CN107063906A - Powder moisture absorption degree of agglomeration quantitatively characterizing method - Google Patents
Powder moisture absorption degree of agglomeration quantitatively characterizing method Download PDFInfo
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- CN107063906A CN107063906A CN201611167451.XA CN201611167451A CN107063906A CN 107063906 A CN107063906 A CN 107063906A CN 201611167451 A CN201611167451 A CN 201611167451A CN 107063906 A CN107063906 A CN 107063906A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
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- G—PHYSICS
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
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Abstract
The invention discloses a kind of powder moisture absorption degree of agglomeration quantitatively characterizing method, including：Powder is placed in be balanced under 0% relative humidity by step (1) obtains absolute dried sample；The absolute dried sample that step (2) is obtained to step (1) carries out low stress compression experiment, forms grain bed；Grain bed is placed under 0% relative humidities by step (3), and grain bed surface initial hardness is determined using ball indentation method；Grain bed is placed under different relative humidities and places different time by step (4), the dynamic variation of grain bed case hardness is determined using ball indentation method, grain bed case hardness and humidity, the dependency relation of temperature and time are set up, determines whether the moisture absorption process of powder is reversible and occur the critical condition of irreversible moisture absorption.The condition selection and control that the present invention can be product in actual production and storage provide data supporting, and the present invention is also few with sample size, the advantage that detection speed is fast and sensitivity is high.
Description
Technical field
The present invention relates to a kind of powder moisture absorption degree of agglomeration quantitatively characterizing method.
Background technology
All it is in the form of powder granule with the presence of more than 70% in the market in all raw material and product form
's.In the different industries such as food, medicine, chemical industry, moisture absorption agglomeration problems of the powder in processing and storage are generally to deposit
The problem of, it can not only significantly reduce product quality, while causing huge economic loss.Powder moisture absorption is lumpd at present
Research method be mainly and determine its hydroscopicity under 75% relative humidity, but only can not be to powder formation by hydroscopicity
Degree of agglomeration size carries out rational judgment.How the degree of agglomeration of stored powder product is expected so that it is determined that its shelf-life is
Major issue urgently to be resolved hurrily in industry.Therefore, hair of the quantitative approach of exploitation powder moisture absorption degree of agglomeration for powder industry
Exhibition has important facilitation.
The content of the invention
For above-mentioned technical problem, the invention provides a kind of powder moisture absorption degree of agglomeration quantitatively characterizing method, it is used
Ball indentation method carries out dynamic detection to case hardness during the different holding conditions of powder granule bed, whether can determine whether powder moisture absorption
For reversible process and the critical condition of the irreversible moisture absorption of generation, correlated results can be product in actual production and storage
Condition selection and control provide data supporting, meanwhile, the present invention also have sample size it is few, detection speed is fast and sensitivity is high
Advantage.
The technical scheme that the present invention is provided is：
A kind of powder moisture absorption degree of agglomeration quantitatively characterizing method, including：
Powder is placed in be balanced under 0% relative humidity by step (1) obtains absolute dried sample；
The absolute dried sample that step (2) is obtained to step (1) carries out low stress compression experiment, forms grain bed；
The grain bed is placed under 0% relative humidities by step (3), at the beginning of determining grain bed surface using ball indentation method
Beginning hardness；
The grain bed is placed under different relative humidities and places different time by step (4), is surveyed using ball indentation method
Determine the dynamic variation of grain bed case hardness under different condition, set up grain bed case hardness and humidity, temperature and time
Dependency relation；And according to the dependency relation and grain bed surface initial hardness determine the moisture absorption process of powder it is whether reversible and
Occurs the critical condition of irreversible moisture absorption.
Preferably, it is described relative in the step (4) in described powder moisture absorption degree of agglomeration quantitatively characterizing method
Humidity range is 11%-90%, and the temperature range is 5-60 DEG C.
Preferably, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, in the step (4), balls
Diameter can be 1.6-10mm, and pressure used is 7mN-5N, and spherical indenter loading velocity is 0.5-2mm/min.
Preferably, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, in the step (3), balls
Diameter can be 1.6-10mm, and pressure used is 3-200mN, and spherical indenter loading velocity is 0.5-2mm/min.
Preferably, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, balls are glass marble.
Preferably, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, in the step (2), it is described it is low should
In force compresses experiment, pressure range used in the low stress compression experiment is 2-8kPa, and piston loading velocity scope is 0.5-
2mm/min。
Preferably, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the powder is food, chemical industry and medicine
Use powder.
Preferably, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the powder is that polyethylene ratio coughs up alkane
Ketone, hydroxypropyl cellulose and mannitol.
Powder moisture absorption degree of agglomeration quantitatively characterizing method of the present invention is different to powder granule bed using ball indentation method
Case hardness carries out dynamic detection during holding conditions, can determine whether whether powder moisture absorption is reversible process and occurs irreversible
The critical condition of moisture absorption, the condition selection and control that correlated results can be product in actual production and storage provides data
Support.The present invention uses ball indentation method, and sample single detection time is less than 2min, with convenient and swift and high stability spy
Point.This method simultaneously can to same grain bed carry out multiple spot dynamic detection, not only save sample size, it is thus also avoided that different samples it
Between caused by error, experimental result accuracy rate is higher.
Brief description of the drawings
Fig. 1 is in ball Indentation Process in the embodiment one of powder moisture absorption degree of agglomeration quantitatively characterizing method of the present invention
Pressure-loaded and unloading curve；
Fig. 2 is different relative humidity in the embodiment one of powder moisture absorption degree of agglomeration quantitatively characterizing method of the present invention
Under the conditions of PVP grain bed case hardnesses kinetic curve；
Fig. 3 is condition of different temperatures in the embodiment two of powder moisture absorption degree of agglomeration quantitatively characterizing method of the present invention
The kinetic curve of lower HPC grain bed case hardnesses；
Fig. 4 is different relative humidity in the embodiment three of powder moisture absorption degree of agglomeration quantitatively characterizing method of the present invention
Under the conditions of mannitol particles bed case hardness kinetic curve.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
The present invention provides a kind of powder moisture absorption degree of agglomeration quantitatively characterizing method, including：
Powder is placed in be balanced under 0% relative humidity by step (1) obtains absolute dried sample；
The absolute dried sample that step (2) is obtained to step (1) carries out low stress compression experiment, forms grain bed；
The grain bed is placed under 0% relative humidities by step (3), at the beginning of determining grain bed surface using ball indentation method
Beginning hardness；
The grain bed is placed under different relative humidities and places different time by step (4), is surveyed using ball indentation method
Determine the dynamic variation of grain bed case hardness under different condition, set up grain bed case hardness and humidity, temperature and time
Dependency relation；And according to the dependency relation and grain bed surface initial hardness determine the moisture absorption process of powder it is whether reversible and
Occurs the critical condition of irreversible moisture absorption.
The present invention carries out dynamic detection using ball indentation method to case hardness during the different holding conditions of powder granule bed,
It can determine whether whether powder moisture absorption is reversible process and occurs the critical condition of irreversible moisture absorption, and correlated results can be product in reality
Border is produced and condition selection and control in storage provide data supporting.The present invention uses ball indentation method, the inspection of sample single
The survey time is less than 2min, the characteristics of with convenient and swift and high stability.This method can carry out multiple spot to same grain bed simultaneously
Dynamic detection, not only saves sample size, it is thus also avoided that error caused by between different samples, experimental result accuracy rate is higher.
In a preferred embodiment, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the step (4)
In, the RH range is 11%-90%, and the temperature range is 5-60 DEG C.
In a preferred embodiment, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the step (4)
In, the diameter of balls can be 1.6-10mm, and pressure used is 7mN-5N, and spherical indenter loading velocity is 0.5-2mm/min.
In a preferred embodiment, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the step (3)
In, the diameter of balls can be 1.6-10mm, and pressure used is 3-200mN, and spherical indenter loading velocity is 0.5-2mm/min.
In a preferred embodiment, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, balls are glass
Glass ball.
In a preferred embodiment, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the step (2)
In, in the low stress compression test, pressure range used in the low stress compression experiment is 2-8kPa, piston loading velocity model
Enclose for 0.5-2mm/min.
In a preferred embodiment, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the powder is
Food, chemical industry and medicinal powder.The present invention is widely used, in the moisture absorption degree of agglomeration to food, chemical industry and medicinal powder
In quantitatively characterizing, accurate characterization result can be obtained.
In a preferred embodiment, in described powder moisture absorption degree of agglomeration quantitatively characterizing method, the powder is
PVP, hydroxypropyl cellulose and mannitol.
To further illustrate technical scheme, following examples are now provided.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., unless otherwise specified, are commercially obtained.
PVP (PVP-K30), hydroxypropyl cellulose (HPC) and mannitol used in following embodiments
(200SD) is bought in AstraZeneca companies of Britain.
Instron test equipments used in following embodiments are bought in Instron companies of Britain.
Lithium chloride used in following embodiments, sodium chloride and magnesium chloride, which buy your experiment equipment (Shanghai) in winged generation, to be had
Limit company, its saturated solution is used to produce 11%, 33% and 75% relative humidity respectively.
Silica gel used in following embodiments is bought in the Foshan City Jiade damp Science and Technology Ltd. of great coast defence.
Moisture absorption degree of agglomeration quantitatively characterizing under the PVP different humidity of embodiment one
(1) 10g PVPs (PVP) powder is weighed in rustless steel container (diameter 4cm), is then placed within
In the drier for filling silica gel, 4d is placed, powder bed quality no longer changes；
(2) using 5kPa pressure to step 1) in PVP powder beds be compressed, piston diameter used is 4cm, and piston adds
Load speed is 1mm/min；
(3) indentation test is carried out using spherical indenter, balls are glass marble, a diameter of 4mm of glass marble used；Using 3-
11mN power carries out ball indentation test, more specifically can be 7mN, the loading velocity of spherical indenter is 1mm/min, obtains grain bed
Initial hardness value under 0% relative humidity；
(4) PVP grain beds are placed into 8d under 25 DEG C, 11%, 33% and 75% relative humidity respectively, using ball indentation method pair
The hardness number of grain bed enters Mobile state measure.The loading velocity of spherical indenter is 1mm/min, and pressure used can be 7mN-5N；
(5) set up grain bed hardness and humidity (11%, 33% and 75%) and the time (0-8d) dependency relation, it is determined that
Whether PVP moisture absorption process is reversible and occurs the critical condition of irreversible moisture absorption.
Please see Figure 2, Fig. 2 is pressure-loaded and unloading curve in ball Indentation Process in the embodiment.The moisture absorption of grain bed surface
Degree of agglomeration is characterized using case hardness (H).Wherein, hardness calculation formula is as follows：
H=Fmax/π(Db×hc,max-h2 c,max),
Wherein, FmaxFor the maximum pressure used, DbFor the diameter of balls, hc,maxFor the discharge degree curve initial stage
Slope under corresponding compression depth.
Then final testing result is as shown in Figure 3.
As can be seen from Figure 3, (11%) does not make significant difference to PVP powder granules bed case hardness under low humidity, shows 11%
Powder granule bed stability is very high under humidity, will not occur moisture absorption caking；Under moderate amount of moisture (33%), although PVP grain beds
Hardness increased over time, but 3 times or so in the case where 5d hardness numbers reach equilibrium valve (3kPa), only 0% humidity,
PVP grain beds still have good mobility；Under high humility (75%), and with the extension of time, PVP grain beds occur sternly
Ascendant trend is presented in the caking phenomenon of weight, hardness number, and peak (2200kPa, under being 0% humidity is reached in the 7th day hardness
2500 times), afterwards with the further absorption of moisture, surface liquefaction, hardness number decreases.For PVP raw materials,
When hardness number is less than 100kPa (5d), powder moisture absorption caking to be reversible, the degree of agglomeration now formed it is relatively low, it is necessary to
Relatively low power can be returned to powder state again.But more than (after 6d), powder moisture absorption is irreversible procedure after 100kPa,
PVP grain beds color is changed into yellow from light yellow.As a result show ball indentation method and exist between relative humidity and time significant
Whether dependency relation, may determine that its moisture absorption degree of agglomeration by the change of grain bed case hardness and be reversible moisture absorption process.
Moisture absorption degree of agglomeration quantitatively characterizing under embodiment dihydroxypropyl cellulose different temperatures
(1) 15g hydroxypropyl celluloses (HPC) powder is weighed in rustless steel container (diameter 4cm), is then placed within and is filled
In the drier of silica gel, 4d is placed, powder bed quality no longer changes；
(2) using 7.5kPa pressure to step 1) in HPC powder beds be compressed, piston diameter used be 4cm, piston
Loading velocity is 1mm/min；
(3) indentation test is carried out using spherical indenter, balls are glass marble, a diameter of 4mm of glass marble used；Using
10-200mN power carries out ball indentation test, more specifically can be 150mN, the loading velocity of spherical indenter is 1mm/min, is obtained
Initial hardness value of the grain bed under 0% humidity；
(4) HPC grain beds are placed into 8d under 25 DEG C and 45 DEG C, 75% relative humidity respectively, using ball indentation method to particle
The hardness number of bed enters Mobile state measure；The loading velocity of spherical indenter is 1mm/min, and pressure used can be 150mN；
(5) grain bed hardness and temperature (25 DEG C and 45 DEG C) and the dependency relation of time (0-8d) are set up, PVP moisture absorptions are determined
Whether process is reversible and occurs the critical condition of irreversible moisture absorption.
Hardness detection method be the same as Example one.
Then final detection result is as shown in Figure 3.
From the figure 3, it may be seen that placing 7-8d under 25 DEG C, 75% relative humidity, product hardness value is relatively stablized
(36kPa), but now there is the phenomenon of volume contraction in sample particle bed, and its moisture absorption agglomeration process is irreversible；Placing 3d
When, grain bed starts the sign (25kPa) for occurring separating with container.The caking speed of HPC grain beds can substantially be accelerated at 45 DEG C
Spend, 45 DEG C, the hardness number that 1d is placed under 75% relative humidity is higher than the hardness number of the 8d under 25 DEG C, 75% relative humidity, and
Particle bed volume starts reduction.At 25 DEG C, 75% relative humidity places 3d, 45 DEG C, is placed under 75% relative humidity after 1d, HPC
Product has lost commodity value.Therefore, for HPC products, its superficial hardness number has preferably steady when being less than 25kPa
It is qualitative.
Moisture absorption degree of agglomeration quantitatively characterizing under the mannitol different humidity of embodiment three
(1) 20g mannitol powder is weighed in rustless steel container (diameter 4cm), is then placed within the drying for filling silica gel
In device, 2d is placed, powder bed quality no longer changes；
(2) using 7.5kPa pressure to step 1) in mannitol powder bed be compressed, piston diameter used be 4cm,
Piston loading velocity is 1mm/min；
(3) indentation test is carried out using spherical indenter, balls are glass marble, a diameter of 4mm of glass marble used；Using 3-
20mN power carries out ball indentation test, more specifically can be 9mN, the loading velocity of spherical indenter is 1mm/min, obtains grain bed
Initial hardness value under 0% humidity；
(4) mannitol particles bed is placed into 8d under 25 DEG C, 11%, 33% and 75% relative humidity respectively, using ball impression
Method enters Mobile state measure to the hardness number of grain bed；The loading velocity of spherical indenter is 1mm/min, and pressure used can be 9-
100mN；
(5) set up grain bed hardness and humidity (11%, 33% and 75%) and the time (0-8d) dependency relation, determine sweet
Whether dew alcohol moisture absorption process is reversible and occurs the critical condition of irreversible moisture absorption.
Hardness detection method be the same as Example one.
Then final detection result is as shown in Figure 4.
As shown in Figure 4,11% and 33% relative humidity has no significant effect to mannitol powder firmness change；And 75%
Under relative humidity, the hardness of mannitol particles bed is with the extension of open-assembly time, the rise of its hardness number, but reaches at second day flat
Weigh (6kPa).But its hardness value changes is much smaller with respect to for PVP and HPC.This be due to mannitol moisture absorption caking be
Reversible, the caking that it is formed is more fragile, can be destroyed with relatively small mechanical force.
The result of three above embodiment shows, ball indentation may determine that different material, different humidity and at a temperature of
Over time under change condition, its formed caking whether it is reversible and it is irreversible caking occur hardness critical value.To sum up institute
State, method of the present invention is a kind of quick, reliable a kind of accurately method of quantitatively characterizing powder moisture absorption degree of agglomeration.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the legend with description.
Claims (8)
1. a kind of powder moisture absorption degree of agglomeration quantitatively characterizing method, it is characterised in that including：
Powder is placed in be balanced under 0% relative humidity by step (1) obtains absolute dried sample；
The absolute dried sample that step (2) is obtained to step (1) carries out low stress compression experiment, forms grain bed；
The grain bed is placed under 0% relative humidities by step (3), and it is initially hard to determine grain bed surface using ball indentation method
Degree；
The grain bed is placed under different relative humidities and places different time by step (4), is determined not using ball indentation method
The dynamic variation of grain bed case hardness with the conditions of, set up grain bed case hardness and humidity, temperature and time it is related
Relation；And determine whether the moisture absorption process of powder is reversible and occurs according to the dependency relation and grain bed surface initial hardness
The critical condition of irreversible moisture absorption.
2. powder moisture absorption degree of agglomeration quantitatively characterizing method as claimed in claim 1, it is characterised in that in the step (4),
The RH range is 11%-90%, and the temperature range is 5-60 DEG C.
3. powder moisture absorption degree of agglomeration quantitatively characterizing method as claimed in claim 1, it is characterised in that in the step (4),
The diameter of balls can be 1.6-10mm, and pressure used is 7mN-5N, and spherical indenter loading velocity is 0.5-2mm/min.
4. powder moisture absorption degree of agglomeration quantitatively characterizing method as claimed in claim 3, it is characterised in that in the step (3),
The diameter of balls can be 1.6-10mm, and pressure used is 3-200mN, and spherical indenter loading velocity is 0.5-2mm/min.
5. powder moisture absorption degree of agglomeration quantitatively characterizing method as claimed in claim 4, it is characterised in that balls are glass
Ball.
6. powder moisture absorption degree of agglomeration quantitatively characterizing method as claimed in claim 1, it is characterised in that in the step (2),
In the low stress compression test, pressure range used in the low stress compression experiment is 2-8kPa, piston loading velocity scope
For 0.5-2mm/min.
7. the powder moisture absorption degree of agglomeration quantitatively characterizing method as any one of claim 1 to 6, it is characterised in that institute
Powder is stated for food, chemical industry and medicinal powder.
8. powder moisture absorption degree of agglomeration quantitatively characterizing method as claimed in claim 7, it is characterised in that the powder is poly- second
Alkene is than pyrrolidone, hydroxypropyl cellulose and mannitol.
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| CN108303346A (en) * | 2017-12-28 | 2018-07-20 | 中国农业科学院农产品加工研究所 | Powder fluidity quantitatively characterizing method |
| WO2024082719A1 (en) * | 2022-10-20 | 2024-04-25 | 天津大学 | Method for predicting critical caking period of crystal particle |
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| WO2024082719A1 (en) * | 2022-10-20 | 2024-04-25 | 天津大学 | Method for predicting critical caking period of crystal particle |
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| Publication number | Publication date |
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| CN107063906B (en) | 2020-01-07 |
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