CN108896711A - A kind of test device and measuring method of liquid accelerator stability - Google Patents

A kind of test device and measuring method of liquid accelerator stability Download PDF

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Publication number
CN108896711A
CN108896711A CN201810648952.2A CN201810648952A CN108896711A CN 108896711 A CN108896711 A CN 108896711A CN 201810648952 A CN201810648952 A CN 201810648952A CN 108896711 A CN108896711 A CN 108896711A
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oil bath
liquid accelerator
low
test device
liquid
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CN108896711B (en
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董耀武
陈健
代柱端
周晓阳
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Wuhan Excellent Technology Co Ltd
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Abstract

The present invention discloses the test device and measuring method of a kind of liquid accelerator stability, test device of the invention is by low-temperature oil bath cabinet, ultrasonic disperse instrument, DC power supply, electrophoresis glass tube column and centrifugal chiller at the electrophoresis glass tube column is placed in the oil bath pan of the low-temperature oil bath cabinet;The DC power supply is electrically connected with electrophoresis glass tube column both ends;The concussion end of the ultrasonic disperse instrument is placed in the oil bath pan of the low-temperature oil bath cabinet.Test device of the invention reduces solute solubility in testing liquid accelerator by low-temperature oil bath cabinet, promote to generate nucleus by ultrasonic disperse instrument and electrophoresis, and the processes such as separation of solid and liquid are made by centrifugation, make the quick unstability crystallization of liquid accelerator, so as to measure the long-time stability of liquid accelerator in a relatively short period of time.Test device of the present invention is simple to operate, and measuring method has many advantages, such as good, repeatable high with correspondence of the current standard to liquid accelerator stability test result.

Description

A kind of test device and measuring method of liquid accelerator stability
Technical field
The invention belongs to inorganic material detection device technical fields, and in particular to a kind of test of liquid accelerator stability Device and measuring method.
Background technique
Liquid accelerator is a kind of cement additive, it can shorten the setting time of concrete slurry, improves concrete The early strength of component.Existing liquid accelerator mainly includes two classes:Alkaline liquid accelerating agent (alkali content >=1.0%) and nothing Alkali liquid quick-setting agent (alkali content < 1.0%), analysis market product discovery, these two types of liquid accelerators are morphologically roughly divided into Following three classes:(1) supernatant liquid;(2) suspension of homogeneous slightly viscosity;(3) suspension etc. with cotton-shaped layering.Above-mentioned three kinds The product of form classification often will appear layering, crystallization, precipitating, even coagulate in the harsh conditions storage such as long-time or low temperature The phenomenon that adhesive curing etc. deteriorates product quality can bring interference very serious in chemical process or product practical application. However, in the current standard of accelerator《JC 477-2005 gunite concrete accelerator》In, to the steady of liquid accelerator product It is qualitative even without being distinctly claimed.
At present sample is placed in by the measurement of liquid accelerator sample stability frequently with the method directly observed 28d is stood in 100mL tool plug graduated cylinder, whether bottom crystal or precipitating is observed more than 5mL, can be considered stable if being less than 5mL i.e. Property is met the requirements, but this method last it is longer and unpredictable to later period accelerated deterioration.Based on this, some scholars propose speed Several rapid assay methods of solidifying agent stability, as CN201510329697.1 is authorized《A kind of measurement liquid accelerator is stable The method of property》It is disclosed with CN201510329667.0《A kind of measuring method of supernatant liquid accelerator stability》, both Method is required to for sample to be tested to be configured to the solution of a certain concentration range, such method can change in raw sample in measurement Ion concentration, destroy raw sample complexation equilibrium that may be present or hydrolysising balance;The measurement of such method later period is using low simultaneously Temperature, high temperature circulation are reciprocal, do so the quality that can also change solvent in cyclic process, therefore cycle-index is to measurement result Repeatability impacts.
Summary of the invention
In response to the problems existing in the prior art, the purpose of the present invention is to provide a kind of test of liquid accelerator stability dresses It sets and measuring method, test method of the present invention is quick and convenient, result is accurate, reproducibility is high.
To achieve the above object, the technical solution adopted by the present invention is that:
It is a kind of measure liquid accelerator stability test device, by low-temperature oil bath cabinet, ultrasonic disperse instrument, DC power supply, Electrophoresis glass tube column and centrifugal chiller are at the electrophoresis glass tube column is placed in the oil bath pan of the low-temperature oil bath cabinet;It is described straight Galvanic electricity source is electrically connected with electrophoresis glass tube column both ends;The concussion end of the ultrasonic disperse instrument is placed in the low-temperature oil bath cabinet Oil bath pan in.
Accelerator stand during, due to the factors such as the aggregation of charge, lolute crystallization, temperature change influence solute gradually Be precipitated, by observation crystallization content number judge the stability of accelerator;Using test device of the invention, it is suitable for difference The liquid accelerator sample stability of character is tested, and such as clarifies shape, suspended liquid, cotton-shaped layering shape, liquid accelerator without It crosses processing and is directly loadable into electrophoresis glass tube column, raw sample complexation equilibrium that may be present or hydrolysising balance, sample knot will not be destroyed Brilliant process more gets close to nature standing method, is conducive to the accuracy and reproducibility that improve test result;Pass through low-temperature oil bath cabinet Realize temperature control, low temperature can reduce the solubility of solute, reduce the solubility of solute in testing liquid accelerator quickly, Shorten test period, while not will lead to solvent in liquid accelerator and volatilizing;By ultrasonic disperse instrument ultrasonic oscillation, make solute Ion obtains acceleration in a short time, obtains it and crystallizes required energy, increases the probability of its collision crystallization, to accelerate to tie Brilliant rate;Electrophoretic action can make to generate certain potential difference in liquid between ion, and solute ions collide shape under potential difference effect Probability at crystallization nucleus increases, and is precipitated to be enriched with crystallization;Liquid accelerator unstability is crystallized by centrifuge, realizes solid-liquid Quick separating, so as to measure the long-time stability of liquid accelerator in a relatively short period of time;Test device through the invention, Simulation accelerates accelerator and stands unstable reason naturally, substantially reduces the accelerator Stability Determination time, improves effect Rate, and experimentation is controllable, improves the reproducibility of measurement result.
The present invention also provides a kind of measuring methods of the test device of liquid accelerator stability, and specific steps are such as Under:
(1) the liquid accelerator sample of certain mass is taken to be directly loadable into electrophoresis glass tube column;
(2) the electrophoresis glass tube column equipped with liquid accelerator sample is placed in the oil bath pan of low-temperature oil bath cabinet, both ends are used DC power supply on-load voltage is arranged oil bath temperature -10~0 DEG C, the concussion end of ultrasonic disperse instrument is placed in low-temperature oil bath cabinet In oil bath pan, ultrasonic disperse instrument oscillation frequency is set, after keeping 8~12h, takes out the electrophoresis glass that liquid accelerator sample is housed Tubing string;
(3) the liquid accelerator sample m that the step of weighing certain mass (2) is taken out1, it is fitted into centrifuge rotor and is put into Low-speed centrifugal in centrifuge weighs supernatant liquor quality m2
(4) crystal accounting V=(m is calculated1-m2)/m1
Wherein, the low-temperature oil bath cabinet temperature range is adjustable, and precision is 0.1 DEG C.Liquid accelerator is typically all solute Near saturated solution or supersaturated solution, such as many alkali-free liquid accelerators are the supersaturated solutions of aluminum sulfate on the market, are used Low-temperature oil bath cabinet is within the scope of -10~0 DEG C, and solvent is not volatile in this temperature range in liquid accelerator, therefore will not change Become the amount of solvent, while reducing liquid accelerator sample temperature can be such that aluminum sulfate solubility in sample significantly reduces, and destroy in this way Sample original crystallization dissolution equilibrium keeps balance mobile to crystallization direction.
Preferably, it is the glass tube column with conductive contact, convenient and DC power supply that the electrophoresis glass tube column, which is both ends, Electrical connection avoids the occurrence of short circuit, improves test device stability.
Preferably, ultrasonic disperse instrument oscillation frequency described in step (2) is adjustable in 19.5~20.5kHz range, precision For 0.1kHz.Ultrasonic wave plays remarkable effect to the control of crystallization process, and ultrasonic wave can effectively substitute crystalline seed, promotes molten Matter nucleation, while using the crystal nucleation of ultrasonic wave promotion liquid accelerator, the crystal habit of formation is smaller and is uniformly dispersed.
Preferably, DC power supply described in step (2) is that exportable DC voltage is adjustable in 0~60V range, and precision is 0.1V.Suitable DC voltage can be applied as needed at the both ends of sample by DC power supply, make to produce between ion in liquid Raw certain potential difference increases collision between solute ions and forms crystallization to make solute ions be enriched within the scope of certain distance The probability of nucleus.
Preferably, centrifuge described in step (3) is centrifuged 5~10min with 2000~4000r/min revolving speed.By low temperature After oil bath, electrophoretic action and ultrasound promote the processing of nucleus growth, it can be generated in liquid accelerator sample evenly dispersed small Crystal grain can not visually determine its yield, will can be quickly separated by solid-liquid separation using 2000~4000r/min low-speed centrifugal, in this way can be with Determine crystal yields.
Compared with prior art, the beneficial effects of the invention are as follows:
(1) it does not need to be diluted liquid accelerator sample or concentration, it is directly tested surely by apparatus It is qualitative;
(2) it is suitable for the liquid accelerator sample of various trait, it is applied widely;
(3) test period is short, and method correspondence is good with standing, and measurement result is accurate, repeatability is high.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the test device of liquid accelerator stability of the present invention;
In figure:1, low-temperature oil bath cabinet;2, electrophoresis glass tube column;3, DC power supply;4, ultrasonic disperse instrument;5, centrifugal basket Son;6, centrifuge.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.Based on the embodiments of the present invention, those of ordinary skill in the art are without making creative work Every other embodiment obtained, shall fall within the protection scope of the present invention.Reagent that unless stated otherwise, the present invention uses, Method and apparatus is the art conventional reagent, method and apparatus.
As shown in Figure 1, the present invention provides a kind of test device of liquid accelerator stability, by low-temperature oil bath cabinet 1, ultrasound Separating apparatus 4, DC power supply 3, electrophoresis glass tube column 2 and centrifuge 6 form, and the electrophoresis glass tube column 2 is placed in the low-temperature oil In the oil bath pan of bath cabinet 1;The DC power supply 3 is electrically connected with 2 both ends of electrophoresis glass tube column;The ultrasonic disperse instrument 4 Concussion end is placed in the oil bath pan of the low-temperature oil bath cabinet 1.
The low-temperature oil bath cabinet 1 is that temperature is adjustable in -10~0 DEG C of range, and precision is 0.1 DEG C.
The ultrasonic disperse instrument 4 is that frequency is adjustable in 19.5~20.5kHz range, precision 0.1kHz.
The DC power supply 3 is that exportable DC voltage is adjustable in 0~60V range, precision 0.1V.
The electrophoresis glass tube column 2 is the glass tube column that both ends have conductive contact.
The centrifuge 6 is adjustable for 2000~4000r/min of revolving speed range, and timing 0~99min range is adjustable, institute Stating 5 capacity of centrifuge rotor is 15mL.
Following embodiment is all made of above-mentioned apparatus and is detected and analyzed to liquid accelerator stability.
Embodiment 1
The present embodiment provides a kind of measuring method of liquid accelerator stability, determination step is as follows:
(1) the liquid accelerator A for choosing a kind of faint yellow clear of certain mass, is loaded into electrophoresis glass tube column In 2;
(2) the electrophoresis glass tube column 2 equipped with sample A is placed in the oil bath for the low-temperature oil bath cabinet 1 that temperature setting is -10 DEG C In pot, both ends load the DC voltage for applying 20V by conductive contact with DC power supply 3, by the concussion end of ultrasonic disperse instrument 4 It is placed in the oil bath pan of low-temperature oil bath cabinet 1, the oscillation frequency of setting ultrasonic disperse instrument 4 is 20kHz, keeps 8h;
(3) the sample quality m after the step of extraction certain mass (2) is disposed1, it is fitted into centrifuge rotor 5 and puts Enter in centrifuge 6 and 10min is centrifuged with 3000r/min revolving speed, weighs supernatant liquor quality m2
(4) crystal accounting V (%)=(m is calculated1-m2)/m1
Test result is as shown in table 1, and table 1 gives what the sample was measured using standing method (under 5 DEG C of environment) simultaneously The data of 28d and 60d bottom crystal object product.
Embodiment 2
The present embodiment provides a kind of measuring methods of liquid accelerator stability, and compared with Example 1, difference exists In 1 oil bath temperature of low-temperature oil bath cabinet is set as 0 DEG C in step (2), and both ends, which are loaded by conductive contact with DC power supply 3, to be applied The concussion end of ultrasonic disperse instrument 4 is placed in the oil bath pan of low-temperature oil bath cabinet 1 by the DC voltage of 60V, and ultrasonic disperse instrument is arranged 4 oscillation frequency is 19.5kHz, keeps 12h.
Test result is as shown in table 1, and table 1 gives what the sample was measured using standing method (under 5 DEG C of environment) simultaneously The data of 28d and 60d bottom crystal object product.
Embodiment 3
The present embodiment provides a kind of measuring methods of liquid accelerator stability, and compared with Example 1, difference exists In in step (3), centrifuge 6 is centrifuged 5min with 2000r/min revolving speed.
Test result is as shown in table 1, and table 1 gives what the sample was measured using standing method (under 5 DEG C of environment) simultaneously The data of 28d and 60d bottom crystal object product.
Embodiment 4
The present embodiment provides a kind of measuring methods of slightly sticky milky white liquid accelerator B stability, with 1 phase of embodiment Than, the difference is that, 1 oil bath temperature of low-temperature oil bath cabinet is set as 0 DEG C in step (2), keeps low temperature oil bath time 8h;Step (3) 6 revolving speed 4000r/min of centrifuge, centrifugation time 8min.
Test result is as shown in table 1, and table 1 gives the 28d that the sample uses standing method (under 5 DEG C of environment) to measure simultaneously With the data of 60d bottom crystal object product.
Embodiment 5
The present embodiment provides a kind of measuring methods of the stability of liquid accelerator C for having a little cotton-shaped layering, with implementation Example 1 is compared, the difference is that, 1 oil bath temperature of low-temperature oil bath cabinet is set as -5 DEG C in step (2), and the oil bath time is 12h;Step Suddenly 6 revolving speed 3500r/min of (3) centrifuge, centrifugation time 9min.
Test result is as shown in table 1, and table 1 gives the 28d that the sample uses standing method (under 5 DEG C of environment) to measure simultaneously With the data of 60d bottom crystal object product.
Comparative example 1
The present embodiment provides a kind of measuring methods of liquid accelerator stability, and compared with Example 4, difference exists In, in step (2) by ultrasonic disperse instrument 4 carry out ultrasonic oscillation processing.
Test result is as shown in table 1, and table 1 gives the 28d that the sample uses standing method (under 5 DEG C of environment) to measure simultaneously With the data of 60d bottom crystal object product.
Comparative example 2
The present embodiment provides a kind of measuring methods of liquid accelerator stability, and compared with Example 4, difference exists In, in step (2) by DC power supply 3 load apply DC voltage.
Test result is as shown in table 1, and table 1 gives the 28d that the sample uses standing method (under 5 DEG C of environment) to measure simultaneously With the data of 60d bottom crystal object product.
Comparative example 3
The present embodiment provides a kind of measuring methods of liquid accelerator stability, and compared with Example 4, difference exists In the speed of 6 revolving speed 1000r/min of centrifuge is centrifuged 10min in step (3).
Test result is as shown in table 1, and table 1 gives the 28d that the sample uses standing method (under 5 DEG C of environment) to measure simultaneously With the data of 60d bottom crystal object product.
Comparative example 4
The present embodiment provides a kind of measuring methods of liquid accelerator stability, and compared with Example 4, difference exists In 1 oil bath temperature of low-temperature oil bath cabinet is set as 35 DEG C in step (2), and the oil bath time is 8h.
Test result is as shown in table 1, and table 1 gives the 28d that the sample uses standing method (under 5 DEG C of environment) to measure simultaneously With the data of 60d bottom crystal object product.
Each embodiment measurement result of table 1
As can be seen from Table 1, the liquid accelerator of the same clear of the embodiment of the present invention 1~3 passes through low temperature Oil bath case reduces solute solubility in testing liquid accelerator, promotes to generate nucleus by ultrasonic disperse instrument and electrophoresis, and pass through Centrifugation makes after being separated by solid-liquid separation with long-time using method validation comparison is stood, and the liquid accelerator clarification of centrifugation front and back is substantially without change Change, can be stored by long-time stable, and the result that measuring method measurement result and quiescent processes are observed through the invention It is almost the same, and embodiment 1 is best, illustrates measuring method and current standard of the present invention to liquid accelerator stability test result Correspondence is good, repeatable height, and measuring method of the present invention is simple and quick;
A kind of slightly sticky milky white liquid accelerator of embodiment 4 reduces testing liquid accelerator by low-temperature oil bath cabinet Middle solute solubility promotes to generate nucleus by ultrasonic disperse instrument and electrophoresis, and is made after being separated by solid-liquid separation by centrifugation and for a long time Using method validation comparison is stood, there are a large amount of precipitates after centrifugation, illustrate the slightly sticky milky white liquid accelerator stability It is poor, and the result that measuring method measurement result and static 60d are observed through the invention is almost the same, illustrates measurement of the present invention Method and current standard is good to the correspondence of liquid accelerator stability test result, repeatable height, and present invention measurement side Method is simple and quick;
A kind of liquid accelerator for having a little cotton-shaped layering of embodiment 5, reduces testing liquid rapid hardening by low-temperature oil bath cabinet Solute solubility in agent promotes to generate nucleus by ultrasonic disperse instrument and electrophoresis, and by centrifugation make after being separated by solid-liquid separation with it is long when Between using method validation comparison is stood, have a small amount of precipitate after centrifugation, illustrate that the slightly sticky milky white liquid accelerator is stablized Property is poor, and the result that measuring method measurement result and static 60d are observed through the invention is almost the same, illustrates survey of the present invention Determine that method and current standard is good to the correspondence of liquid accelerator stability test result, repeatable height, and the present invention measures Method is simple and quick;
1 liquid accelerator of comparative example does not pass through ultrasonic disperse instrument and carries out ultrasonic oscillation processing, makes solid-liquid point by centrifugation From rear and long-time using method validation comparison is stood, the crystal of formation is less, the knot that measurement result is observed with static 60d Fruit differs greatly, and shows to carry out ultrasonic oscillation by ultrasonic disperse instrument, may advantageously facilitate crystal nucleation crystallization.
2 liquid accelerator of comparative example does not pass through the load of DC power supply 3 and applies DC voltage, after making separation of solid and liquid by centrifugation With long-time using method validation comparison is stood, the crystal of formation is less, and measurement result and the result that static 60d is observed are poor It is different larger, show to load application DC voltage by DC power supply, is conducive to increase collision between solute ions and forms crystallization crystalline substance The probability of core accelerates solute ions enriching rate.
3 liquid accelerator of comparative example reduce centrifuge centrifugation rate, the crystal of formation is less, measurement result with it is static The result difference that 60d is observed is larger, shows that centrifugation rate is too low and is unfavorable for accelerator separation of solid and liquid, increases measurement result error Greatly.
Comparative example 4 changes the heating temperature of low-temperature oil bath cabinet, and the crystal of formation increases, and measurement result and static 60d are seen The result difference observed is larger, shows that the heating temperature for improving oil bath case can accelerate solvent volatilization, becomes the stability of accelerator Difference is unfavorable for the preservation of accelerator, reduces the accuracy of measurement result.
In conclusion test device of the present invention is simple to operate, measuring method and current standard are steady to liquid accelerator The advantages that correspondence of qualitative test result is good, repeatability is high, and measure quickly, it is applied widely.
The above, only of the invention illustrates embodiment, not to the present invention in any form with substantial limitation, It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, that makes several changes It also should be regarded as protection scope of the present invention into supplement.All those skilled in the art, do not depart from spirit of that invention and In the case where range, using the equivalent variations of a little change, modification and differentiation that disclosed above technology contents are made, it is Equivalent embodiment of the invention;Meanwhile any equivalent variations that all substantial technologicals according to the present invention do above-described embodiment Change, modification and differentiation, still fall within protection scope of the present invention.

Claims (6)

1. a kind of test device of liquid accelerator stability, which is characterized in that by low-temperature oil bath cabinet (1), ultrasonic disperse instrument (4), DC power supply (3), electrophoresis glass tube column (2) and centrifuge (6) composition, the electrophoresis glass tube column (2) is placed in described low In the oil bath pan of warm oil bath case (1);The DC power supply (3) is electrically connected with electrophoresis glass tube column (2) both ends;The ultrasound The concussion end of separating apparatus (4) is placed in the oil bath pan of the low-temperature oil bath cabinet (1).
2. a kind of measuring method of the test device of liquid accelerator stability described in claim 1, which is characterized in that including Following steps:
(1) the liquid accelerator sample of certain mass is taken to be directly loadable into electrophoresis glass tube column (2);
(2) step (1) is placed in the oil bath pan of low-temperature oil bath cabinet (1) equipped with the electrophoresis glass tube column (2) of liquid accelerator sample In, both ends DC power supply (3) on-load voltage is arranged oil bath temperature -10~0 DEG C, the concussion end of ultrasonic disperse instrument (4) is set In the oil bath pan of low-temperature oil bath cabinet (1), ultrasonic disperse instrument (4) oscillation frequency is set, after keeping 8~12h, takes out and liquid is housed The electrophoresis glass tube column (2) of accelerator sample;
(3) the liquid accelerator sample m that the step of weighing certain mass (2) is taken out1, it is fitted into centrifuge rotor (5) and is put into centrifugation Low-speed centrifugal in machine (6) weighs supernatant liquor quality m2
(4) crystal accounting V=(m is calculated1-m2)/m1
3. a kind of test device of liquid accelerator stability according to claim 1, which is characterized in that the electrophoresis glass Glass tubing string (2) both ends have conductive contact.
4. a kind of measuring method of the test device of liquid accelerator stability according to claim 2, which is characterized in that Ultrasonic disperse instrument (4) oscillation frequency is adjustable in 19.5~20.5kHz range in step (2), precision 0.1kHz.
5. a kind of measuring method of the test device of liquid accelerator stability according to claim 2, which is characterized in that DC power supply (3) is that exportable DC voltage is adjustable in 0~60V range in step (2), precision 0.1V.
6. a kind of measuring method of the test device of liquid accelerator stability according to claim 2, which is characterized in that Centrifuge (6) is centrifuged 5~10min with 2000~4000r/min revolving speed in step (3).
CN201810648952.2A 2018-06-22 2018-06-22 Testing device and measuring method for stability of liquid accelerator Active CN108896711B (en)

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