CN107449699A - The durothermic detection method of gel micro-ball - Google Patents
The durothermic detection method of gel micro-ball Download PDFInfo
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- CN107449699A CN107449699A CN201710552814.XA CN201710552814A CN107449699A CN 107449699 A CN107449699 A CN 107449699A CN 201710552814 A CN201710552814 A CN 201710552814A CN 107449699 A CN107449699 A CN 107449699A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
Abstract
The invention discloses a kind of durothermic detection method of gel micro-ball, belong to field of petroleum exploitation.The detection method includes：Obtain the aqueous solution of the gel micro-ball of preset quality concentration；Obtain respectively the aqueous solution of the gel micro-ball before heating, after unit volume absorbance；According to the unit volume absorbance, the particle retention of the gel micro-ball is obtained；According to the particle retention, the temperature tolerance of the gel micro-ball is judged.The present invention by obtain the aqueous solution of gel micro-ball before heating, after unit volume absorbance, the particle retention of gel micro-ball can be obtained, and then judge to be affected by temperature and be fused into the quantity of the gel micro-ball of liquid, and then quantitatively judge the temperature tolerance of gel micro-ball, detection method provided by the invention can avoid human error, can more accurately and fast judge the temperature tolerance of gel micro-ball.
Description
Technical field
The present invention relates to field of petroleum exploitation, more particularly to a kind of durothermic detection method of gel micro-ball.
Background technology
Gel micro-ball, it is a kind of pre-crosslinked gel microballoon, can be as the new profile control agent of oil field development.Such profile control agent according to
Formation pore throat is blocked by the gel micro-ball of nanoscale, micron order or submillimeter level, oil deposit deep part fluid diversion is realized, expands
The purpose of water drive swept volume.Because gel micro-ball has the characteristics of plugging effect is good, construction technology is simple, so being opened in oil field
During hair, its frequency of use also more and more higher.The heat resistance of gel micro-ball influences formation pore throat plugging effect, i.e. gel is micro-
It is one item important application inspection target that whether ball can also keep granular size stable gel microballoon at high temperature.It can be seen that, there is provided
A kind of durothermic detection method of gel micro-ball is very necessary.
At present, the micro- sem observation detection method of generally use detects to gel micro-ball temperature tolerance, including：By gel micro-ball
The sample coexisted with continuous media (such as water and crude oil) is placed under microscope, and detects gel micro-ball respectively using visually
Before heating, the particle size after, then according to the change of gel micro-ball particle size, to judge the temperature tolerance of gel micro-ball
Energy.
Inventor has found that prior art at least has problems with：
On the one hand, the droplet measurement of gel micro-ball is selected gel micro-ball particle by naked eyes and detected under the microscope,
In the presence of the deficiency that artificial difference and detection amounts of particles are limited, Fig. 1 is seen；On the other hand, gel micro-ball solution is showing after high temperature
It is difficult to separate itself and continuous media under micro mirror, observation difficulty is big, sees Fig. 2.
The content of the invention
In order to solve the above problems, the embodiments of the invention provide a kind of durothermic detection method of gel micro-ball.It is described
Technical scheme is as follows：
A kind of durothermic detection method of gel micro-ball, the detection method include：
Obtain the aqueous solution of the gel micro-ball of preset quality concentration；
Obtain respectively the aqueous solution of the gel micro-ball before heating, after unit volume absorbance；
According to the unit volume absorbance, the particle retention of the gel micro-ball is obtained；
According to the particle retention, the temperature tolerance of the gel micro-ball is judged.
Specifically, the aqueous solution of the gel micro-ball for obtaining preset quality concentration, including：
Gel micro-ball sample is purified, obtains gel micro-ball working substance；
The gel micro-ball working substance of scheduled volume is added in distilled water, prepares the aqueous solution of the gel micro-ball.
Specifically, it is described that gel micro-ball sample is purified, gel micro-ball working substance is obtained, including：
Absolute ethyl alcohol is added in the gel micro-ball sample, stirs to the gel micro-ball and separates out；
The solution for being precipitated with the gel micro-ball is filtered using Buchner funnel, obtains gel micro-ball filter cake；
Using absolute ethyl alcohol to the gel micro-ball Washing of Filter Cake, dry, obtain the gel micro-ball working substance.
Preferably, the mass concentration of the gel micro-ball in the aqueous solution of the gel micro-ball is 1%~2%.
Specifically, the calculation formula of the unit volume absorbance is：
B=A/V
In formula：
The unit volume absorbance of the aqueous solution of B --- gel micro-ball, %/ml；
The absorbance of the aqueous solution of A --- gel micro-ball, %；
The volume of the aqueous solution of V --- gel micro-ball, ml.
Specifically, the aqueous solution for obtaining the gel micro-ball respectively before heating, after unit volume absorbance, bag
Include：
The absorbance of the aqueous solution of the gel micro-ball before heating is detected using laser particle analyzer；
The aqueous solution of the gel micro-ball is put into the insulating box of preset temperature, heats preset time, cooling；
The absorbance of the aqueous solution of the detection gel micro-ball after the heating is obtained using the laser particle analyzer；
According to the calculation formula of the unit volume absorbance, the aqueous solution that the gel micro-ball is calculated is heating
Forward and backward unit volume absorbance.
Preferably, the preset time is 1 day, 4 days or 9 days.
Preferably, the preset temperature is 100 DEG C~130 DEG C.
Specifically, the calculation formula of the particle retention of the gel micro-ball is：
P=Bt × 100%/B0
In formula：
The particle retention of P --- gel micro-ball, %；
Unit volume absorbance of the aqueous solution of Bt --- gel micro-ball after the t periods are heated, %/ml；
B0--- the unit volume absorbance of the aqueous solution of gel micro-ball before heating, %/ml.
Specifically, the aqueous solution of the gel micro-ball is put into 120 DEG C of insulating box, after heating 9 days, if described solidifying
When the particle retention of glue microballoon is more than 80%, judge that the gel micro-ball temperature tolerance is good.
The beneficial effect that technical scheme provided in an embodiment of the present invention is brought is：
By obtain the aqueous solution of gel micro-ball before heating, after unit volume absorbance, gel micro-ball can be obtained
Particle retention, and then judge to be affected by temperature and be fused into the quantity of the gel micro-ball of liquid, and then quantitatively judge gel
The temperature tolerance of microballoon.It can be seen that detection method provided in an embodiment of the present invention, can avoid human error, can more accurately and fast
Judge the temperature tolerance of gel micro-ball.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, make required in being described below to embodiment
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for
For those of ordinary skill in the art, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is that prior art provides, the MIcrosope image of gel micro-ball before heating；
Fig. 2 is that prior art provides, the MIcrosope image of gel micro-ball after the heating；
Fig. 3 is the schematic flow sheet of the durothermic detection method of gel micro-ball provided in an embodiment of the present invention.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to embodiment party of the present invention
Formula is described in further detail.
The embodiments of the invention provide a kind of durothermic detection method of gel micro-ball, referring to Fig. 3, this method includes：
Step 1：Obtain the aqueous solution of the gel micro-ball of preset quality concentration.
Step 2：Respectively obtain gel micro-ball the aqueous solution before heating, after unit volume absorbance.
Step 3：According to unit volume absorbance, the particle retention of gel micro-ball is obtained.
Step 4：According to particle retention, the temperature tolerance of gel micro-ball is judged.
The durothermic detection method of gel micro-ball provided in an embodiment of the present invention, it is solidifying in the aqueous solution based on gel micro-ball
After glue microballoon heating a period of time, it can melt and become liquid, then the intensity of light through the aqueous solution of gel micro-ball will strengthen, from
And the absorbance of the aqueous solution of gel micro-ball is reduced.
The embodiment of the present invention in view of above-mentioned mechanism, by obtain the aqueous solution of gel micro-ball before heating, after unit bodies
Product absorbance, can obtain the particle retention of gel micro-ball, and then judge to be affected by temperature and be fused into the gel micro-ball of liquid
Quantity, and then quantitatively judge the temperature tolerance of gel micro-ball.It can be seen that detection method provided in an embodiment of the present invention, can be avoided
Human error, it can more accurately and fast judge the temperature tolerance of gel micro-ball.
It is understood that above-mentioned detection method is applied to detect the temperature tolerance of polytype gel micro-ball,
Such as SMG (Soft Micro Gel, flexible microgel) gel micro-ball.
Each step of above-mentioned detection method is illustrated below.
Step 1 is the aqueous solution for the gel micro-ball for obtaining preset quality concentration.
For the ease of preserving, gel micro-ball is usually dispersed in silicone oil, and suspension (i.e. gel micro-ball is collectively forming with silicone oil
Sample).Therefore before the aqueous solution of gel micro-ball is prepared, in order to avoid the impurity in gel micro-ball sample is to the water of gel micro-ball
The detection of solution absorbance is had an impact, it is necessary to be purified to the gel micro-ball in suspension.
Specifically, the method for obtaining the aqueous solution of the gel micro-ball of preset quality concentration, including：
Step 101：Gel micro-ball sample is purified, obtains gel micro-ball working substance.
The purpose of the step, mainly obtain the gel micro-ball working substance of high-purity.Wherein, gel micro-ball working substance is matter
Measure the gel micro-ball that fraction is more than 99%.
In practical operation, the mode that is purified to gel micro-ball sample has a variety of, such as following methods, this method bag
Include：
Step 1011：Absolute ethyl alcohol is added in gel micro-ball sample, stirs to gel micro-ball and separates out.
Specifically, while the absolute ethyl alcohol of scheduled volume is added in gel micro-ball sample, and gel micro-ball sample is entered
Row stirring, and after adding absolute ethyl alcohol, continue stirring a period of time (such as 5min, 10min etc.), until the gel micro-ball of white
All separate out.
In practical operation, in order that absolute ethyl alcohol can effectively separate out the gel micro-ball in gel micro-ball sample, and and can
Reduce absolute ethyl alcohol dosage, the volume of absolute ethyl alcohol and gel micro-ball sample can be arranged to it is identical, for example, can be by absolute ethyl alcohol
It is all provided with being set to 50ml with the volume of gel micro-ball sample.
It should be noted that because gel micro-ball sample is suspension, should be by gel micro-ball before absolute ethyl alcohol is added
Sample stirs.
Step 1012：The solution for being precipitated with gel micro-ball is filtered using Buchner funnel, obtains gel micro-ball filter cake.
Specifically, Buchner funnel is provided with the cylinder of multiple circular holes including bottom and is connected with bottom of cylinder elongated
Bar tubular exports.Before the solution to being precipitated with gel micro-ball filters, filter paper is placed in the upper base surface of cylinder so that analysis
Go out to have the solution of gel micro-ball when passing through filter paper, gel micro-ball does not pass through filter paper, and the solids of pie is formed on filter paper
(can be described as gel micro-ball filter cake).
Step 1013：Using absolute ethyl alcohol to gel micro-ball Washing of Filter Cake, dry, obtain gel micro-ball working substance.
In order to further obtain the gel micro-ball of high-purity, the embodiment of the present invention continues using absolute ethyl alcohol to gel
Microballoon Washing of Filter Cake.Specifically, adding absolute ethyl alcohol into the Buchner funnel equipped with gel micro-ball filter cake, pass through absolute ethyl alcohol
Gel micro-ball filter cake is flowed into tubular outlet, and then plays the purpose of detergent gel microballoon filter cake.
In practical operation, as the case may be gel micro-ball filter cake can be carried out using absolute ethyl alcohol repeatedly to wash (example
As 2 times, 3 times, it is 4 inferior), to obtain the gel micro-ball filter cake of high-purity.
After gel micro-ball Washing of Filter Cake is completed, gel micro-ball filter cake is removed from Buchner funnel, desiccant gel microballoon
Obtain gel micro-ball working substance.
Wherein, have to the mode of gel micro-ball filtration cakes torrefaction it is a variety of, for example, can be entered using baking oven to gel micro-ball filter cake
Row drying, or (20 DEG C~30 DEG C) drying a period of times (such as 12h, 24h, 36h etc.) are extremely dried at room temperature.When using nothing
When water-ethanol is to purify gel micro-ball, it should not select baking oven that glue microballoon filter cake is dried.
It should be noted that after gel micro-ball filtration cakes torrefaction forms gel micro-ball working substance completely, in order to avoid gel
Microballoon working substance makes moist, and gel micro-ball working substance need to be put into drier standby.
Step 102：The gel micro-ball working substance of scheduled volume is added in distilled water, prepares the aqueous solution of gel micro-ball.
In order to avoid containing impurity in water, and the detection to the aqueous solution absorbance of gel micro-ball has an impact, the present invention
Embodiment prepares the aqueous solution of gel micro-ball using distilled water, and while the aqueous solution of gel micro-ball is prepared, and carry out
Stirring.
In practical operation, in order that laser particle analyzer can more accurately obtain the extinction of the aqueous solution of gel micro-ball
Spend, the mass concentration of the gel micro-ball in the aqueous solution of gel micro-ball is 1%~2% (such as 1%, 2% etc.).
Step 2 be obtained respectively by laser particle analyzer the aqueous solution of gel micro-ball before heating, after unit volume inhale
Luminosity.
It is understood that use the absorbance (also referred to as absorptance) of laser particle analyzer detection sample common for this area
, wherein, laser particle analyzer can use the laser particle analyzer that Malvern Instr Ltd. of Britain produces and sold, or
Nanometer laser particle size analyzer of the models of Analysette 22 of Fritsch companies production etc..
Wherein, the calculation formula of the unit volume absorbance of the aqueous solution of gel micro-ball is：
B=A/V
In formula：
The unit volume absorbance of the aqueous solution of B --- gel micro-ball, %/ml；
The absorbance of the aqueous solution of A --- gel micro-ball, %；
The volume of the aqueous solution of V --- gel micro-ball, ml.
When by laser particle analyzer to obtain the unit volume absorbance of the aqueous solution of gel micro-ball before heating, first will
The aqueous solution of gel micro-ball stirs, and recycles laser particle analyzer to detect the absorbance of the aqueous solution of gel micro-ball, afterwards
According to above-mentioned calculation formula, to obtain the unit volume absorbance of the aqueous solution of gel micro-ball before heating.
When by laser particle analyzer come obtain the aqueous solution of gel micro-ball before heating, after unit volume absorbance when,
It can be operated according to following methods：
Step 201：The volume absorbance of the aqueous solution of gel micro-ball before heating is detected using laser particle analyzer.
Step 202：The aqueous solution of gel micro-ball is put into the insulating box of preset temperature, heats preset time, cooling.
Specifically, the aqueous solution of gel micro-ball is put into preset temperature, (preset temperature is typically chosen gel micro-ball application
Target reservoir formation temperature, such as 100 DEG C~130 DEG C, can be specially 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C etc.) constant temperature
In case, and preset time (wherein, preset time can be determined as the case may be, such as 1 day, 4 days or 9 days) is heated, it
Cool down (room temperature, such as 20 DEG C~30 DEG C can be cooled to) afterwards.
It should be noted that in order to prevent the aqueous solution of gel micro-ball from being volatilized in insulating box in heating process, and
The accuracy of detection of laser particle analyzer is influenceed, the aqueous solution of gel micro-ball need to be placed in closed container, place into perseverance afterwards
In incubator.
Further, since the laser particle analyzer of different model is respectively provided with the minimum absorbance that can be detected, this requires that gel is micro-
The aqueous solution of ball has minimum absorbance, such as the nanometer laser grain of the models of Analysette 22 of Fritsch companies production
Degree instrument requires that the absorbance of the aqueous solution of gel micro-ball is at least 7%, otherwise can influence the accuracy of detection.Again because gel is micro-
Heat time of the aqueous solution of ball in insulating box is longer, and the partial gel microballoon in the aqueous solution of gel micro-ball can be fused into liquid
Body, the absorbance after the aqueous solution heating of gel micro-ball can be caused to be less than 7%.The embodiment of the present invention is in order to avoid this kind of situation
Occur, heat time that can be according to the aqueous solution of gel micro-ball in insulating box, to determine the volume of the aqueous solution of gel micro-ball,
Specially：Longer, the aqueous solution for the gel micro-ball of test when heat time of the aqueous solution in insulating box of gel micro-ball
Sampling volume it is also bigger, and then can ensure there are enough gel micro-balls in the aqueous solution of gel micro-ball, even if there is one
The gel micro-ball divided is fused into liquid, also can guarantee that the absorbance of the aqueous solution of gel micro-ball is more than 7%, for example, when gel is micro-
For the aqueous solution of ball in the heating 4 days during temperature is 120 DEG C of insulating box, the volume of the aqueous solution of gel micro-ball takes 5ml；And add
When hot 9 days, the volume of the aqueous solution of gel micro-ball takes 75ml.
It should be noted that the aqueous solution of gel micro-ball used in this step is gel micro-ball used in previous step
The aqueous solution, i.e., after the unit volume absorbance of the aqueous solution of gel micro-ball before heating has been obtained, to the gel micro-ball
The aqueous solution is heated, to obtain the unit volume absorbance of the aqueous solution of the gel micro-ball after the heating.
Or the aqueous solution of gel micro-ball can be also divided into two parts, the aqueous solution that portion is used for obtaining gel micro-ball is adding
Unit volume absorbance before heat, in addition portion heated, for obtaining the unit of the aqueous solution of gel micro-ball after the heating
Volume absorbance.
Step 203：The absorbance of the aqueous solution of gel micro-ball after the heating is obtained using laser particle analyzer.
When using laser particle analyzer to obtain the unit volume absorbance of the aqueous solution of gel micro-ball after the heating, first will
The aqueous solution of gel micro-ball stirs, and recycles laser particle analyzer to detect the absorbance of the aqueous solution of gel micro-ball, afterwards
Further according to the calculation formula of the unit volume absorbance of the aqueous solution of above-mentioned calculated for gel microballoon, to obtain the water-soluble of gel micro-ball
The unit volume absorbance of liquid after the heating.
Step 204：According to the calculation formula of unit volume absorbance, the aqueous solution that gel micro-ball is calculated is heating
Forward and backward unit volume absorbance.
Step 3 be according to the aqueous solution of gel micro-ball before heating, after unit volume absorbance, obtain gel micro-ball
Particle retention.
Wherein, the calculation formula of the particle retention of gel micro-ball is：
P=Bt × 100%/B0
In formula：
The particle retention of P --- gel micro-ball, %；
Unit volume absorbance of the aqueous solution of Bt --- gel micro-ball after the t periods are heated, %/ml；
B0--- the unit volume absorbance of the aqueous solution of gel micro-ball before heating, %/ml.
After the embodiment of the present invention characterizes gel micro-ball heating using the particle retention of gel micro-ball, its amounts of particles
Change.Wherein, if the particle retention of gel micro-ball is higher, illustrate that the temperature tolerance of gel micro-ball is better；If gel micro-ball
Particle retention is lower, then illustrates that the temperature tolerance of gel micro-ball is poorer.
Step 4 is that the temperature tolerance of gel micro-ball is judged according to particle retention.
Temperature due to insulating box and the heat time in insulating box can all influence the particle retention of gel micro-ball, institute
With when judging the temperature tolerance of gel micro-ball, the temperature of insulating box is combined and in the two factors of the heat time of insulating box
Considered.
For example, the aqueous solution of gel micro-ball is put into 120 DEG C of insulating box, after heating 9 days, if of gel micro-ball
When grain retention rate is more than 80%, then judge that gel micro-ball temperature tolerance is good.
The present invention will be further described through by specific embodiment below.
In specific examples below, the unreceipted condition person of involved operation, according to normal condition or manufacturer
It is recommended that condition carry out.Raw materials used unreceipted production firm and specification person are can be by the conventional products of acquisition purchased in market.
Embodiment 1
Based on method provided in an embodiment of the present invention, durothermic detection of the present embodiment to the gel micro-ball of submillimeter level
Method illustrates.Wherein, the embodiment of the present invention uses nanometer laser particle size analyzer (the laser grains of the model of Analysette 22
Degree instrument requires 7%) absorbance of the aqueous solution of gel micro-ball is at least.
It is described in detail as steps described below below：
(1) gel micro-ball sample is purified, obtains gel micro-ball working substance
Poured into specifically, taking out 50ml samples after gel micro-ball sample is stirred first in beaker, then into beaker
50ml absolute ethyl alcohols are added, continues to stir 10min afterwards, separates out white precipitate (i.e. gel micro-ball).
Then the solution for being precipitated with gel micro-ball is poured into Buchner funnel and filtered, obtain gel micro-ball filter cake.
Afterwards again using absolute ethyl alcohol to the gel micro-ball Washing of Filter Cake in Buchner funnel three times；Finally by Buchner funnel
Gel micro-ball filter cake remove and be laid on filter paper, and 24h is dried under 25 DEG C of normal temperature, obtains gel micro-ball working substance, it
After be put into it is standby in drier.
(2) aqueous solution of gel micro-ball is prepared using distilled water
The aqueous solution for the gel micro-ball that mass concentration is 1% is prepared with distilled water, specifically, it is effective first to weigh gel micro-ball
The quality of thing, it is then determined that the addition of distilled water, in the present embodiment, the quality of gel micro-ball working substance is 10g, due to distillation
The density of water is 1g/ml, then the addition of distilled water is 990ml.
(3) absorbance of the aqueous solution of gel micro-ball before heating is detected
3ml solution example is taken out from the aqueous solution of above-mentioned gel micro-ball, and is stirred.Afterwards, utilize
The nanometer laser particle size analyzers of Analysette 22 carry out the above-mentioned solution example absorbance before heating that detection volume is 3ml, and it is examined
Survey the results are shown in Table 1.
(4) absorbance of the aqueous solution of gel micro-ball after the heating is detected
Take out the water of 100ml, 200ml, 500ml gel micro-ball in the aqueous solution of gel micro-ball respectively from step (2)
Solution, and being respectively implanted into 3 closed containers, be put into temperature afterwards for heated respectively in 120 DEG C of insulating boxs 1 day, 4 days, 9
My god.
Then, this 3 closed containers are taken out from insulating box, and after being cooled to room temperature.Afterwards, from this 3 closed appearances
Device takes out 3ml, 5ml, 75ml the gel micro-ball aqueous solution respectively, and is examined using the nanometer laser particle size analyzers of Analysette 22
The absorbance of the aqueous solution of gel micro-ball after the heating is surveyed, its testing result is shown in Table 1.
(5) particle retention of gel micro-ball is obtained
The micron order gel micro-ball temperature tolerance testing result table of table 1
(6) interpretation of result
Go out from the experimental results, it is normal in order to carry out after being heated 9 days to the aqueous solution of gel micro-ball at 120 DEG C
Detection, the volume of the aqueous solution of gel micro-ball increase to 75ml by 3ml, illustrate that partial gel microballoon has dropped at high temperature
Solution, gel micro-ball quantity are decreased obviously.With the extension of constant temperature time, the particle retention of gel micro-ball declines, degraded aggravation.
It can be seen in table 1 that after the gel micro-ball aqueous solution is heated 9 days, the particle retention of gel micro-ball is only 3%,
Less than 80%, then it can determine whether that the temperature tolerance of gel micro-ball is bad.
Embodiment 2
Based on method provided in an embodiment of the present invention, durothermic detection side of the present embodiment to micron-sized gel micro-ball
Method illustrates.Wherein, the embodiment of the present invention uses the nanometer laser particle size analyzer (laser particle sizes of the model of Analysette 22
Instrument requires 7%) absorbance of the aqueous solution of gel micro-ball is at least.
It is described in detail as steps described below below：
(1) gel micro-ball sample is purified, obtains gel micro-ball working substance
Poured into specifically, taking out 50ml samples after gel micro-ball sample is stirred first in beaker, then into beaker
50ml absolute ethyl alcohols are added, continues to stir 10min afterwards, separates out white precipitate (i.e. gel micro-ball).
Then the solution for going out to have gel micro-ball is poured into Buchner funnel and filtered, obtain gel micro-ball filter cake.
Afterwards again using absolute ethyl alcohol to the gel micro-ball Washing of Filter Cake in Buchner funnel three times；Finally by Buchner funnel
Gel micro-ball filter cake remove and be laid on filter paper, and 24h is dried under 25 DEG C of normal temperature, obtains gel micro-ball working substance, it
After be put into it is standby in drier.
(2) aqueous solution of gel micro-ball is prepared using distilled water
The aqueous solution for the gel micro-ball that mass concentration is 1% is prepared with distilled water, specifically, it is effective first to weigh gel micro-ball
The quality of thing, it is then determined that the addition of distilled water, in the present embodiment, the quality of gel micro-ball working substance is 10g, due to distillation
The density of water is 1g/ml, then the addition of distilled water is 990ml.
(3) absorbance of the aqueous solution before heating is detected
3ml solution example is taken out from the aqueous solution of above-mentioned gel micro-ball, and is stirred.Afterwards, utilize
The nanometer laser particle size analyzers of Analysette 22 carry out the above-mentioned solution example absorbance before heating that detection volume is 3ml, and it is examined
Survey the results are shown in Table 2.
(4) absorbance of the aqueous solution of gel micro-ball after the heating is detected
Take out the water of 100ml, 200ml, 500ml gel micro-ball in the aqueous solution of gel micro-ball respectively from step (2)
Solution, and being respectively implanted into 3 closed containers, be put into temperature afterwards for heated respectively in 120 DEG C of insulating boxs 1 day, 4 days, 9
My god.
Then, this 3 closed containers are taken out from insulating box, and after being cooled to room temperature.Afterwards, from this 3 closed appearances
Device takes out 3ml, 5ml, 75ml the gel micro-ball aqueous solution respectively, and is examined using the nanometer laser particle size analyzers of Analysette 22
The absorbance of the aqueous solution of gel micro-ball after the heating is surveyed, its testing result is shown in Table 2.
(5) particle retention of gel micro-ball is obtained
The micron order gel micro-ball temperature tolerance testing result table of table 2
(6) interpretation of result
Go out from the experimental results, it is normal in order to carry out after being heated 9 days to the aqueous solution of gel micro-ball at 120 DEG C
Detection, the volume of the aqueous solution of gel micro-ball increase to 75ml by 3ml, illustrate that partial gel microballoon has dropped at high temperature
Solution, gel micro-ball quantity are decreased obviously.With the extension of constant temperature time, the particle retention of gel micro-ball declines, degraded aggravation.
As seen from Table 2, after the aqueous solution of gel micro-ball is heated 9 days, the particle retention of gel micro-ball is
16.7%, less than 80%, then it can determine whether that gel micro-ball temperature tolerance is bad.
Above-mentioned all optional technical schemes, any combination can be used to form the alternative embodiment of the disclosure, herein no longer
Repeat one by one.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (10)
1. a kind of durothermic detection method of gel micro-ball, it is characterised in that the detection method includes：
Obtain the aqueous solution of the gel micro-ball of preset quality concentration；
Obtain respectively the aqueous solution of the gel micro-ball before heating, after unit volume absorbance；
According to the unit volume absorbance, the particle retention of the gel micro-ball is obtained；
According to the particle retention, the temperature tolerance of the gel micro-ball is judged.
2. detection method according to claim 1, it is characterised in that the gel micro-ball for obtaining preset quality concentration
The aqueous solution, including：
Gel micro-ball sample is purified, obtains gel micro-ball working substance；
The gel micro-ball working substance of scheduled volume is added in distilled water, prepares the aqueous solution of the gel micro-ball.
3. detection method according to claim 2, it is characterised in that it is described that gel micro-ball sample is purified, obtain
Gel micro-ball working substance, including：
Absolute ethyl alcohol is added in the gel micro-ball sample, stirs to the gel micro-ball and separates out；
The solution for being precipitated with the gel micro-ball is filtered using Buchner funnel, obtains gel micro-ball filter cake；
Using absolute ethyl alcohol to the gel micro-ball Washing of Filter Cake, dry, obtain the gel micro-ball working substance.
4. detection method according to claim 1, it is characterised in that the gel micro-ball in the aqueous solution of the gel micro-ball
Mass concentration be 1%~2%.
5. detection method according to claim 1, it is characterised in that the calculation formula of the unit volume absorbance is：
B=A/V
In formula：
The unit volume absorbance of the aqueous solution of B --- gel micro-ball, %/ml；
The absorbance of the aqueous solution of A --- gel micro-ball, %；
The volume of the aqueous solution of V --- gel micro-ball, ml.
6. detection method according to claim 5, it is characterised in that the aqueous solution for obtaining the gel micro-ball respectively
Before heating, the unit volume absorbance after, including：
The absorbance of the aqueous solution of the gel micro-ball before heating is detected using laser particle analyzer；
The aqueous solution of the gel micro-ball is put into the insulating box of preset temperature, heats preset time, cooling；
The absorbance of the aqueous solution of the detection gel micro-ball after the heating is obtained using the laser particle analyzer；
According to the calculation formula of the unit volume absorbance, be calculated the aqueous solution of the gel micro-ball before heating, after
Unit volume absorbance.
7. detection method according to claim 6, it is characterised in that the preset time is 1 day, 4 days or 9 days.
8. detection method according to claim 6, it is characterised in that the preset temperature is 100 DEG C~130 DEG C.
9. detection method according to claim 5, it is characterised in that the calculating of the particle retention of the gel micro-ball is public
Formula is：
P=Bt × 100%/B0
In formula：
The particle retention of P --- gel micro-ball, %；
Unit volume absorbance of the aqueous solution of Bt --- gel micro-ball after the t periods are heated, %/ml；
B0--- the unit volume absorbance of the aqueous solution of gel micro-ball before heating, %/ml.
10. detection method according to claim 1, it is characterised in that the aqueous solution of the gel micro-ball is put into 120
DEG C insulating box in, heating 9 days after, if the particle retention of the gel micro-ball be more than 80%, judge the gel micro-ball
Temperature tolerance is good.
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