CN106865591A - The screening technique of calcium inhibitors is fluorinated under a kind of high temperature system - Google Patents
The screening technique of calcium inhibitors is fluorinated under a kind of high temperature system Download PDFInfo
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- CN106865591A CN106865591A CN201611089414.1A CN201611089414A CN106865591A CN 106865591 A CN106865591 A CN 106865591A CN 201611089414 A CN201611089414 A CN 201611089414A CN 106865591 A CN106865591 A CN 106865591A
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- calcirm
- fluoride
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- inhibitor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/22—Fluorides
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Abstract
A kind of screening technique the present invention relates to be fluorinated calcium inhibitors under high temperature system, the method being combined using centrifugation technique and high-temperature heating, after multiple centrifuge tube high temperature heating weighed are added separately to added with the various different inhibitor of calcirm-fluoride powder, supernatant is removed by centrifugation, weigh undissolved calcirm-fluoride quality, according to of poor quality before and after calcirm-fluoride, calcirm-fluoride dissolution rate is calculated, and then various fluorination calcium inhibitorses are screened according to numerical values recited.The present invention has advantages below：One is method simple to operate, quick, high precision, reproducible, and can disposably screen various inhibitors；Two is the influence that the method fully takes into account hot conditions, can objective evaluation inhibition under the high temperature conditions, filter out the fluorination calcium inhibitors for meeting hot conditions application, it is practical；Three is that the method is based on solubilizing mechanism, and opposite direction screens fluorination calcium inhibitors by determining the size of calcirm-fluoride dissolution rate in inhibitor.
Description
Technical field
The invention belongs to water process and acidification of oil field measure technical field, it is related to be fluorinated calcium inhibitors under a kind of high temperature system
Screening technique.
Background technology
Calcirm-fluoride is derived partly from nature fluorite ore, fluorination work and photovoltaic industry fluoride waste precipitation process and is formed
Calcium fluoride sludge, in addition, also most of calcirm-fluoride come from acidification of oil field treatment process hydrofluoric acid or mud acid with
The calcirm-fluoride mineral of the reaction generation such as calcite, dolomite, anorthite, zeolite, clay of sandstone reservoir, the fluorine produced by these
Changing calcium can pollute environment or block stratum.
It is fluorinated what traditional evaluation method of calcium inhibitors was typically all carried out at ambient temperature, and actual acidification of oil field operation
In due to formation temperature it is higher, cause the evaluation method to lose certain practicality, tend to occur at the suppression screened under normal temperature
The good fluorination calcium inhibitors of effect processed, calcium fluoride precipitate can be produced when being applied to the hot environments such as stratum because of inhibition difference
Phenomenon.Current this area is higher to the temperature conditionss required by fluorination calcium inhibitors, typically all at 100 DEG C or so, but consults state
Inside and outside pertinent literature, in addition to indivedual enterprises have formulated the technical indicator of correlation to fluorination calcium inhibitors, to being fluorinated under high temperature system
The evaluation method of calcium inhibitors is still without related standard and elaboration.Therefore, develop as early as possible and quickly sieve under a kind of high temperature system
The method of choosing fluorination calcium inhibitors, is one of this area urgent problem.
The content of the invention
It is an object of the invention to be solved to the problem that prior art is present, calcirm-fluoride under a kind of high temperature system is proposed
The screening technique of inhibitor, is used to for Fast Evaluation fluorination calcium inhibitors provides help under high-temperature body system.
The technical solution used to realize above goal of the invention is as described below.
The screening technique of calcium inhibitors is fluorinated under a kind of high temperature system, it is characterised in that comprise the following steps：
1) it is m by a quality2Calcirm-fluoride powder and a quality be m4A kind of inhibitor be added to one and dried
Constant weight quality be m1Centrifuge tube in；
2) centrifuge tube is placed in baking oven and is heated 2~3 hours with 70~100 DEG C of temperature；
3) to centrifugation liquid in pipe do centrifugal treating, through centrifugation after, pour out supernatant, at twice with distillation water washing it is not molten
Thing, and pour out；
4) by centrifuge tube and remaining not molten thing drying, constant weight gross mass is m3；
5) according to of poor quality before and after calcirm-fluoride, dissolution rate of the calcirm-fluoride in the inhibitor is 1. calculated by formula,
In formula：η-calcirm-fluoride dissolution rate,
m1- centrifuge tube quality, unit is g,
m2- calcirm-fluoride powder quality, unit is g,
m3- centrifuge tube and not molten thing gross mass, unit is g；
6) it is m by another quality2Calcirm-fluoride powder and another quality be m4Another inhibitor be added to it is another
The individual constant weight quality dried is m1Centrifuge tube in；
7) repeat step 2)~step 5), obtain calcirm-fluoride dissolution rate η of the calcirm-fluoride in another inhibitor；
8) repeat step 6)~step 7), calcirm-fluoride dissolution rate η of the calcirm-fluoride in various different inhibitor is obtained respectively；
9) numerical values recited according to η evaluates the inhibition of various different inhibitor used by These steps, and η values are bigger,
Illustrate that the amount that calcirm-fluoride is dissolved in inhibitor is more, not molten thing is fewer, i.e., inhibition is better, so that can be in each suppression used
The best fluorination calcium inhibitors of inhibition is filtered out in preparation.
It is fluorinated in the screening technique of calcium inhibitors under above-mentioned high temperature system, the quality m of calcirm-fluoride powder2It is 0.1~4g, suppression
Quality of the pharmaceutical preparations m4It is 1~10g.
It is fluorinated in the screening technique of calcium inhibitors under above-mentioned high temperature system, rotating speed centrifugal treating is done to centrifugation liquid in pipe
Centrifugal rotational speed is 3000~4000rpm, and centrifugation time is 5~10min.
It is fluorinated in the screening technique of calcium inhibitors under above-mentioned high temperature system, the drying temperature in each step is 105 ± 1
DEG C, centrifuge tube constant weight quality m1It is exquisite to 0.0001g, calcirm-fluoride powder quality m2It is exquisite to 0.0001g, centrifuge tube and not molten thing
Gross mass m3It is exquisite to 0.0001g.
The screening technique that calcium inhibitors is fluorinated under high temperature system of the present invention is a kind of screening based on solubilizing mechanism
Method, its place for being different from traditional normal temperature screening technique is, under the high temperature conditions, the method combination on-site actual situations
Inhibition is evaluated by determining the size of calcirm-fluoride dissolution rate in inhibitor, fluorination calcium inhibitors is then filtered out.With
Prior art is compared, and the present invention has advantages below：One is method simple to operate, quick, high precision, reproducible, and can one
Secondary property screens various inhibitors；Two is the influence that the method fully takes into account hot conditions, can objective evaluation suppression under the high temperature conditions
Effect processed, filters out the fluorination calcium inhibitors for meeting hot conditions application, practical；Three is that the method is based on solubilizing mechanism, instead
Fluorination calcium inhibitors is screened by determining the size of calcirm-fluoride dissolution rate in inhibitor in direction.
Specific embodiment
Present invention is described further below with reference to embodiment, it is necessary to explanation is, following lifted implementations
The invention is not limited in any way for example, and all technical schemes obtained by the way of equivalent or equivalent transformation are fallen
Within the scope of the present invention.
Embodiment 1
The screening technique of calcium inhibitors is fluorinated under a kind of high temperature system, is comprised the following steps：
(1) 10 centrifuge tubes are dried to constant weight at 104 DEG C, weigh (m respectively1, 1) quality be shown in Table.
(2) 10 kinds of inhibitor (being specifically shown in Table 1) are selected, the calcirm-fluoride powder of each inhibitor of 2.5g and 1g or so is weighed respectively
(m2, 1) specific quality be shown in Table, be respectively placed in different centrifuge tubes.
(3) above-mentioned centrifuge tube is placed in baking oven and in heating 3h at 75 DEG C.
(4) 6min and then by the centrifuge tube after above-mentioned heating is centrifuged under 4000rpm rotating speeds, interior upper strata will be managed after centrifugation clear
Liquid is poured out, then uses not molten thing in each pipe of distillation water washing at twice, and is poured out.
(5) each centrifuge tube and corresponding not molten one piece of thing are dried to constant weight at 104 DEG C respectively, weigh (m3, quality is shown in Table
1)。
(6) according to of poor quality before and after calcirm-fluoride, dissolution rate of the calcirm-fluoride in variant inhibitor is calculated, the results are shown in Table 1.
Dissolving situation of the calcirm-fluoride of table 1 in different inhibitor
As seen from Table 1, under the conditions of 75 DEG C, calcirm-fluoride has different degrees of molten more than in 10 kinds of different inhibitor
Solution, especially dissolution rate is up to 99.3% in HK608.It can be seen that when 10 kinds of inhibitor are screened under the high temperature conditions, HK608 pairs
The dissolubility of calcirm-fluoride is good, and inhibition is good, can screen to adapt to the fluorination calcium inhibitors of hot environment.
Embodiment 2
The screening technique of calcium inhibitors is fluorinated under a kind of high temperature system, is comprised the following steps：
(1) 9 centrifuge tubes are dried to constant weight at 105 DEG C, weigh (m respectively1, 2) quality be shown in Table.
(2) 9 kinds of inhibitor (being specifically shown in Table 2) are selected, the calcirm-fluoride powder (m of each inhibitor of 5g and 2g or so is weighed respectively2,
2) specific quality is shown in Table, and is respectively placed in different centrifuge tubes.
(3) above-mentioned centrifuge tube is placed in baking oven in heating 2.5h at 85 DEG C.
(4) 8min and then by the centrifuge tube after above-mentioned heating is centrifuged under 3500rpm rotating speeds, by the upper strata in pipe after centrifugation
Clear liquid is poured out, then uses not molten thing in each pipe of distillation water washing at twice, and is poured out.
(5) each centrifuge tube and corresponding not molten one piece of thing are dried to constant weight at 105 DEG C respectively, weigh (m3, quality is shown in Table
2)。
(6) according to of poor quality before and after calcirm-fluoride, dissolution rate of the calcirm-fluoride in variant inhibitor is calculated, the results are shown in Table 2.
Dissolving situation of the calcirm-fluoride of table 2 in different inhibitor
As seen from Table 2, under the conditions of 85 DEG C, calcirm-fluoride has molten to some extent more than in 9 kinds of different inhibitor
Solution, especially dissolution rate is up to more than 99% in HK608, HK508 inhibitor, it is seen that 9 kinds of inhibitor are carried out under the high temperature conditions
During screening, HK608, HK508 are good to the dissolubility of calcirm-fluoride, and inhibition is good, can screen to adapt to the calcirm-fluoride of hot environment
Inhibitor.
Embodiment 3
The screening technique of calcium inhibitors is fluorinated under a kind of high temperature system, is comprised the following steps：
(1) 8 centrifuge tubes are dried to constant weight at 106 DEG C, weigh (m respectively1, 3) quality be shown in Table.
(2) 8 kinds of inhibitor (being specifically shown in Table 3) are selected, the calcirm-fluoride powder (m of each inhibitor of 10g and 4g or so is weighed respectively2,
3) specific quality is shown in Table, and is respectively placed in different centrifuge tubes.
(3) above-mentioned centrifuge tube is placed in baking oven in heating 2h at 100 DEG C.
(4) 6min and then by the centrifuge tube after above-mentioned heating is centrifuged under 3000rpm rotating speeds, by the upper strata in pipe after centrifugation
Clear liquid is poured out, then uses not molten thing in each pipe of distillation water washing at twice, and is poured out.
(5) each centrifuge tube and corresponding not molten one piece of thing are dried to constant weight at 106 DEG C respectively, weigh (m3, quality is shown in Table
3)。
(6) according to of poor quality before and after calcirm-fluoride, dissolution rate of the calcirm-fluoride in variant inhibitor is calculated, the results are shown in Table 3.
Dissolving situation of the calcirm-fluoride of table 3 in different inhibitor
As seen from Table 3, under the conditions of 100 DEG C, calcirm-fluoride 8 more than in have molten to some extent in different inhibitor
Solution, especially dissolution rate is up to more than 99.5% in HK508 inhibitor, it is seen that 8 kinds of inhibitor are screened under the high temperature conditions
When, HK508 preferably, can be screened to adapt to the fluorination calcium inhibitors of hot environment to calcirm-fluoride inhibition.
Claims (4)
1. the screening technique of calcium inhibitors is fluorinated under a kind of high temperature system, it is characterised in that comprised the following steps：
1) it is m by a quality2Calcirm-fluoride powder and a quality be m4A kind of inhibitor be added to a perseverance dried
Heavy amount is m1Centrifuge tube in；
2) centrifuge tube is placed in baking oven and is heated 2~3 hours with 70~100 DEG C of temperature；
3) to centrifugation liquid in pipe do centrifugal treating, through centrifugation after, pour out supernatant, at twice with distillation the not molten thing of water washing,
And pour out；
4) by centrifuge tube and remaining not molten thing drying, constant weight gross mass is m3；
5) according to of poor quality before and after calcirm-fluoride, dissolution rate of the calcirm-fluoride in the inhibitor is 1. calculated by formula,
In formula：η-calcirm-fluoride dissolution rate,
m1- centrifuge tube quality, unit is g,
m2- calcirm-fluoride powder quality, unit is g,
m3- centrifuge tube and not molten thing gross mass, unit is g；
6) it is m by another quality2Calcirm-fluoride powder and another quality be m4Another inhibitor be added to another
The constant weight quality of drying is m1Centrifuge tube in；
7) repeat step 2)~step 5), obtain dissolution rate η of the calcirm-fluoride in another inhibitor；
8) repeat step 6)~step 7), dissolution rate η of the calcirm-fluoride in various different inhibitor is obtained respectively；
9) numerical values recited according to η evaluates the inhibition of the various different inhibitor used by each step, and η values are bigger, suppresses effect
Fruit is better, so as to filter out the best fluorination calcium inhibitors of inhibition wherein.
2. the screening technique of calcium inhibitors is fluorinated under high temperature system according to claim 1, it is characterised in that calcium fluoride powder
The quality m at end2It is 0.1~4g, inhibitor quality m4It is 1~10g.
3. the screening technique of calcium inhibitors is fluorinated under high temperature system according to claim 1, it is characterised in that to centrifuge tube
The centrifugal rotational speed that interior liquid does rotating speed centrifugal treating is 3000~4000rpm, and centrifugation time is 5~10min.
4. the screening technique of calcium inhibitors is fluorinated under high temperature system according to claim 1, it is characterised in that in each step
Drying temperature be in 105 ± 1 DEG C, centrifuge tube constant weight quality m1It is exquisite to 0.0001g, calcirm-fluoride powder quality m2Exquisiteness is extremely
0.0001g, centrifuge tube and not molten thing gross mass m3It is exquisite to 0.0001g.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680350A (en) * | 2012-06-01 | 2012-09-19 | 南京大学 | Scale inhibitor performance evaluation device and method suitable for circulating cooling water systems |
| CN103837657A (en) * | 2014-03-18 | 2014-06-04 | 山东大学 | Method suitable for evaluating performance of deep-layer brine scale inhibitor |
| CN105628540A (en) * | 2014-10-30 | 2016-06-01 | 赵建英 | Performance evaluation method of scale inhibitor for petrochemical process |
-
2016
- 2016-12-01 CN CN201611089414.1A patent/CN106865591A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680350A (en) * | 2012-06-01 | 2012-09-19 | 南京大学 | Scale inhibitor performance evaluation device and method suitable for circulating cooling water systems |
| CN103837657A (en) * | 2014-03-18 | 2014-06-04 | 山东大学 | Method suitable for evaluating performance of deep-layer brine scale inhibitor |
| CN105628540A (en) * | 2014-10-30 | 2016-06-01 | 赵建英 | Performance evaluation method of scale inhibitor for petrochemical process |
Non-Patent Citations (2)
| Title |
|---|
| 张曙光等: "极限碳酸盐硬度法评定阻垢剂的阻垢性能", 《工业水处理》 * |
| 聂宗利等: "阻垢剂的阻垢性能评价方法", 《应用化工》 * |
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Application publication date: 20170620 |