscosity at 25 DEG C by Brookfield viscosimeter, then packing rapidly
Into high transparent glass graduated cylinder, after the graduated cylinder is sealed, it is placed in 25 DEG C &50%RH climatic chambers, standing 70~
74 hours；
S4: taking out graduated cylinder, then successively detects in the environment of not shaking and not rocking: 1) point regimen condition；2) illumination light transmission
Rate；3) degree is settled；
S5: storage stability evaluation, comprising:
(1) divide the standards of grading of water degree
9: passing through: suspending completely, compared with before storage in climatic chamber, do not change；
6: acceptable: to there is clear layering to occur: the volume of hyaline layer≤filling volume of sample 2%；
3: more serious: to there is obvious light yellow to transparent layering to occur: filling 2% < of volume of sample layering volume≤filling examination
Sample volume 30%；
0: serious: to there is obvious buff to transparent layering to occur: layering volume > filling volume of sample 30%；
(2) standards of grading of illumination
9: standard deviation≤10
Standard deviation≤15 6:10 <
3:15 < standard deviation
0: starting illumination > 100lex；
(3) standards of grading of degree are settled
9: having no obvious sediment, graduated cylinder bottom is completely exposed；
6: having slight precipitating, the graduated cylinder center that probe touches is still exposed；
3: without apparent pit after thering is more precipitating, probe to touch；
0: having after thering is more precipitating, probe to touch obvious recessed；
Be finally conclusive evaluation with " passing through " or " not passing through ", when the scoring of three above test item >=6 timesharing,
It is assessed as passing through, conversely, not passing through；And according to rating score can relatively each sample storage stability superiority and inferiority.
Further, 1000~1200rpms of revolving speed of the S2 high speed dispersion machine disperses 10~15min.
Further, the volume of the S3 graduated cylinder be 250ml, minimum division value 2ml.
Further, the detection of the S4 illumination light transmittance uses laser illumination instrument, and the laser illumination instrument includes illumination
Probe, laser c LASSII molded line light source and measurement magazine, the center of surface and laser c LASSII molded line light of the illumination probe
The laser light incident direction that source is projected is vertical.
Further, the laser c LASSII molded line light source is that the high-penetration that output power is 0.8~1.0mW is linearly green
Color laser beam, beam exit mouth diameter≤4mm.
Further, the laser illumination instrument uses in black space, the black space to all wavelengths reflect because
Several and nominal value difference is no more than 0.2%.
Further, the black space is that black velvet material completely spreads D65 light source box space.
The utility model has the advantages that
The present invention has the advantages that test method of the present invention stores 30 days test methods relative to former 50 DEG C of heating
Can more rapidly, the storage stability of quantitative judgement product, determine that the time shorten to the 1/10 of former heat storage standard time, be equivalent to
The 1/120 of normal temperature storage time.Detecting efficiency and data reliability are greatly improved.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the very poor curve graph of illumination.
Fig. 2 is illumination tester structure chart.
Wherein, 1. illumination probe, 2. laser c LASSII molded line light sources 3. measure 4. graduated cylinder of magazine.
Specific embodiment
To keep the present invention more readily apparent understandable, hereby it is illustrated with preferred embodiment combination attached drawing.
Instrument used in a kind of test method of emulsion paint storage stability of the present invention and material are as follows:
Drying box: it is able to maintain 50 ± 2 DEG C of air dry oven；
Climatic chamber: T:25 ± 2 DEG C, the container of H:50 ± 5% are able to maintain；
Container: 330ml spiral cover sample smooth surface straight barrel type PP tank；
Balance: scale division value 0.01g；
Viscosimeter: digital rotational viscometer (Brookfield) and paddle rotor Stormer (Stormer) viscosimeter；
Graduated cylinder: minimum division value 2ml, the high penetration cylinder of maximum volume 250ml high borosilicate sand；
High speed disperser: maximum speed 2000rpms matches the two-sided tooth-like dispersion impeller in periphery；
Stopwatch: scale division value 0.1s；
Thermometer: 0~50 DEG C, 0.5 DEG C of scale division value；
Toolsetting: paint toolsetting, long 100mm or so, wide 12mm of cutter head or so；
Laser light source: green CLASS II type stabilized lasers source；
Measurement magazine: see Fig. 2；
Colour temperature illumination photometer: 0.1~99990lx range, Ev xy colour system, 2% ± 1 display numerical value of Ev precision；
Stainless steel probe: 201 materials, the long 400mm probe cross section of probe areIsometrical cylinder is constituted, end of probe
HaveBall.
Test method is as follows:
(1) sample being taken and prepares:
By the regulation of GB 3186-82 " samplings of coating products ", aliquot part or laboratory field fabrication are taken out
Sample to be tested (room temperature 24 hours after the completion of being made) be respectively classified into 2 it is canned enter container in.
(2) storage and experimental condition
It is packed into the 2/3 of container standard volume, and is the high speed disperser of container diameter 1/2 with dispersion disk diameter, uses water
It stirs and is sufficiently stirred within 10~15 minutes under sample viscosity is adjusted to standard environment within the scope of 61~65Ku, under 1000rpms
It is even, will adjust it is viscous after sample be drained in graduated cylinder with probe, total injection amount is not lower than the 90% of graduated cylinder maximum range, on liquid level
Side must not have contamination coating, avoid the test for influencing experimental result；Graduated cylinder oral area is covered with adhesive plaster, to the amount of being filled in graduated cylinder and always
It weighs and records by balance again.Graduated cylinder is put into climatic chamber and is stored, multiple title is taken out after 3 days, it is small to be filled with weight loss
Graduated cylinder in 1% stores sample to be effective
(3) estimation of stability:
3.1 points of water inspections:
Effective storage sample after acceleration is taken out from climatic chamber, then the case where not vibrating or not shaking container
Down in visual graduated cylinder liquid top plan, read at once, avoid the graduated cylinder upper end steam as caused by the temperature difference agglutination caused by read
Number error, reads the intersection of even laminating to the amount of liquid on liquid level top.
Divide the evaluation of water degree:
9: passing through: suspending completely, compared with before storage in climatic chamber, do not change.
6: acceptable: to there is clear layering to occur: the volume of hyaline layer≤filling volume of sample 2%.
3: more serious: to there is obvious light yellow to transparent layering to occur: filling 2% < of volume of sample layering volume≤filling examination
Sample volume 30%.
0: serious: to there is obvious buff to transparent layering to occur: layering volume > filling volume of sample 30%
The test of 3.2 illumination:
As shown in Fig. 2, graduated cylinder 4 is put in measurement magazine 3, laser c LASSII molded line light source 2 is opened, passes through illumination probe 1
Measurement.The capacity record of the illumination measured and corresponding graduated cylinder is got off.
Wherein, the linear laser incident direction that the center of surface of illumination probe 1 and laser c LASSII molded line light source 2 project
Vertically to core.The laser c LASSII molded line light source 2 is the linear green laser beam of CLASS II (0.8~1.0mW) high-penetration,
Beam exit mouth diameter≤4mm, other such as blues and red co-energy laser, the linear and energy retentivity of light is not so good as green
Color it is good.Entire illumination test environment is black space, difference of the black space to all wavelengths reflectivity and nominal value
No more than 0.2%, it is preferable to use black velvet material completely spreads D65 light source box space.
The evaluation of illumination
The viscosity of paint vehicle is adjusted to 61~65Ku or so to be determined, is put into climatic chamber after capping, is stored 3 days
After take out, when being higher than 100lex such as starting point illumination, then the storage stability of paint vehicle is bad, the problems such as being also easy to produce point water loose colour,
It is assessed as 0 point.Otherwise 7 grades very poor according to product when standard deviation determine that grade form is as follows:
9: standard deviation≤10
Standard deviation≤15 6:10 <
3:15 < standard deviation
0: starting illumination > 100lex
3.3 sedimentation degree inspections
The paint vehicle tested has been toppled over from graduated cylinder, if there is skinning on surface, carefully should avoid influencing with toolsetting removal existing
The observation of elephant is inverted and starts to be placed back into just after vertically toppling over 1min, then cleans graduated cylinder with probe drainage tap water and repeats to walk
Operation, is cleaned twice repeatedly.It is gently placed on the beds of precipitation after having cleaned with the round end of probe.
The evaluation of sedimentation degree
9: having no obvious sediment, graduated cylinder bottom is completely exposed；
6: having slight precipitating, the graduated cylinder center that probe touches is still exposed；
3: without apparent pit after thering is more precipitating, probe to touch；
0: having after thering is more precipitating, probe to touch obvious recessed；
The method of the invention is finally conclusive evaluation with " passing through " or " not passing through ", when three above test item
Scoring >=6 timesharing, be assessed as passing through, conversely, do not pass through, but according to rating score can relatively each sample stable storing
The superiority and inferiority of property.
It is as follows using storage stability test of the above method to commercially available 5 kinds of latex paint formulations:
Formula 1:
Auxiliary material includes following components
Calcined kaolin 10%~12%
Calcium carbonate 15%~18%
Talcum powder 5%~8%
Formula 2:
Auxiliary material includes following components
Calcined kaolin 5%~10%
Calcium carbonate 18%~20%
Talcum powder 10%~13%
Formula 3:
Auxiliary material includes following components
Calcined kaolin 8%~10%
Calcium carbonate 36%~40%
Formula 4:
Auxiliary material includes following components
Calcined kaolin 4%~5%
Calcium carbonate 30%~32%
Talcum powder 15%~20%
Formula 5:
Auxiliary material includes following components
Kaolin 10%~15%
Calcium carbonate 30%~32%
Above five sections of emulsion paints are the product for meeting national standard test.
It was found that it can be found that when dilution is modulated in experiment after being tested by the different group experiments to same experimental program
When viscosity is lower than 60Ku, sample occurs dividing that water layer thickness sharply increases and illumination light transmittance shows as sharply declining,
When viscosity continues to drop below 50Ku, product divides the rising of water layer turbidity, light transmittance decrease.In conjunction with above 5 groups of experimental programs
50 DEG C of accelerating storages, 30 days results and previous product normal temperature storage as a result, choose 60Ku or more section test phenomenon
It matches with the data of 50 DEG C of thermmal storages, meets application.And polyisomenism with test before it is identical.
The dilution viscosity above that this programme passes through the different amounts of being watered is within the scope of 63 ± 2Ku, is further tested.
Table 1: the dilution BROOKFIELD viscosity table of formula 1~5
50 DEG C of storages are carried out to paint sample and compare new method: 1) being diluted；2) it stands；3) survey light transmission, it can be found that paint sample according to
Test method of the present invention can show that stability compares screening quickly.
Table 2: the illumination result that 1~5# of case study on implementation is tested after standing constant temperature 1 day 3 days
By upper table it can be found that accelerating 1# and 5# Case comparison during thermmal storage to stablize, illumination corresponds to very poor
Mean variation gradient is also smaller, it may be assumed that (location A illumination-B location illumination)/(location A/position 10ml-B/10ml) tests number
Value such as table 3:
Table 3: the illumination very poor gradient table of each experiment case study is calculated when fixed upper limit
From figure 1 it appears that the variation tendency in figure will tend towards stability after selected point >=8 (7 grades).
It then passes through to 7 very poor standard deviation distributions it can be found that when 7 grades or more very poor data standard differences are less than 15
When, the storage stability of product is good.
4:7 grades of table or more standard deviation table
| 7 grades | 11.2 | 17.1 | 203.6 | 29.2 | 9.5 |
| 8 grades | 12.6 | 17.9 | 201.0 | 31.6 | 9.6 |
| 9 grades | 13.9 | 18.7 | 198.0 | 34.3 | 9.9 |
| 10 grades | 14.6 | 19.8 | 195.0 | 33.7 | 10.1 |
By the numerical tabular of standard deviation, we can be found that the coating of stable storing, and the very poor distribution of illumination is very uniform,
And both less than 15.
In summary: we can be found that:
1) diluted viscosity is at 63 ± 2Ku, and the storage sample of emulsion paint sample can comparatively fast obtain available illumination；
2) experiment needs to obtain illumination data by the device to test of Fig. 2；
3) illumination test initial point position < 100lex is qualification, does not otherwise have to the judgement for carrying out down two steps；
4) illumination test data only needs top-down 8 or more points；
5) standard deviation is asked to be distributed the very poor of test data, the storage stability performance of product is good when numerical value is less than 15, number
It is worth the smaller the better.
When subtle variation, visual method is also not enough to solve the problems, such as quantitative.This test method passes through in CLASS
The different luminous fluxes in the different height beds of precipitation are collected using illumination instrument under the action of the laser beam of II energy.If light made
For the particle for passing through space, then reach the light beam of curved surface luminous flux and unit interval inner impact curved surface population at
Ratio.The light for reaching illumination photometer measurement spherical surface is related with the amounts of particles of the suspended matter of liquid.
By a series of experiment, our integrated applications have carried out the knot that laser illumination equipment staticly settles dilution in 3 days
Fruit is detected, during simulating heat storage completely, 1) and viscosity reduction；2) dissociated ion amount increases；3) flocculated generation；And
And the viscosity by the way that aqueous latex paint to be diluted with water to 63 ± 2Ku, the variation of light transmittance is tested in the graduated cylinder of high transparency
Trend, to calculate its very poor standard deviation and determine the storage stability of product.30 days energy are stored relative to former 50 DEG C of heating
More rapidly, the storage stability of quantitative judgement product determines that the time shorten to the 1/10 of former heat storage standard time, is equivalent to often
The 1/120 of warm storage time.Detecting efficiency and data reliability are greatly improved.
It should be pointed out that as described above is only to explain the preferred embodiments of the invention, it is right accordingly to be not intended to
The present invention is subject to any form of limitation, therefore all have any modification for making the related present invention under identical spirit
Or change, it should all be included in the scope that the invention is intended to protect.
Claims (7)
1. a kind of test method of emulsion paint storage stability, which comprises the following steps:
S1: emulsion paint to be measured is stood to placement 23~25 hours in 25 DEG C &50%RH constant-temperature constant-humidity environments；
S2: the emulsion paint after S1 is stood is sampled according to GB 3186-82 regulation, and in the PP container of 330ml, is led to
It crosses addition water to disperse under high speed disperser, the emulsion paint is diluted to sample of the viscosity within the scope of 63 ± 2Ku；
S3: sample made from S2 is tested into the viscosity at 25 DEG C by Brookfield viscosimeter, is then dispensed into height rapidly
It in saturating glass cylinder, after the graduated cylinder is sealed, is placed in 25 DEG C &50%RH climatic chambers, it is small to stand 70~74
When；
S4: taking out graduated cylinder, then successively detects in the environment of not shaking and not rocking: 1) point regimen condition；2) illumination light transmittance；3)
Sedimentation degree；
S5: storage stability evaluation, comprising:
(1) divide the standards of grading of water degree
9: passing through: suspending completely, compared with before storage in climatic chamber, do not change；
6: acceptable: to there is clear layering to occur: the volume of hyaline layer≤filling volume of sample 2%；
3: more serious: to there is obvious light yellow to transparent layering to occur: filling 2% < of volume of sample layering volume≤filling sample body
Product 30%；
0: serious: to there is obvious buff to transparent layering to occur: layering volume > filling volume of sample 30%；
(2) standards of grading of illumination
9: standard deviation≤10
Standard deviation≤15 6:10 <
3:15 < standard deviation
0: starting illumination > 100lex；
(3) standards of grading of degree are settled
9: having no obvious sediment, graduated cylinder bottom is completely exposed；
6: having slight precipitating, the graduated cylinder center that probe touches is still exposed；
3: without apparent pit after thering is more precipitating, probe to touch；
0: having after thering is more precipitating, probe to touch obvious recessed；
Be finally conclusive evaluation with " passing through " or " not passing through ", when the scoring of three above test item >=6 timesharing, evaluation
To pass through, conversely, not passing through；And according to rating score can relatively each sample storage stability superiority and inferiority.
2. the test method of emulsion paint storage stability according to claim 1, which is characterized in that the S2 high speed point
1000~1200rpms of revolving speed of machine is dissipated, 10~15min is dispersed.
3. the test method of emulsion paint storage stability according to claim 1, which is characterized in that the appearance of the S3 graduated cylinder
Product is 250ml, minimum division value 2ml.
4. the test method of emulsion paint storage stability according to claim 1, which is characterized in that the S4 illumination light transmission
The detection of rate use laser illumination instrument, the laser illumination instrument include illumination probe (1), laser c LASSII molded line light source (2) and
It measures magazine (3), the laser light incident side that the center of surface and laser c LASSII molded line light source (2) of the illumination probe (1) project
To vertical.
5. the test method of emulsion paint storage stability according to claim 4, which is characterized in that the laser
CLASSII molded line light source (2) is the linear green laser beam of high-penetration that output power is 0.8~1.0mW, beam exit mouth diameter
≤4mm。
6. the test method of emulsion paint storage stability according to claim 4, which is characterized in that the laser illumination instrument
It is used in black space, the black space is no more than 0.2% to the difference of all wavelengths reflectivity and nominal value.
7. the test method of emulsion paint storage stability according to claim 6, which is characterized in that the black space is
Black velvet material completely spreads D65 light source box space.
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| CN201811447750.8A CN109580554B (en) | 2018-11-29 | 2018-11-29 | Method for testing storage stability of latex paint |
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|---|---|---|---|
| CN201811447750.8A CN109580554B (en) | 2018-11-29 | 2018-11-29 | Method for testing storage stability of latex paint |
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Cited By (1)
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| CN114264577A (en) * | 2021-12-30 | 2022-04-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for rapidly detecting dispersion stability of nano titanium dioxide in oil phase |
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| CN114264577A (en) * | 2021-12-30 | 2022-04-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for rapidly detecting dispersion stability of nano titanium dioxide in oil phase |
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| Publication number | Publication date |
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| CN109580554B (en) | 2021-07-02 |
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