CN111044550B - Method for rapidly determining stability of ink - Google Patents
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- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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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
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- G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
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- G—PHYSICS
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- 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
- G01N21/47—Scattering, i.e. diffuse reflection
- G01N2021/4704—Angular selective
- G01N2021/4709—Backscatter
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Abstract
The invention discloses a method for rapidly determining the stability of ink, which establishes 4 accelerated aging technical standards, applies a low-field nuclear magnetic analysis method and a multiple light scattering method to the stability research of emulsified ink for the first time, can know the stability state of the ink through the quantitative test data, can better reveal the internal structural characteristics of the ink, shortens the research and development period of the emulsified ink, and provides powerful technical support for research, development and production of the emulsified ink.
Description
Technical Field
The invention relates to a method for rapidly determining the stability of ink, and belongs to the technical field of ink testing.
Background
Emulsified ink is becoming accepted in the market due to its green and environment-friendly properties and excellent writing performance. In the production process of the emulsified ink, a certain amount of water is used for replacing an organic solvent, and the emulsified ink belongs to a thermodynamically unstable system, and can be agglomerated in the storage process, and the viscosity is increased. The pen industry generally uses a method of storing the product for 18 months and detecting the performance of the product by writing an index. The test method not only greatly prolongs the research and development period of the ink, but also mainly writes data, and can not well reflect the change of the internal structure and the property of the ink. Therefore, an emulsified ink testing method which is convenient and quick can not be found by means of an advanced analysis tester is also an important link in research and development.
The emulsified ink has the characteristics of dark color, multiple components and the like, so that the evolution process of a multiple dispersion system under different conditions is difficult to characterize and detect by adopting visual means such as a conventional optical microscope and the like. The methods such as an electron microscope and the like need to dilute and prepare samples, and the emulsified ink samples can cause recombination of an emulsified system after dilution, so that the actual form of the samples cannot be observed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for rapidly determining the stability of ink. 4 accelerated aging technical standards are established, the low-field nuclear magnetic analysis method and the multiple light scattering method are applied to stability research of the emulsified ink for the first time, the stability state of the ink can be known through the quantitative test data, the internal structural characteristics of the ink can be better revealed, and powerful technical support is provided for research, development and production of the emulsified ink.
A first object of the present invention is to provide a method for rapidly determining the stability of ink, comprising the steps of:
s1, rapidly aging qualified emulsified ink: carrying out quick ageing treatment on the qualified emulsified ink which is not stored to obtain quick ageing emulsified ink;
s2, establishing a rapid aging standard: testing stability parameters of the rapidly aged emulsified ink under different rapid aging treatment conditions by adopting low-field nuclear magnetism or multiple scattering, and setting treatment conditions with obvious stability parameters reduced as rapid aging standards;
s3, detecting the stability of the ink to be detected: testing the stability parameters of the ink to be tested under the rapid aging standard established in the step (2) by adopting the test conditions of low-field nuclear magnetism or multiple scattering which are the same as those of the step (2), and comparing the stability parameters with the stability parameters of the qualified emulsified ink under the rapid aging standard to judge the stability of the ink to be tested;
the rapid aging treatment is heating, heating and cooling circulation, cooling or centrifugation.
Further, the qualified emulsified ink is an emulsified ink capable of being stored for 18 months.
Further, the rapid aging standard of the heating treatment is that the heating treatment is stored for 20 to 40 days at the temperature of 40 to 60 ℃.
Further, the rapid aging standard of the heating and cooling circulation is that the materials are circularly stored for 2 to 5 times at the temperature of between 10 ℃ below zero and 0 ℃ below zero and the temperature of between 40 and 60 ℃ below zero, and the storage time is 20 to 30 hours each time.
Further, the cooling rapid aging standard is that the cooling rapid aging standard is stored for 5 to 10 days at the temperature of-10 to 0 ℃.
Further, the centrifugal rapid aging standard is 2000-6000 rpm, and the centrifugal rapid aging standard rotates for 1-10 hours.
Further, the low-field nuclear magnetism is used for testing water in different emulsifying states in the emulsified ink.
Further, the multiple scattering is used for measuring the relation between the back scattering light intensity and the height of the emulsified ink, and the stability parameter is calculated through the formula (1); the formula (1) is as follows:
wherein,,
d i is a stability parameter;
h is the specimen height at the time of testing;
∑ h |scan i (h)-scan i-1 (h) And I is the signal difference of the ith scanning and the i-1 scanning with the same height.
The beneficial effects of the invention are as follows:
the invention establishes 4 technical standards for accelerating aging, applies the low-field nuclear magnetic analysis method and the multiple light scattering method to the stability research of the emulsified ink for the first time, can not only know the stability state of the ink but also better reveal the internal structural characteristics of the ink through the quantitative test data, shortens the research and development period of the emulsified ink, and provides powerful technical support for research, development and production of the emulsified ink.
Drawings
FIG. 1 is a low field nuclear magnetic pattern of different samples;
FIG. 2 is a graph of the multiple light scattering back scattering and projected light intensity versus volume fraction for a styrene emulsion sample;
FIG. 3 is a graph of styrene emulsion particle size versus back-scattered light intensity;
FIG. 4 is a graph of the sample backscattering versus sample height for a homogeneous styrene emulsion;
FIG. 5 is a graph of backscattering versus height for styrene emulsions over time;
FIG. 6 is a graph of backscattering versus height for fresh samples of different emulsified inks versus 18 months of storage;
FIG. 7 is a graph of stability parameter test results for emulsified ink 388 after 18 months of storage;
FIG. 8 is a graph of the relationship between the high temperature treatment time and the stability parameter of different emulsified ink samples;
FIG. 9 is a graph of low temperature processing time versus stability parameters for different emulsified ink samples;
FIG. 10 is a graph showing the relationship between the number of high and low temperature treatments and the stability parameter of different emulsified ink samples;
FIG. 11 is a graph showing the relationship between the centrifugation time and the stability parameter of different emulsified ink samples.
Detailed Description
The present invention will be further described with reference to specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the present invention and practice it.
Low field nuclear magnetic analysis of emulsified ink emulsifying system
The aggregation state of water in emulsified ink is complex, and besides water in a free state, a part of water is dispersed into emulsion droplets by an emulsifier to be uniformly dispersed in an ink system. The low-field nuclear magnetic energy can be used for very accurately measuring and expressing water in an emulsion system, and the method for measuring the water content of the emulsion ink by using the low-field nuclear magnetic energy is also applied to measurement of the water content of the emulsion ink and stability analysis for the first time.
Aiming at the problems that the emulsified ink is dark in color, complex in system and difficult to analyze by using the conventional methods such as DLS, electron microscope and the like, the characterization work of the emulsified ink is carried out by using low-field nuclear magnetism. The typical spectrum is shown in figure 1.
From the results of the graph, it was found that the relaxation time of water in a free state in the low-field nuclear magnetism was 1000ms or more, the relaxation time was several tens ms or less, and most of the organic matters, and signals between several tens ms and 1000ms were water in different emulsion states. The signal between tens ms and 1000ms is changed when the same emulsified ink is measured under different storage time, and the change of the emulsion state water in the ink can be known through the displacement of the peak and the measurement of the height, so that the stability state of the ink is determined. We performed low field nuclear magnetic test analysis with a certain batch 388, 488, 788 of three color emulsion inks. The inks produced were divided into the following experimental control groups: the normal temperature natural condition storage group is sampled and analyzed once at intervals of 3 months, and samples stored for 3 months, 6 months, 12 months and 18 months at normal temperature are respectively represented by normal temperature of 3, normal temperature of 6, normal temperature of 12 and normal temperature of 18. Quick 1, quick 2, quick 3 and quick 4 respectively represent the quick ageing technology (1) of 4 kinds of treatment inks, and the treatment inks are placed in an electrothermal constant temperature incubator at 50 ℃ for 30 days; (2) Circularly storing for 3 times at-5 ℃ and 50 ℃ for 24 hours each time, namely storing for 24 hours at-5 ℃ and then storing for 24 hours at room temperature, and then storing for 24 hours in a 50 ℃ incubator, and sequentially circularly carrying out 3 times; (3) storing at-5 ℃ for 1 week; (4) The sample was placed in a centrifuge with a radius of 10cm and spun at 4000rpm for 5 hours.
Tables 1 and 388 Black emulsion ink Low field Nuclear magnetism Extrance and peak height
| Normal 3 | Often 6 | Normally 12 | Constant 18 | |
| Displacement of | 1.2；10.8；85.3 | 1.3；11.5；86.3 | 1.3；12.0；86.5 | 1.4；13.0；88.3 |
| Peak height | 18.4；10.3；4.0 | 18.0；10.3；4.3 | 17.0；9.5；5.0 | 15.4；9.3；5.5 |
| Fast 1 | Fast 2 | Fast 3 | Fast 4 | |
| Displacement of | 1.4；13.2；88.6 | 1.4；13.3；88.5 | 1.4；13.0；88.6 | 1.4；13.1；88.4 |
| Peak height | 15.2；9.1；5.6 | 15.3；9.3；5.5 | 15.3；9.2；5.6 | 15.2；9.3；5.6 |
Tables 2 and 488 Red emulsion ink Low field Nuclear magnetism Extrance and peak height
| Normal 3 | Often 6 | Normally 12 | Constant 18 | |
| Displacement of | 2.2；120.3 | 2.3；120.5 | 2.5；124.2 | 2.6；125.0 |
| Peak height | 16.9；3.5 | 16.7；3.6 | 15.8；3.8 | 15.4；3.9 |
| Fast 1 | Fast 2 | Fast 3 | Fast 4 | |
| Displacement of | 2.6；125.3 | 2.7；125.1 | 2.6；125.0 | 2.7；125.5 |
| Peak height | 15.4；4.0 | 15.3；3.9 | 15.5；3.9 | 15.4；4.0 |
Tables 3 and 788 blue emulsion ink Low field Nuclear magnetism Extrance and peak height
| Normal 3 | Often 6 | Normally 12 | Constant 18 | |
| Displacement of | 5.2；130.5 | 5.3；134.5 | 5.5；135.2 | 5.6；140.0 |
| Peak height | 17.9；3.0 | 16.3；3.2 | 15.8；3.4 | 15.4；3.5 |
| Fast 1 | Fast 2 | Fast 3 | Fast 4 | |
| Displacement of | 5.6；140.2 | 5.5；139.8 | 5.6；140.1 | 5.6；140.0 |
| Peak height | 15.4；3.4 | 15.3；3.5 | 15.4；3.6 | 15.2；3.5 |
By data comparison, we can find that the water in emulsion state in the ink changes along with the storage time of the emulsified ink, and the main reason for the phenomenon is that particles in emulsion state in the ink are agglomerated, so that the shape and the quantity of the water in emulsion state change. From the data we can also find that the data of speed 1-speed 4 are substantially consistent with the data of speed 18, indicating that the rapid aging method we employ is reliable and viable.
Multiple light scattering of emulsion system of emulsion ink
Multiple light scattering detection is based on the mie scattering theory, and the back-scattered light intensity BS and the transmitted light intensity T of light passing through a heterogeneous system depend on the heterogeneous particle size and particle concentration (volume fraction). Therefore, if a heterogeneous system is repeatedly scanned by adopting a multiple light scattering method to layer different positions of the emulsified ink, the variation of the back scattering light intensity in different scanning can be compared, and the variation of the particle size and concentration of heterogeneous particles in the emulsified ink can be characterized. The method can select 880nm light which is not obviously absorbed by water, organic solvent, polymer, pigment dye and other additives as a detection light source, so that the sample is not required to be diluted, and the nondestructive in-situ observation of the sample is realized.
We performed stability analysis tests on the samples using a turbidiscan multiple light scattering tester.
Screening work of test conditions was first performed using polystyrene emulsion, and the results are shown in fig. 2. From the results in the figure, it can be seen that as the volume fraction of polystyrene in the polystyrene emulsion increases, the intensity of transmitted light rapidly decreases, and the transmitted light approaches zero at a volume fraction of about 0.1%. With further increases in the polystyrene volume fraction, the intensity of the backscattered light is gradually increased. And the increase of the back scattering light intensity basically shows a linear relation within the volume fraction of 0.1-30%. By combining the composition of the emulsified ink sample, the distribution of the disperse phase in the heterogeneous ink system can be monitored by utilizing the back scattering light intensity in the multiple light scattering.
Further development of the variation of the intensity of the back-scattered light and the different styrene emulsion particles is carried out, and as shown in fig. 3, the back-scattered light intensity shows a trend of increasing and then decreasing with the variation of the size of the particles, and the demarcation point is at 0.6 microns. Thus, the change process of the heterogeneous dispersion particle size in the system can be judged according to the intensity change of the back-scattered light for the same sample.
For samples with uniform distribution, the detection of the back scattered light intensity is carried out according to different heights, the difference of the back scattered light intensity under different height states is recorded, the result shown in fig. 4 can be obtained, and the obtained result shows that the back scattered light of the samples under different heights is uniform and unchanged. When the sample is placed for a long time, sedimentation occurs due to gravity, the back scattering light intensity changes obviously along with the change of the height, and a typical spectrogram is shown in fig. 5. By counting this height variation, stability parameters can be calculated using the following formula, which can be used to characterize the sample particle size and the concentration gradient variation of the particles at different heights in the sample vial.
Wherein,,
d i is a stability parameter;
h is the specimen height at the time of testing;
∑ h |scan i (h)-scan i-1 (h) And I is the signal difference of the ith scanning and the i-1 scanning with the same height.
According to the method, the relationship between the back scattering light intensity and the height of the ink sample under different conditions is measured by using a multiple light scattering tester, and the stability parameter is calculated through instrument data, so that the method for rapidly analyzing the stability of the emulsified ink is constructed. The results of the preliminary tests are shown in fig. 6, and it can be found from the results in the graph that after the three samples of the emulsified ink are stored for 18 months, the intensity of the back scattered light is significantly higher than that of the fresh samples in the height range of scanning, which indicates that the samples are agglomerated, combined and the like during the storage period, and the particle size of the dispersed phase in the samples is increased.
Based on this result, we used a sample stored for eighteen months as a reference sample to determine its stability parameters, as shown in fig. 7, which shows the stability kinetics of 388-18 month stored samples over 24 hours, the fluctuation range of which is relatively large from the structural point of view, and the stability parameter value is about 1.65.
Example 1: high temperature storage time and stability parameters
The samples were placed in an electrothermal incubator at 50 ℃ for various times and their stability parameters were determined after restoring to room temperature. The results are shown in FIG. 8. From the results in the graph, it is shown that the change of the ink can be significantly accelerated under the high temperature storage at 50 ℃. The stability parameter of the emulsion ink is dramatically increased after about 29 days of high temperature storage, which indicates that the emulsion ink has changed stability. Therefore, if the storage time at 50 ℃ is set to be more than 30 days, the ink stability parameter is not changed, so that the ink is still in a stable state, and the internal disperse phase is not changed obviously.
Example 2: cryogenic temperature treatment and stability parameters
The samples were stored at-5℃for various periods of time and their stability parameters were determined after room temperature was restored. The results are shown in FIG. 9. As can be seen from the graph, after the emulsified ink is stored at-5 ℃ for different times, the stability parameter of the emulsified ink is continuously increased along with the extension of time, the emulsified ink is in a relatively stable state within 6 days, and after the emulsified ink exceeds 6 days, the stability parameter is sharply increased, so that the stability is greatly reduced. Thus, setting a storage time of 7 days can be used for the judgment of its long-term stability.
Example 3: alternating temperature treatment and stability parameters
The samples are circularly stored at the temperature of minus 5 ℃ and 50 ℃ for 24 hours respectively, namely, after being stored at the temperature of minus 5 ℃ for 24 hours, the samples are stored at room temperature for 24 hours, then the samples are put into a 50 ℃ incubator for 24 hours, the cycle numbers are sequentially carried out, and the stability parameters are measured after the temperature is restored to the room temperature. The results are shown in FIG. 10. The graph shows that the influence of the high-low temperature alternating preservation experiment on the stability is obvious, the emulsified ink shows better stability after 1 time of alternating preservation, but the stability is obviously reduced after 2 times of alternating treatment, and the stability is obviously reduced after 3 times of alternating treatment. Therefore, the high-low temperature alternation is set as the standard of stability judgment for 3 times.
Example 4: stability in centrifugal test
The samples were placed in a centrifuge having a radius of 10cm and centrifuged at 4000rpm for various periods of time, and the relationship between the centrifugation time and the stability parameter was measured, and the results are shown in FIG. 11.
From the figure, it can be seen that the stability effect of the emulsified ink sample after 3 hours of centrifugation was insignificant. Further prolonging the centrifugation time to more than 3 hours, the stability of the emulsified ink tends to be obviously reduced, and after the centrifugation time to more than 5 hours, the stability parameter of the emulsified ink is close to that of a sample stored for 18 months. The centrifugation time was set at 5 hours as a threshold for rapid analysis of stability.
In summary, through a series of examinations, the invention determines 4 stability rapid aging test standards of the emulsified ink: (1) placing in an electrothermal constant temperature incubator at 50 ℃ for 30 days; (2) Circularly storing for 3 times at-5 ℃ and 50 ℃ for 24 hours each time, namely storing for 24 hours at-5 ℃ and then storing for 24 hours at room temperature, and then storing for 24 hours in a 50 ℃ incubator, and sequentially circularly carrying out 3 times; (3) storing at-5 ℃ for 1 week; (4) The sample was placed in a centrifuge with a radius of 10cm and spun at 4000rpm for 5 hours. All of these 4 criteria are equivalent to 18 months of storage at normal temperature under natural conditions. And (3) performing stability analysis test on the sample by using a low-field nuclear magnetism TURBISCAN multiple light scattering tester, and establishing stability analysis data and a model. The rapid aging standard, the corresponding testing method and the data model have good reliability and practicality, and a very efficient quantitative description and testing method is provided for the stability test of the emulsified ink.
The above-described embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of the present invention is not limited thereto. Equivalent substitutions and modifications will occur to those skilled in the art based on the present invention, and are intended to be within the scope of the present invention. The protection scope of the invention is subject to the claims.
Claims (6)
1. A method for rapidly determining the stability of an ink, comprising the steps of:
s1, rapidly aging qualified emulsified ink: carrying out quick ageing treatment on the qualified emulsified ink which is not stored to obtain quick ageing emulsified ink; the rapid aging treatment is heating, heating and cooling circulation, cooling or centrifugation;
s2, establishing a rapid aging standard: the displacement and peak height of the rapidly aged emulsified ink and the qualified emulsified ink after 18 months of storage are tested by adopting a low-field nuclear magnetism test, and the stability parameters of the rapidly aged emulsified ink and the qualified emulsified ink after 18 months of storage are tested by adopting a multiple scattering test, wherein the displacement and peak height of the rapidly aged emulsified ink are consistent with the qualified emulsified ink after 18 months of storage, and the rapid aging treatment conditions of the stability parameters are also consistent with the qualified emulsified ink after 18 months of storage are determined as rapid aging standards of the emulsified ink; the multiple scattering is used for measuring the relation between the back scattering light intensity and the height of the emulsified ink, and calculating to obtain a stability parameter;
s3, detecting the stability of the ink to be detected: and (3) adopting the same multiple scattering test condition as that of the step (2), testing the stability parameter of the ink to be tested under the rapid aging standard established in the step (2), and comparing the stability parameter with the stability parameter of the qualified emulsified ink under the rapid aging standard to judge the stability of the ink to be tested.
2. The method of claim 1, wherein the heated flash aging is 40-60 o C, storing for 20-40 days.
3. The method according to claim 1, wherein the rapid aging criteria for the heating and cooling cycle is within the range of-10 to 0 o C and 40-60 o C is circularly stored for 2-5 times, each timeThe storage time is 20-30 h.
4. The method according to claim 1, wherein the cooling rapid aging standard is at-10 to 0 o C, storing for 5-10 days.
5. The method of claim 1, wherein the centrifugal rapid aging criteria is 2000 to 6000rpm rotation for 1 to 10 hours.
6. The method of claim 1, wherein the acceptable emulsified ink is an emulsified ink that is capable of being stored for 18 months.
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| WO2005092993A1 (en) * | 2004-03-26 | 2005-10-06 | Canon Kabushiki Kaisha | Active energy radiation hardenable water base ink and utilizing the same, method of inkjet recording, ink cartridge, recording unit and inkjet recording apparatus |
| CN103196690A (en) * | 2013-04-01 | 2013-07-10 | 上海晨光文具股份有限公司 | Method for quickly detecting stability of gel ink ball-point pen |
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| US7150996B2 (en) * | 2003-06-18 | 2006-12-19 | Stable Solutions, Inc. | Stability assessment of dispersions and emulsions |
| CN110441345A (en) * | 2019-09-06 | 2019-11-12 | 苏州大学 | Method based on the aqueous printing ink formula of low-field nuclear magnetic resonance Technology design |
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| CN103196690A (en) * | 2013-04-01 | 2013-07-10 | 上海晨光文具股份有限公司 | Method for quickly detecting stability of gel ink ball-point pen |
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