CN109752292A - A kind of test method of the particle size and its distribution of three aluminum hydrides - Google Patents
A kind of test method of the particle size and its distribution of three aluminum hydrides Download PDFInfo
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- CN109752292A CN109752292A CN201811604992.3A CN201811604992A CN109752292A CN 109752292 A CN109752292 A CN 109752292A CN 201811604992 A CN201811604992 A CN 201811604992A CN 109752292 A CN109752292 A CN 109752292A
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Abstract
A kind of test method of the particle size and its distribution of three aluminum hydrides, this method application wet process laser diffractometry test AlH3Particle size and its distribution.Decentralized medium is added in three aluminum hydrides in this method (1)；The decentralized medium is lecithin-butyl acetate solution of mass fraction (1~3) % or nonylphenol polyoxyethylene ether-butyl acetate solution of (1~3) %；(2) combination ingredient in step (1) is dispersed, preparation has fully decentralized AlH3Suspension system；(3) particle size and its distribution of three aluminum hydrides in step (2) processing rear suspension liquid is measured using wet process laser particle analyzer.The relative standard deviation of partial size multiple measurement results of the present invention is not more than 5%, and the precision of method is preferable.
Description
Technical field
The present invention relates to a kind of test methods of the particle size and its distribution of three aluminum hydrides.
Background technique
AlH3It is a kind of new selective reducing agent, can be used as the hydrogen source and polymerization catalyst of hydrogen storage material, fuel cell
Deng.Due to AlH3With heats of combustion and specific impulse, and by the high-energy propellant fuel novel as one kind in solid propellant
Research extensively, for improving the combustibility and energy characteristics of solid propellant.AlH3Granularity and size distribution, used with it
Performance is closely related, is the important indicator of its product quality monitoring.AlH3As a kind of novel energetic material, not ready-made grain
It is available to spend test method.Currently, most widely used testing graininess method is laser diffractometry, which is divided into wet process and dry method again
Two kinds.Wet process can be used for insensitiveness or energetic material test, but need to fish for suitable decentralized medium, dispersion and dispersion
Mode.Dry method is simpler compared with wet process test, and testing efficiency is higher, but there are security risks for test energetic material.Therefore wet process is surveyed
Examination is more often used.
Summary of the invention
The invention aims to provide one kind three aluminum hydride (AlH3) particle size and its distribution test method, thus
For AlH3Testing graininess in production, use process, provides technological means for its control of product quality.The characteristics of this method is
Continuous mode is simple and convenient, and experimental result is intuitively efficient, has saved the testing time.
The technical scheme is that suitable decentralized medium and dispersion are selected, by AlH3Sample powder is surpassed
Sound dispersion, controls the suitable time, testing graininess is carried out using wet process laser particle analyzer, to obtain AlH3Granularity and
Size distribution.It includes the following steps:
(1) decentralized medium is added in three aluminum hydrides；The decentralized medium is the lecithin-of mass fraction (1~3) %
The nonylphenol polyoxyethylene ether of butyl acetate solution or (1~3) %-butyl acetate solution；
(2) combination ingredient in step (1) is dispersed, preparation has fully decentralized AlH3Suspension system；
(3) granularity and granularity point of three aluminum hydrides in step (2) processing rear suspension liquid are measured using wet process laser particle analyzer
Cloth.
Preferably, it is lecithin-butyl acetate that mass fraction is 2.5% that decentralized medium in the step (1) is optimal
Or 2.5% nonylphenol polyoxyethylene ether-butyl acetate solution, dispersion solvent are butyl acetate.
Preferably, the dispersing mode in the step (2) is 5~10min of ultrasonic disperse.
Preferably, the supersonic frequency 50Hz~80Hz.
Preferably, it is ultrasound 50Hz that the dispersing mode is optimal, disperses 5min.
Preferably, until wet process laser particle analyzer is surveyed under the conditions of index of refraction is 5%~10% in the step (3)
Examination.
Preferably, granularity uses median d in the step (3)50(μm) and volume average particle size d4,3(μm) indicates,
Size distribution is indicated with particle size distribution figure.
Preferably, three aluminum hydrides and decentralized medium ratio are that tri- aluminum hydride of 1g~3g is added in 30mL~50mL decentralized medium
Preferably, three aluminum hydrides and decentralized medium best proportion are that tri- aluminum hydride of 1g is added in 30mL decentralized medium.
The beneficial effects of the present invention are:
(1) present invention selectes 2.5% lecithin-acetic acid by screening different dispersions and different ultrasonic times
Butyl ester or 2.5% wetting agent P-40 (nonylphenol polyoxyethylene ether)-butyl acetate solution are as dispersion, ultrasonic time 5
~10min carries out ultrasonic disperse as AlH3Testing graininess condition；Having had for suitable particle distribution test can be prepared
The AlH dispersed entirely3Suspension system.
(2) present invention can directly measure AlH by wet process laser diffractometry3Particle size and its distribution, can be used for AlH3It is raw
Particle size and its distribution test during production, to provide essential technological means for its control of product quality.
(3) relative standard deviation of multiple measurement results of the present invention is not more than 5%, and the precision of method is preferable.
Detailed description of the invention
Fig. 1 is AlH3 particle size distribution figure in the embodiment of the present invention 1；
Fig. 2 is AlH3 particle size distribution figure in the embodiment of the present invention 2；
Fig. 3 is AlH3 particle size distribution figure in the embodiment of the present invention 3.
Specific embodiment
The content of present invention is further described combined with specific embodiments below:
Embodiment 1
The AlH of certain lot number3The test of sample, particle size and its distribution is as follows: opening wet process laser particle analyzer, preheating half
Hour, the included testing graininess software of operation wet process laser particle analyzer uses Butylacetate instrument pipeline.In software window
Middle conditioning instrumentation centering, test equipment background.Weigh the AlH of 1.0g or so3Sample is placed in 100mL beaker, and it is left that 30mL is added
Right 2.5% lecithin-butyl acetate solution, ultrasonic (50Hz or so) disperse 5min, after the completion of instrumental background test, by sample
Product solution is added in sample cell, and the index of refraction of setting wet process laser particle analyzer is 5%~10% or so, is arranged in software and is respectively surveyed
Parameter is tried, sample is tested, computer provides test result automatically after the completion of test.Testing graininess result is with median
d50(μm) and volume average particle size d4,3(μm) indicates.Particle size distribution figure as shown in Figure 1, particle size and its distribution test result such as
Shown in table 1.
Embodiment 2
The AlH of certain lot number3The test of sample, particle size and its distribution is as follows: opening wet process laser particle analyzer, preheating half
Hour.Testing graininess software is run, Butylacetate instrument pipeline is used.In software window in conditioning instrumentation pair, test
Instrumental background.Weigh the AlH of 1.0g or so3Sample is placed in 100mL beaker, and the 2.5% wetting agent P-40 of 30mL or so is added
(nonylphenol polyoxyethylene ether)-butyl acetate solution, ultrasonic disperse 5min, after the completion of instrumental background test, by sample solution
It is added in sample cell, until index of refraction is 5%~10% or so, each test parameter in software is set, sample is tested,
Computer provides test result automatically after the completion of test.Testing graininess result is with median d50(μm) and volume average particle size
d4,3(μm) indicates.Particle size distribution figure is as shown in Fig. 2, particle size and its distribution test result is as shown in table 1.
Embodiment 3
The AlH of certain lot number3The test of sample, particle size and its distribution is as follows: opening wet process laser particle analyzer, preheating half
Hour.Testing graininess software is run, Butylacetate instrument pipeline is used.In software window in conditioning instrumentation pair, test
Instrumental background.Weigh the AlH of 1.0g or so3Sample is placed in 100mL beaker, and the 2.5% lecithin-acetic acid of 30mL or so is added
Butyl acetate solution, sample solution is added in sample cell by ultrasonic disperse 10min after the completion of instrumental background test, until refractive power
Rate is 5%~10% or so, and each test parameter in software is arranged, tests sample, computer is given automatically after the completion of test
Test result out.Testing graininess result is with median d50(μm) and volume average particle size d4,3(μm) indicates.Particle size distribution figure is such as
Shown in Fig. 3, particle size and its distribution test result is as shown in table 1.
1 AlH of table3Sample granularity test result
The above, optimal specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
The content that description in the present invention is not described in detail belongs to the well-known technique of professional and technical personnel in the field.
Claims (9)
1. a kind of test method of the particle size and its distribution of three aluminum hydrides, it is characterised in that the following steps are included:
(1) decentralized medium is added in three aluminum hydrides；The decentralized medium is lecithin-acetic acid of mass fraction (1~3) %
The nonylphenol polyoxyethylene ether of butyl acetate solution or (1~3) %-butyl acetate solution；
(2) combination ingredient in step (1) is dispersed, preparation has fully decentralized AlH3Suspension system；
(3) particle size and its distribution of three aluminum hydrides in step (2) processing rear suspension liquid is measured using wet process laser particle analyzer.
2. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 1, it is characterised in that: institute
It is lecithin-butyl acetate or 2.5% polyoxyethylene nonyl phenyl that mass fraction is 2.5% that it is optimal, which to state the decentralized medium in step (1),
Vinethene-butyl acetate solution, dispersion solvent are butyl acetate.
3. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 1, it is characterised in that: institute
Stating the dispersing mode in step (2) is 5~10min of ultrasonic disperse.
4. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 3, it is characterised in that: institute
Supersonic frequency 50Hz~the 80Hz stated.
5. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 4, it is characterised in that: institute
The optimal dispersing mode stated is ultrasound 50Hz, disperses 5min.
6. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 1, it is characterised in that: institute
It states in step (3) until wet process laser particle analyzer is tested under the conditions of index of refraction is 5%~10%.
7. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 1, it is characterised in that: institute
It states granularity in step (3) and uses median d50(μm) and volume average particle size d4,3(μm) indicates, size distribution size distribution
Figure indicates.
8. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 1, it is characterised in that: three
Aluminum hydride and decentralized medium ratio are that tri- aluminum hydride of 1g~3g is added in 30mL~50mL decentralized medium.
9. a kind of test method of the particle size and its distribution of three aluminum hydride according to claim 8, it is characterised in that: three
Aluminum hydride and decentralized medium best proportion are that tri- aluminum hydride of 1g is added in 30mL decentralized medium.
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Cited By (4)
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| CN110411920A (en) * | 2019-08-22 | 2019-11-05 | 攀钢集团攀枝花钢铁研究院有限公司 | The detection method of titanium white first product granularity |
| CN111982763A (en) * | 2020-08-17 | 2020-11-24 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
| CN112763383A (en) * | 2019-11-04 | 2021-05-07 | 乐凯华光印刷科技有限公司 | Method for measuring particle size and distribution of thermoplastic nano-micro particles by using photon-correlated nano-particle size analyzer |
| CN113125317A (en) * | 2021-04-14 | 2021-07-16 | 江苏联环药业股份有限公司 | Method for testing particle size and particle size distribution of epristeride bulk drug |
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| CN112763383B (en) * | 2019-11-04 | 2024-04-26 | 乐凯华光印刷科技有限公司 | Method for measuring particle size and distribution of thermoplastic nano-micron particles by using photon correlation nano-particle sizer |
| CN111982763A (en) * | 2020-08-17 | 2020-11-24 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
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| CN113125317A (en) * | 2021-04-14 | 2021-07-16 | 江苏联环药业股份有限公司 | Method for testing particle size and particle size distribution of epristeride bulk drug |
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