CN103196690A - Method for quickly detecting stability of gel ink ball-point pen - Google Patents
Method for quickly detecting stability of gel ink ball-point pen Download PDFInfo
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Abstract
The invention provides a method for quickly detecting the stability of a gel ink ball-point pen. The method comprises the steps of testing initial writing perform, ink outgoing amount and dry-resisting day number of a gel ink ball-point pen refill and viscosity, surface tension, granularity, ZETA potential and a back scattering curve of ink in the refill, and utilizing test results of the initial writing perform, the ink outgoing amount, the dry-resisting day number, the viscosity, the surface tension, the granularity, the ZETA potential and the back scattering curve to judge a stable storage period of the gel ink ball-point pen. On the premise that an ink system is not damaged, the method performs comprehensive monitoring of performance indexes related with the ink pigment dispersion stability and the system rheological stability within a short period of time, adopts multiple parameters and combines the ink stability to perform evaluation and quickly and reliably judges the stability of the gel ink ball-point pen.
Description
Technical field
The present invention relates to a kind of Neutral writing ink ball pen stability method for quick, specifically, relate to a kind of method for quick of color type Neutral writing ink ball pen long-time stability situation.
Background technology
Neutral writing ink in last century the eighties by the invention of Japan's system company, the nineties enters domestic bringing into use.Neutral writing ink has water-base ink and oily ink advantage concurrently, the Neutral writing ink ball pen that it is made, and it is smooth to write out China ink, comfortable feel, the dense and fast drying of person's handwriting is liked by people quite, make it develop into current most popular writing implement rapidly, occupied ball pen half market share approximately at present.Neutral writing ink is gel ink (gel-ink), and gel belongs to the steady state that is situated between in dynamics, its stability and prescription design itself, and preparation technology, accumulating and service condition are closely related.Common stability problem shows as mainly that pigment returns slightly in the process of depositing, flocculation even precipitation situation, and perhaps the system multiviscosisty causes situations such as rheological property variation.
The stable storage phase of Neutral writing ink ball pen normally requires to be not more than 80% in relative humidity, and environment temperature is under 0～40 ℃ the condition, places through nature, and it is smooth to keep writing out China ink all the time, and feel is along sliding, and the person's handwriting color and luster is stable etc.Generally believe that in the industry the qualified Neutral writing ink ball pen stable storage phase should be not less than 12 months.
At present, Neutral writing ink ball pen stability testing method commonly used is the keeping quality test A method of QB/T2625-2011 " Neutral writing ink ball pen and pen core ", requires at 50 ± 2 ℃, and pen core or pen kept flat 10 days, still met every index of writing quality.Described test period is grown (10 days), even and stand the test can't prove that still its stability reaches requirement because when test findings is had objection, the B method is just for the arbitration test method.
Keeping quality test B method requires at 40 ± 2 ℃, and humidity is that pen core or pen kept flat 90 days, still met every index of writing quality under 55 ± 5% the condition.Described test period long (90 days).
In addition, also have now by high temperature or centrifugal mode, accelerate the variation of dispersed system from different aspects, analyze theoretically and disclose the stability of ink situation in conjunction with the Arrhenius experimental formula, this method has certain degree of discrimination to stability of ink.For Neutral writing ink, color type Neutral writing ink especially, high temperature mainly are that to accelerate reunion, the resin of pigment particles cancellated aging and then cause the variation of system particle size or size-grade distribution and the variation of viscosity or other rheological properties; And centrifugal mainly be the surface property, rheological property etc. that accelerate the come-up of pigment particles causes pigment particles with cancellated separation of resin sedimentation or some auxiliary agent molecule and then change system.
Diao Hongliang, Liu Shoujun etc. disclose the method that detects Neutral writing ink stability respectively by high speed centrifugation and high-temperature baking from different perspectives in " fast characterizing of Neutral writing ink stability (China's system pen 2007.1) ", be specially after Neutral writing ink passes through 72 hours two kinds of destructive tests of 8000rpm (relative centrifugal force(RCF) is 4250 acceleration of gravity) high speed centrifugation 30 minutes and 60 ℃ of bakings respectively, by examining or check the Separation of Solid and Liquid degree of its centrifugal dilution, heating back pigment disperses to have or not flocculation, the mean grain size change degree, whether viscosity can keep stable four indexs that wait, in conjunction with a large amount of experimental results, judge whether its shelf-life reaches 18 months.
But, also there are some problems in said method: in the step that detects absorbance, the sample ink is diluted by certain multiple, originally particle has flocculated or the situation of reuniting has been destroyed (dispersion) artificially, or surpassed the limit, ink system is destroyed, obvious layering occurs, the reliability of test difficult of proof; Down baking is after 72 hours at 60 ℃ for some Neutral writing ink, and the system of its ink is destroyed, changes greatlyyer, and its result can only illustrate that this ink is through can't stand 60 ℃ of high temperature; Whether the stability that can only judge ink reaches 18 months, has certain limitation; Only the physicochemical property to barreled or bottled ink detects, and has ignored the applied environment of ink reality.In the situation of change of ink character under pen core storage China ink pipe or the written environment certainly and different under barreled or the bottled environment, the experimental result that obtains at barreled or bottled ink can't reflect the practical application situation, the particularly stability of usability aspect of Neutral writing ink ball pen comprehensively, accurately, objectively.
Therefore, this area needs a kind of method that detects Neutral writing ink ball pen stability fast, comprehensively, reliably that overcomes above-mentioned technical matters.
Summary of the invention
For overcoming above-mentioned technical matters, the inventor is through studying for a long period of time, a kind of method of Neutral writing ink ball pen stability fast detecting has been proposed, in conjunction with from a plurality of test items and corresponding detection method thereof multi-faceted, multidimensional formation, come the stability of synthetic determination Neutral writing ink ball pen with testing result.
On the one hand, the invention provides a kind of method of fast detecting Neutral writing ink ball pen stability, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve that described method comprises first write performance to described Neutral writing ink ball pen, go out ink in China ink amount and anti-dried fate and the described pen core are measured, and utilize described write performance just, stable storage phase that the measurement result that goes out China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve is judged described Neutral writing ink ball pen.
In an embodiment according to said method of the present invention, described mensuration comprises: the physicochemical property to ink in the usability of described pen core and the pen core is measured, and obtains described write performance just, goes out the primary data of China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve; Treated pen core is carried out the physicochemical property of ink in usability and the pen core and measures, obtain described write performance just, go out China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve through the time data; Utilize measured primary data and through the time data, just write performance, hundred meters go out China ink amount fluctuation rate of change absolute value, anti-dried fate rate of change absolute value, viscosity rate of change absolute value, viscosity ratio rate of change absolute value, surface tension variations rate absolute value, granularity rate of change absolute value, ZETA potential change rate absolute value and stability parameter to obtain handling the back.
In another embodiment according to said method of the present invention, described rate of change absolute value refer to (through the time data-primary data)/absolute value of primary data * 100%, described stability parameter is measured by the stability analysis instrument, according to described through the time backward scattering curve and described initial backward scattering curve calculation draw.
In another embodiment according to said method of the present invention, described processing is included in the baking oven that temperature is 45～55 ℃ (preferred 50 ℃) and kept 3～5 days, leaves standstill then 60 minutes; And be 2000～3000rpm at rotating speed, relative centrifugal force(RCF) is to keep 30～90 minutes (preferred 30 minutes) in the horizontal centrifuge of 800～1800 acceleration of gravity (preferred 2500rpm, relative centrifugal force(RCF) is that 1250 gravity accelerate), leaves standstill then 60 minutes.
In another embodiment according to said method of the present invention, the mensuration of described viscosity comprises by rotational rheometer respectively with 1.256s
-1And 4500s
-1Shear rate ink in the described pen core is carried out viscosity measurement, obtain 1.256s
-1Viscosity data and 4500s
-1Viscosity data.
In another embodiment according to said method of the present invention, described viscosity rate of change absolute value adopts 4500s
-1Viscosity data calculate.
In another embodiment according to said method of the present invention, described viscosity ratio is 1.256s
-1Viscosity data and 4500s
-1The ratio of viscosity data.
In another embodiment according to said method of the present invention, the mensuration of described granularity comprises by laser particle size analyzer carries out the measurement of granularity D50 to ink in the described pen core.
In another embodiment according to said method of the present invention, described Neutral writing ink ball pen comprises black Neutral writing ink ball pen, blue Neutral writing ink ball pen and red Neutral writing ink ball pen.
In another embodiment according to said method of the present invention, when viscosity rate of change absolute value is lower than 20%, viscosity ratio rate of change absolute value is lower than 10%, surface tension variations rate absolute value is lower than 10%, granularity rate of change absolute value is lower than 20%, ZETA potential change rate absolute value is lower than 10%, black Neutral writing ink ball pen, the stability parameter of blue Neutral writing ink ball pen and red Neutral writing ink ball pen is lower than 0.1 respectively, 5 and 5, handling the back pen core just writes in the 100mm normal, hundred meters go out China ink amount fluctuation rate of change absolute value and are lower than 45%, anti-dried fate rate of change absolute value is lower than at 45% o'clock, and the described Neutral writing ink ball pen stable storage phase is more than 12 months.
In another embodiment according to said method of the present invention, when viscosity rate of change absolute value is lower than 10%, viscosity ratio rate of change absolute value is lower than 5%, surface tension variations rate absolute value is lower than 5%, granularity rate of change absolute value is lower than 10%, ZETA potential change rate absolute value is lower than 5%, black Neutral writing ink ball pen, the stability parameter of blue Neutral writing ink ball pen and red Neutral writing ink ball pen is lower than 0.04 respectively, 0.9 and 2, handling the back pen core initially writes namely normal, hundred meters go out China ink amount fluctuation rate of change absolute value and are lower than 25%, anti-dried fate rate of change absolute value is lower than at 25% o'clock, and the described Neutral writing ink ball pen stable storage phase is more than 24 months.
Method of the present invention is detected object with the ink stock solution in the Neutral writing ink ball pen, research technique in conjunction with centrifugation accelerates and high temperature acceleration, be prerequisite not destroy ink system, carry out comprehensive monitoring to the physicochemical property that relates to ink pigment dispersion stabilization and system rheology stability and the usability of pen core within a short period of time, judges the long-time stability of the actual usability of Neutral writing ink ball pen fast, comprehensively, reliably.
Description of drawings
Also with reference to following specifying, those of ordinary skill in the art will be better appreciated by above-mentioned and other feature and advantage of the present invention by reference to the accompanying drawings.In the accompanying drawings:
Fig. 1 is the initial backward scattering curve map of A type black Neutral writing ink ball pen;
Fig. 2 be A type black Neutral writing ink ball pen through the time backward scattering curve map;
Fig. 3 is the initial backward scattering curve map of the blue Neutral writing ink ball pen of Type B;
Fig. 4 be the blue Neutral writing ink ball pen of Type B through the time backward scattering curve map;
Fig. 5 is the initial backward scattering curve map of the red Neutral writing ink ball pen of C type; And
Fig. 6 be the red Neutral writing ink ball pen of C type through the time backward scattering curve map.
Embodiment
Be described more specifically the present invention below by embodiment, but the present invention is not limited to these embodiment.
In a kind of preferred implementation of the present invention, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve that the method for fast detecting Neutral writing ink ball pen stability of the present invention comprises first write performance to described Neutral writing ink ball pen, go out ink in China ink amount and anti-dried fate and the described pen core are measured, and utilize described write performance just, stable storage phase that the measurement result that goes out China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve is judged described Neutral writing ink ball pen.
Wherein said mensuration comprises: the physicochemical property to ink in the usability of described pen core and the pen core is measured, and obtains described write performance just, goes out the primary data of China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve; Treated pen core is carried out the physicochemical property of ink in usability and the pen core and measures, obtain described write performance just, go out China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve through the time data; Utilize measured primary data and through the time data, just write performance, hundred meters go out China ink amount fluctuation rate of change absolute value, anti-dried fate rate of change absolute value, viscosity rate of change absolute value, viscosity ratio rate of change absolute value, surface tension variations rate absolute value, granularity rate of change absolute value, ZETA potential change rate absolute value and stability parameter to obtain handling the back.
Wherein said rate of change absolute value refer to (through the time data-primary data)/absolute value of primary data * 100%, described stability parameter is measured by the stability analysis instrument, according to described through the time backward scattering curve and described initial backward scattering curve calculation draw.
It is to keep 3～5 days in 45～55 ℃ the baking oven that wherein said processing is included in temperature, leaves standstill then 60 minutes; And be 2000～3000rpm at rotating speed, relative centrifugal force(RCF) is to keep 30～90 minutes in the horizontal centrifuge of 800～1800 acceleration of gravity, leaves standstill then 60 minutes.
Wherein said Neutral writing ink ball pen comprises black Neutral writing ink ball pen, blue Neutral writing ink ball pen and red Neutral writing ink ball pen.
The mensuration of each parameter is specific as follows in the method for the present invention:
Rotational rheometer is adopted in the measurement of viscosity, respectively with 1.256s
-1And 4500s
-1Shear rate, detect in the initial pen core ink samples and handle ink samples in the pen core of back, measure ink 1.256s
-1Viscosity data and 4500s
-1Viscosity data, with 4500s
-1Viscosity data be foundation, obtain viscosity rate of change absolute value by following formula:
Wherein, viscosity ratio rate of change absolute value adopts above-mentioned data, obtains viscosity ratio and viscosity ratio rate of change absolute value by following formula:
Surface tension instrument is adopted in capillary measurement, detects in the initial pen core ink samples respectively and handles ink samples in the pen core of back, draw respectively the initial surface tension value and through the time surface tension value, obtain surface tension variations rate absolute value by following formula:
Laser particle degree analyser is adopted in the measurement of granularity, detect ink samples and the granularity D50 value of handling ink samples in the pen core of back in the initial pen core respectively, draw respectively primary particles degree D50 value and through the time granularity D50 value, obtain granularity rate of change absolute value by following formula:
Granularity rate of change absolute value is granularity D50 rate of change absolute value among the present invention.
The ZETA potentiometer is adopted in the measurement of ZETA current potential, detects in the initial pen core ink samples respectively and handles ink samples in the pen core of back, draw respectively initial ZETA potential value and through the time ZETA potential value, obtain ZETA potential change rate absolute value by following formula:
The mensuration of backward scattering curve adopts the stability analysis instrument, ink in the initial pen core is packed in the special test bottle, put into the initial backward scattering curve of stability analysis instrument specimen, after measuring the same processing of bottle taking-up process and pen core, put into again stability analysis instrument specimen through the time backward scattering curve, according to the degree of backward scattering curvilinear motion, the stability analysis instrument can calculate the stability parameter of this ink samples automatically.
The aforementioned stable parameter is more little, shows that the stability of this ink is more good.Owing to ink color is different its photo absorption performance and light transmission are had nothing in common with each other, therefore, stability parameter is pressed color classification relatively, and this method is temporarily with the most frequently used black, blueness and red classification.
Just write performance obtains the first write performance testing result of first write performance and the processing back pen core of initial pen core respectively according to 7.1 test methods of QB/T2625-2011 " Neutral writing ink ball pen and pen core ";
Go out the China ink amount according to 6 general test apparatuses, material and the condition of QB/T2625-2011 " Neutral writing ink ball pen and pen core ", according to 7.2 test methods, obtain respectively initial hundred meters of initial pen core go out China ink amount data and handle the back pen core through the time hundred meters go out China ink amount data, obtain hundred meters by following formula and go out the fluctuation of China ink amount and hundred meters and go out the fluctuate absolute values of rate of change of China ink amount:
Hundred meters go out=hundred meters of China ink amount fluctuations and go out China ink amount maximal value-hundred and meter go out China ink amount mean value
Anti-dried fate is tested in 50 ℃ of baking ovens by horizontal storage that pen core is raised one's hat, regularly detect its usability, maximum up to can not accord with Q B/T2625-2011 " Neutral writing ink ball pen and pen core " standard-required the time is deposited the anti-dried fate that fate is this pen core, measure the anti-dried fate of initial pen core and processing back pen core respectively, obtain initial anti-dried fate with through the time anti-dried fate, obtain the absolute value of anti-dried fate rate of change by following formula:
Through repetitious test and calculating, the criterion of Neutral writing ink ball pen stability method for quick of the present invention is as shown in table 1.
Table 1
Criterion according to table 1, when viscosity rate of change absolute value is lower than 20%, viscosity ratio rate of change absolute value is lower than 10%, surface tension variations rate absolute value is lower than 10%, granularity rate of change absolute value is lower than 20%, ZETA potential change rate absolute value is lower than 10%, black Neutral writing ink ball pen, the stability parameter of blue Neutral writing ink ball pen and red Neutral writing ink ball pen is lower than 0.1 respectively, 5 and 5, handling the back pen core just writes in the 100mm normal, hundred meters go out China ink amount fluctuation rate of change absolute value and are lower than 45%, anti-dried fate rate of change absolute value is lower than at 45% o'clock, and the Neutral writing ink ball pen stable storage phase is more than 12 months.
Criterion according to table 1, when viscosity rate of change absolute value is lower than 10%, viscosity ratio rate of change absolute value is lower than 5%, surface tension variations rate absolute value is lower than 5%, granularity rate of change absolute value is lower than 10%, ZETA potential change rate absolute value is lower than 5%, black Neutral writing ink ball pen, the stability parameter of blue Neutral writing ink ball pen and red Neutral writing ink ball pen is lower than 0.04 respectively, 0.9 and 2, handling the back pen core initially writes namely normal, hundred meters go out China ink amount fluctuation rate of change absolute value and are lower than 25%, anti-dried fate rate of change absolute value is lower than at 25% o'clock, and the Neutral writing ink ball pen stable storage phase is more than 24 months.
As used herein, term " viscosity " refers to kinetic viscosity.
As used herein, term " granularity D50 " refer to the sample fluid mechanics median particle diameter that obtained by dynamic light scattering method.
Slipping plane when As used herein, term " ZETA current potential " refer to that charged particle in the sample its surface-stable layer and diffusion layer under electric field action relatively move with respect to sample in away from the potential difference (PD) of certain point of this slipping plane.
As used herein, term " stability parameter " refer to the value of the sign sample separation degree that gone out through certain change calculations of handling the back scattered light intensity according to whole sample by the stability analysis instrument.
As used herein, term " stable storage phase " refer to that the Neutral writing ink ball pen deposits still living forever most the storage time of accord with Q B/T2625-2011 " Neutral writing ink ball pen and pen core " standard code of back its physicochemical property and usability at normal temperatures.
Embodiment
The following example will be described more specifically the present invention.
Embodiment 1
A type black Neutral writing ink ball pen (from Shanghai M ﹠ G Stationery Inc., perfusion black Neutral writing ink, coupling P type 6700.5 stainless steel nibs)
(1) above-mentioned ball pen is divided into two groups, one group places under the room temperature, another group kept 3 days in temperature is 50 ℃ baking oven earlier, left standstill then 60 minutes, be 2500rpm at rotating speed then, relative centrifugal force(RCF) is middle the maintenance 30 minutes of horizontal centrifuge (the safe instrument of Changsha English, TG21C table model high speed centrifuge) of 1250 acceleration of gravity, leaves standstill then 60 minutes.
(2) two groups of pen cores that respectively step (1) obtained carry out just writing, going out the test of China ink amount according to the test method among the QB/T2625-2011 " Neutral writing ink ball pen and pen core ", obtain pen core is just write, hundred meters go out the China ink amount primary data and through the time data; And with the pen core level of raising one's hat put into 50 ℃ of baking oven internal memories put into the test of capable dry tolerance obtain the anti-dried fate of pen core primary data and through the time data (seeing Table 2);
(3) ink of getting respectively in two groups of pen cores that step (1) obtains is an amount of, adopt rotary flow graph (German Haake, the rotary flow graph of RS6000), surface tension instrument (the auspicious instrument in Shanghai side, the full-automatic surface tension instrument of QBZY), (american wheat very restrains laser particle degree analyser, Nanotrac Wave nano particle size instrument), ZETA potentiometer (U.S. Colloidal Dynamics, the Zetaprobe potentiometric analyzer), ink detects respectively in two groups of pen cores that step (1) is obtained, drawing ink is 1.256s in shear rate
-1And 4500s
-1The time viscosity, surface tension, granularity D50, ZETA current potential primary data and through the time data (seeing Table 2); Ink in the initial pen core is packed in the special test bottle, put into the initial backward scattering curve of stability analysis instrument specimen, with measure bottle take out through and the same processing of pen core after, put into again stability analysis instrument specimen through the time backward scattering curve, see Fig. 1 and Fig. 2 respectively;
(4) calculate hundred meters of pen cores according to the measurement result of step (2) and step (3) and go out China ink amount fluctuation rate of change absolute value, anti-dried fate rate of change absolute value, viscosity rate of change absolute value, viscosity ratio rate of change absolute value, surface tension variations rate absolute value, granularity rate of change absolute value, ZETA rate of change absolute value and stability parameter (seeing Table 3), and the stable storage phase of A type black Neutral writing ink ball pen is judged in the criterion of reference table 1.
Table 2
| Project | Initial value | Through duration |
| 1.256s -1Viscosity/cp | 4137.1 | 4455.7 |
| 4500s -1Viscosity/cp | 22.5 | 23.12 |
| Surface tension/mN.m -1 | 29.74 | 30.15 |
| Granularity D50/ μ m | 1.052 | 1.135 |
| Zeta potential/mV | -46.6 | -45.6 |
| The backward scattering curve | See Fig. 1 | See Fig. 2 |
| First write performance | Initially namely write normal | Initially namely write normal |
| Hundred meters go out China ink amount fluctuation/mg/100m | 12 | 14 |
| Anti-dried fate/sky | 9 | 7 |
Table 3
The criterion of reference table 1 judges that the stable storage phase of A type black Neutral writing ink ball pen can reach more than 24 months.
In order to verify the correctness of this result of determination, with same A type black Neutral writing ink ball pen horizontal positioned at room temperature, regularly detect according to QB/T2625-2011 " Neutral writing ink ball pen and pen core " standard during this time, discovery every index qualification rate in the time of 24 months is 100% still, this shows that the stable storage phase of this A type black Neutral writing ink ball pen is more than 24 months.
Embodiment 2
Detection method is identical with embodiment 1, difference is that used sample is that the blue Neutral writing ink ball pen of Type B is (from Shanghai M ﹠ G Stationery Inc., pour into blue Neutral writing ink, mate 6700.5 stainless steel nibs), test result sees Table 4, result of calculation sees Table 5, and the testing result of backward scattering curve is seen Fig. 3, Fig. 4.
Table 4
| Project | Initial value | Through duration |
| 1.256s -1Viscosity/cp | 1839.23 | 2070.1 |
| 4500s -1Viscosity/cp | 53.47 | 56.19 |
| Surface tension/mN.m -1 | 30.16 | 30.81 |
| Granularity D50/ μ m | 2.37 | 2.71 |
| Zeta potential/mV | -34.1 | -32 |
| The backward scattering curve | See Fig. 3 | See Fig. 4 |
| First write performance | Initially namely write normal | Initially namely write normal |
| Hundred meters go out China ink amount fluctuation/mg/100m | 18 | 23 |
| Anti-dried fate/sky | 6 | 4 |
Table 5
The criterion of reference table 1 is judged the stable storage phase of the blue Neutral writing ink ball pen of Type B more than 12 months, but is not reached 24 months.
In order to verify the correctness of this result of determination, with same A type Neutral writing ink ball pen horizontal positioned at room temperature, regularly detect according to QB/T2625-2011 " Neutral writing ink ball pen and pen core " standard during this time, discovery every index qualification rate in the time of 12 months still is 100%, but defective situation appears in above-mentioned four indices in the time of 24 months, this shows the stable storage phase of the blue Neutral writing ink ball pen of this Type B more than 12 months, but do not reach 24 months.
Embodiment 3
Detection method is identical with embodiment 1, difference is that used sample is that the red Neutral writing ink ball pen of C type is (from Shanghai M ﹠ G Stationery Inc., pour into red Neutral writing ink, mate 6700.5 stainless steel nibs), test result sees Table 6, result of calculation sees Table 7, and the testing result of backward scattering curve is seen Fig. 5, Fig. 6.
Table 6
| Project | Initial value | Through duration |
| 1.256s -1Viscosity/cp | 2094.7 | 2750.7 |
| 4500s -1Viscosity/cp | 35.48 | 39.37 |
| Surface tension/mN.m -1 | 28.3 | 30.09 |
| Granularity D50/ μ m | 1.918 | 2.38 |
| Zeta potential/mV | -30.8 | -28.4 |
| The backward scattering curve | See Fig. 5 | See Fig. 6 |
| First write performance | Initially namely write normal | Write normal in the 100mm |
| Hundred meters go out China ink amount fluctuation/mg/100m | 19 | 28 |
| Anti-dried fate/sky | 4 | 2 |
Table 7
The criterion of reference table 1 judges that the stable storage phase of the red Neutral writing ink ball pen of C type is in 12 months.
In order to verify the correctness of this result of determination, with same A type Neutral writing ink ball pen horizontal positioned at room temperature, regularly detect according to QB/T2625-2011 " Neutral writing ink ball pen and pen core " standard during this time, defective situation appears in discovery above-mentioned four indices in the time of 12 months, this shows that the stable storage phase of the red Neutral writing ink ball pen of this C type is no more than 12 months.
By the result of embodiment 1～3 as seen, method of the present invention is prerequisite not destroy ink system, carry out comprehensive monitoring to the performance index that relate to ink pigment dispersion stabilization and system rheology stability within a short period of time, adopt multiparameter in conjunction with the stability of ink is estimated, judge the stability of Neutral writing ink ball pen fast, comprehensively, reliably.
Those skilled in the art should be noted in the discussion above that embodiment described in the invention only is exemplary, can make various other replacements, changes and improvements within the scope of the invention.Thereby, the invention is not restricted to above-mentioned embodiment, and only be defined by the claims.
Claims (12)
1. the method for a fast detecting Neutral writing ink ball pen stability, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve that described method comprises first write performance to described Neutral writing ink ball pen, go out ink in China ink amount and anti-dried fate and the described pen core are measured, and utilize described write performance just, stable storage phase that the measurement result that goes out China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve is judged described Neutral writing ink ball pen.
2. according to the process of claim 1 wherein that described mensuration comprises: described pen core is measured, obtained described write performance just, go out the primary data of China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve; Treated pen core is measured, obtain described write performance just, go out China ink amount, anti-dried fate, viscosity, surface tension, granularity, ZETA current potential and backward scattering curve through the time data; Utilize measured primary data and through the time data, just write performance, hundred meters go out China ink amount fluctuation rate of change absolute value, anti-dried fate rate of change absolute value, viscosity rate of change absolute value, viscosity ratio rate of change absolute value, surface tension variations rate absolute value, granularity rate of change absolute value, ZETA potential change rate absolute value and stability parameter to obtain handling the back.
3. according to the method for claim 2, wherein said rate of change absolute value refer to (through the time data-primary data)/absolute value of primary data * 100%, described stability parameter is measured by the stability analysis instrument, according to described through the time backward scattering curve and described initial backward scattering curve calculation draw.
4. according to the method for claim 2, it is to keep 3～5 days in 45～55 ℃ the baking oven that wherein said processing is included in temperature, leaves standstill then 60 minutes; And be 2000～3000rpm at rotating speed, relative centrifugal force(RCF) is to keep 30～90 minutes in the horizontal centrifuge of 800～1800 acceleration of gravity, leaves standstill then 60 minutes.
5. according to the method for claim 4, it is to keep 3 days in 50 ℃ the baking oven that wherein said processing is included in temperature, leaves standstill then 60 minutes; And be 2500rpm at rotating speed, relative centrifugal force(RCF) is to keep 30 minutes in the horizontal centrifuge of 1250 acceleration of gravity, leaves standstill then 60 minutes.
6. according to the method for claim 2, the mensuration of wherein said viscosity comprises by rotational rheometer respectively with 1.256s
-1And 4500s
-1Shear rate described Neutral writing ink is carried out viscosity measurement, obtain 1.256s
-1Viscosity data and 4500s
-1Viscosity data.
7. according to the method for claim 6, its medium viscosity rate of change absolute value adopts 4500s
-1Viscosity data calculate.
8. according to the method for claim 6, wherein said viscosity ratio is 1.256s
-1Viscosity data and 4500s
-1The ratio of viscosity data.
9. according to the method for claim 2, the mensuration of wherein said granularity comprises the measurement of described Neutral writing ink being carried out granularity D50 by laser particle size analyzer.
10. according to the method for aforementioned each claim, wherein said Neutral writing ink ball pen comprises black Neutral writing ink ball pen, blue Neutral writing ink ball pen and red Neutral writing ink ball pen.
11. the method according to aforementioned each claim, wherein work as viscosity rate of change absolute value and be lower than 20%, viscosity ratio rate of change absolute value is lower than 10%, surface tension variations rate absolute value is lower than 10%, granularity rate of change absolute value is lower than 20%, ZETA potential change rate absolute value is lower than 10%, black Neutral writing ink ball pen, the stability parameter of blue Neutral writing ink ball pen and red Neutral writing ink ball pen is lower than 0.1 respectively, 5 and 5, handling the back pen core just writes in the 100mm normal, hundred meters go out China ink amount fluctuation rate of change absolute value and are lower than 45%, anti-dried fate rate of change absolute value is lower than at 45% o'clock, and the described Neutral writing ink ball pen stable storage phase is more than 12 months.
12. the method according to aforementioned each claim, wherein work as viscosity rate of change absolute value and be lower than 10%, viscosity ratio rate of change absolute value is lower than 5%, surface tension variations rate absolute value is lower than 5%, granularity rate of change absolute value is lower than 10%, ZETA potential change rate absolute value is lower than 5%, black Neutral writing ink ball pen, the stability parameter of blue Neutral writing ink ball pen and red Neutral writing ink ball pen is lower than 0.04 respectively, 0.9 and 2, handling the back pen core initially writes namely normal, hundred meters go out China ink amount fluctuation rate of change absolute value and are lower than 25%, anti-dried fate rate of change absolute value is lower than at 25% o'clock, and the described Neutral writing ink ball pen stable storage phase is more than 24 months.
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| CN111044550B (en) * | 2019-12-25 | 2023-06-30 | 苏州雄鹰笔墨新材料有限公司 | Method for rapidly determining stability of ink |
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